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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Divisional Application of, and claims priority to, under 35 U.S.C. § 121, U.S. Non-Provisional application Ser. No.: 10/886,196, entitled Carbonated Cleaning Composition and Method of Use, by Edward E. Durrant, filed on Jul. 7, 2004.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to carbonated compositions for cleaning textile fibers. More particularly the present invention relates to carbonated compositions containing carbonate salt and an acid with a low solubility for delaying the production of carbon dioxide.
[0004] 2. Description of the Related Art
[0005] There are innumerable cleaning compositions for cleaning textile fibers such as carpets, upholstery, drapery, and the like. Each type of cleaning composition is formulated to loosen and disperse the soil from the textile fibers either physically or by chemical reaction. The soil can then be solubilized or suspended in such a manner that it can be removed from the fibers being cleaned.
[0006] Most of these cleaning compositions are based on soaps or detergents, both of which are generically referred to as “surfactants”. By “detergent” is meant a synthetic amphipathic molecule having a large non-polar hydrocarbon end that is oil-soluble and a polar end that is water soluble. “Soap” is also an amphipathic molecule made up of an alkali salt, or mixture of salts, of long-chain fatty acids wherein the acid end is polar or hydrophilic and the fatty acid chain is non-polar or hydrophobic. Detergents are further classified as non-ionic, anionic, or cationic. Anionic or nonionic detergents are the most common.
[0007] These surfactants function because the hydrophobic ends of the molecules coat or adhere to the surface of soils and oils and the water soluble hydrophilic (polar) ends are soluble in water and help to solubilize or disperse the soils and oils in an aqueous environment.
[0008] There are several problems associated with the use of surfactants for cleaning fibers, such as carpeting and upholstery. First, large amounts of water are generally required to remove the surfactants and suspended or dissolved particles. This leads to long drying times and susceptibility to mildew. Second, surfactants generally leave an oily hydrophobic coating on the fiber surface. The inherent oily nature of the hydrophobic end of the surfactants causes premature resoiling even when the surfaces have a surfactant coating which is only a molecule thick. Third, surfactants can sometimes cause irritation or allergic reactions in people who are sensitive to these chemicals. Fourth, several environmental problems are associated with the use of soaps and detergents; some are non-biodegradable and some contain excessive amounts of phosphates, which are also environmentally undesirable.
[0009] In an attempt to solve at least some of these problems, numerous cleaning compositions have been developed. A significant improvement in the art of cleaning textile fibers, and carpets and upholstery teaches that when detergent solutions are carbonated and applied to the fibers, the solution rapidly penetrates the fibers and, through the effervescent action of the carbonation, quickly lifts the suspended soil and oil particles to the surface of the fiber from which they can be removed by vacuuming or transfer to an absorptive surface. Moreover, effervescent action requires less soap or other surfactant applied to the fibers. Because less soap or other surfactant is needed, less water is needed to affect the cleaning, and therefore, the fibers dry more rapidly than do fibers treated with conventional steam cleaning or washing applications, and little residue is left on the fibers. This results in less resoiling due to the reduced residue and a decreased likelihood of brown out because of the more rapid drying of the fibers. Although this effervescent action process is clearly advantageous over prior art methods, it still requires the use of some surfactant and, in some instances, added phosphates, which are undesirable in today's environmentally conscious society.
[0010] Generally, carbon dioxide, and thus the carbonation, is created by mixing a powdered carbonate with an acid. Because gases, including carbon dioxide, are much less soluble in hot water than cold water, it has generally been advised to mix the cleaning solution (the powdered product, which is powdered carbonate and powdered acid) in cold water to help preserve higher levels of carbonation in the cleaning solution. It is between the mixing of the powdered product with water, and before the container containing the mixture is capped, that some of the carbon dioxide is released and lost into the surrounding atmosphere. If hot water is used to make the cleaning solution, an even greater amount of carbon dioxide can escape before the lid is secured. On the other hand, cleaning solutions generally clean more effectively when they are at elevated temperatures.
[0011] Accordingly systems have been created, which hold the acid and carbonate salt in separate reservoirs and individually heat the solutions before being combined into a third container, or before being sprayed onto the textile. The result is a complex and expensive system requiring numerous reservoirs, valves, nozzles, hoses, solutions, etc.
[0012] Thus, it can be clearly recognized that there is a need for a cleaning composition formulated in a single reservoir with hot water, carbonate salt, and an acid with low solubility, which produces a delayed high level of carbonation for an extended period of time.
SUMMARY OF THE INVENTION
[0013] The various elements of the present invention have been developed in response to the present state of the art, and in particular, in response to the problems and needs in the art that have not yet been fully solved by currently available cleaning compositions. Accordingly, the present invention provides an improved internally carbonated cleaning solution using an acid with low water solubility.
[0014] More particularly, the present invention relates to an internally carbonated aqueous cleaning composition for textiles comprising about 20 to 60%, in percent by weight, of at least one carbonate salt, about 20 to 60%, in percent by weight, of at least one acid, the acid having a solubility less than two grams per 100 grams of water at about twenty five degrees Celsius. An aqueous medium is added to the carbonate salt and the acid to produce carbon dioxide.
[0015] In another embodiment, the composition comprises about 40 to 60% of the acid and about 35 to 50% of the carbonate salt.
[0016] In one embodiment, the solid acid is either fumaric acid or adipic acid.
[0017] In another embodiment, the carbonate salt is selected from the group consisting of sodium carbonate, sodium percarbonate, sodium bicarbonate, lithium carbonate, lithium percarbonate, lithium bicarbonate, potassium carbonate, potassium percarbonate, potassium bicarbonate, ammonium carbonate, sodium sesquicarbonate, potassium sesquicarbonate, lithium sesquicarbonate, and ammonium sesquicarbonate, and ammonium bicarbonate, or any other effective carbonate salt.
[0018] In another embodiment, the aqueous medium is added to the carbonate salt and the acid at a temperature above thirty two degrees Celsius.
[0019] In another embodiment, when the composition is mixed with the aqueous medium to form a solution, the composition concentration resulting from the carbonate salt and acid in the solution is between about 0.5 to 3%.
[0020] In another embodiment, the present invention relates to a method of cleaning textile fibers comprising the steps of applying to the fibers, an internally-carbonating cleaning composition, the composition being prepared by admixing 20 to 60%, in percent by weight, a carbonate salt and 20 to 60%, in percent by weight, an acid with a solubility less than two grams per 100 grams of water at twenty five degrees Celsius, and wherein when the carbonate salt and the acid are mixed in an aqueous medium, the carbonate salt and acid react to produce carbon dioxide.
[0021] Reference throughout this specification to features, advantages, or similar language does not imply that all of the features and advantages that may be realized with the present invention should be or are in any single embodiment of the invention. Rather, language referring to the features and advantages is understood to mean that a specific feature, advantage, or characteristic described in connection with an embodiment is included in at least one embodiment of the present invention. Thus, discussion of the features and advantages, and similar language, throughout this specification may, but do not necessarily, refer to the same embodiment.
[0022] Furthermore, the described features, advantages, and characteristics of the invention may be combined in any suitable manner in one or more embodiments. One skilled in the relevant art will recognize that the invention can be practiced without one or more of the specific features or advantages of a particular embodiment. In other instances, additional features and advantages may be recognized in certain embodiments that may not be present in all embodiments of the invention.
[0023] These features and advantages of the present invention will become more fully apparent from the following description and appended claims, or may be learned by the practice of the invention as set forth hereinafter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] In order for the advantages of the invention to be readily understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings. Understanding that these drawings depict only typical embodiments of the invention and are not therefore to be considered to be limiting of its scope, the invention will be described and explained with additional specificity and detail through the use of the accompanying drawings, in which:
[0025] FIG. 1 illustrates a comparison graph showing the response of carbon dioxide production versus time for fumaric and citric acid; and
[0026] FIG. 2 illustrates a comparison graph showing the response of carbon dioxide production versus time for fumaric and tartaric acid.
DETAILED DESCRIPTION OF THE INVENTION
[0027] For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the exemplary embodiments illustrated in the drawings, and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended. Any alterations and further modifications of the inventive features illustrated herein, and any additional applications of the principles of the invention as illustrated herein, which would occur to one skilled in the relevant art and having possession of this disclosure, are to be considered within the scope of the invention.
[0028] Reference throughout this specification to “one embodiment,” “an embodiment,” or similar language means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, appearances of the phrases “one embodiment,” “an embodiment,” and similar language throughout this specification may, but do not necessarily, all refer to the same embodiment, different embodiments, or component parts of the same or different illustrated invention. Additionally, reference to the wording “an embodiment,” or the like, for two or more features, elements, etc. does not mean that the features are related, dissimilar, the same, etc. The use of the term “an embodiment,” or similar wording, is merely a convenient phrase to indicate optional features, which may or may not be part of the invention as claimed.
[0029] Each statement of an embodiment is to be considered independent of any other statement of an embodiment despite any use of similar or identical language characterizing each embodiment. Therefore, where one embodiment is identified as “another embodiment,” the identified embodiment is independent of any other embodiments characterized by the language “another embodiment.” The independent embodiments are considered to be able to be combined in whole or in part one with another as the claims and/or art may direct, either directly or indirectly, implicitly or explicitly.
[0030] Finally, the fact that the wording “an embodiment,” or the like, does not appear at the beginning of every sentence in the specification, such as is the practice of some practitioners, is merely a convenience for the reader's clarity. However, it is the intention of this application to incorporate by reference the phrasing “an embodiment,” and the like, at the beginning of every sentence herein where logically possible and appropriate.
[0031] As used herein, “comprising,” “including,” “containing,” “is, “are,” “characterized by,” and grammatical equivalents thereof are inclusive or open-ended terms that do not exclude additional unrecited elements or method steps. “Comprising” is to be interpreted as including the more restrictive terms “consisting of” and “consisting essentially of.”
[0032] In a first embodiment, a solid acid and carbonate salt are prepared and admixed in a single container and then diluted with a desired amount of water. The carbonate salt may be any one of, or a combination of the group consisting of sodium carbonate, sodium percarbonate, sodium bicarbonate, lithium carbonate, lithium percarbonate, lithium bicarbonate, potassium carbonate, potassium percarbonate, potassium bicarbonate, ammonium carbonate, sodium sesquicarbonate, potassium sesquicarbonate, lithium sesquicarbonate, and ammonium sesquicarbonate, and ammonium bicarbonate, or any other effective carbonate salt. The solid acid, preferably, has a low solubility, with a maximum solubility of approximately two grams of acid per one hundred grams of water at twenty five degrees Celsius. Examples of solid acids with low solubility include Fumaric acid, with a solubility of 0.63 grams per one hundred grams of water at twenty five degrees Celsius, and Adipic acid, with a solubility of about 1.44 grams per one hundred grams of water at twenty five degrees Celsius. Other solid acids with low solubility will also work.
[0033] The solid acids and carbonate salts are mixed or ground together to form a solid mixture. The solid mixture contains from about 20% to 60% carbonate salts and about 20% to 60% of a natural solid acid with a low solubility. The most preferable mixture contains 35% to 50% carbonate salt and 40% to 60% acid.
[0034] Additionally, in another embodiment, the water temperature exceeds forty eight degrees Celsius. However, it is recognized that the water temperature may be as low as room temperature. Preferably, the temperature is not below thirty two degrees Celsius as the time for the acid to mix with the water may be excessively long. When the water is added to the solid mixture of acid and carbonate salt, the ingredients react to form the carbon dioxide, which creates effervescent bubbles.
[0035] The solution is applied to the textiles as a spray; however, other known methods of applying the solution may be used. When sprayed, for example, through a wand from a pressurized container, the pressure is released when the solution is exposed to the atmosphere, and the carbonated cleaning solution breaks into a myriad of tiny effervescent bubbles.
[0036] The combined carbonation action and the cleaning solution results in a low water volume. Specifically, the soils or oil on the fibers being cleaned are surrounded by a complex of carbon dioxide bubbles and polar and non-polar ended molecules that bind with and suspend the soil. The cleaning solution then can be lifted from the fibers into the surrounding carbonating aqueous environment. By “aqueous” it is meant that there is a certain amount of water, but that does not suggest that copious amounts of water are present. In fact, it has been found that only a slight dampening of the fiber may be sufficient to promote the lifting action of the effervescent carbonated solution to loosen or dislodge the soil or oil particles from the fiber. Additionally, it has been found that the active salts, created by the carbonate/bicarbonate mix, and carbon dioxide interactive substance or complex, hold the soil particles in suspension for a time sufficient for them to be removed from the fiber by means of vacuuming or adsorption onto a textile pad, toweling or similar adsorbent material.
[0037] Typically, the acid, carbonate salt, and water ingredients are mixed in a single container. Advantageously, because the acid has a low solubility, the creation of carbonation is delayed longer than high solubility acids. This delayed carbonation provides the user with sufficient time to mix the ingredients together and seal the container before any considerable amount of the carbonation is lost to the atmosphere.
[0038] FIG. 1 illustrates a comparison graph showing the response time of carbon dioxide production for fumaric and citric acid. To quantify these results, a sample of carbonate salt solution was prepared at a concentration of 0.01 Molar and at 120 degrees Fahrenheit. A carbon dioxide ion selective electrode (previously calibrated at 120 degrees Fahrenheit) was placed in the solution and initial readings were taken for about one hundred seconds. In the first test, an effective amount of citric acid crystals, (0.0067 Molar citrate solution, enough to neutralize all of the carbonate salt solution) were mixed with the carbonate salt solution. The carbon dioxide electrode began to detect carbon dioxide almost immediately after mixture. As illustrated, the carbon dioxide reached a maximum concentration of 0.0082 Molar within about forty five seconds of adding the acid. The carbon dioxide level then began to drop after holding a maximum concentration for about fifteen seconds.
[0039] The previous experiment was repeated using a sample of fumaric acid. An effective amount of fumaric acid was mixed with a sample of carbonate salt solution, which was at a concentration of 0.01 Molar and at 120 degrees Fahrenheit. As shown in the figure, the initial production of carbon dioxide was delayed slightly when compared to the production of carbon dioxide for citric acid. The carbon dioxide reached a maximum concentration of 0.0095 Molar within about 120 seconds of mixing. The carbon dioxide level then began to drop after holding a maximum concentration for about thirty seconds, approximately twice as long as the reaction with citric acid.
[0040] FIG. 2 illustrates a comparison graph showing the response of carbon dioxide production for fumaric and tartaric acid. After approximately 80 seconds of initial readings with the carbon dioxide ion selective electrode, an effective amount of tartaric acid was combined with a sample of carbonate solution at a concentration of 0.01 Molar and at 120 degrees Fahrenheit. A maximum level of carbon dioxide production occurred almost immediately and maxed out at approximately 0.0085 M. With fumaric acid as the acidulent, the carbon dioxide reached a maximum concentration of 0.0095 M within about 120 seconds of adding the acid.
[0041] Tartaric acid is a closer relative to fumaric acid than citric acid. Like fumaric acid, tartaric acid is a diprotic acid with very similar acid strengths for each acidic proton. The main characteristic of these acids is their difference in water solubility. Fumaric acid is about two hundred time less soluble than tartaric acid in water at room temperature.
[0042] Using fumaric acid as the acidulent, the nearly two minute delay in maximum carbon dioxide level production will allow a user to mix the cleaning solution in a single container, with hot water, and cap the container without losing a great deal of carbonation.
[0043] In practice, 227 grams of fumaric acid is admixed to 190 grams of sodium carbonate, and mixed with five gallons of hot water, around 120 degrees Fahrenheit. The amounts of fumaric acid and sodium carbonate may be increased or decreased approximately five to ten grams. Similarly, 252 grams of adipic acid is admixed with 165 grams of sodium carbonate and mixed with five gallons of hot water, around 120 degrees Fahrenheit. The amounts of adipic acid and sodium carbonate may be increased or decreased approximately five to ten grams.
[0044] It is understood that the above-described embodiments are only illustrative of the application of the principles of the present invention. The present invention may be embodied in other specific forms without departing from its spirit or essential characteristics. The described embodiment is to be considered in all respects only as illustrative and not restrictive. The scope of the invention is, therefore, indicated by the appended claim rather than by the foregoing description. All changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
[0045] For example, it is envisioned that other additives commonly found in commercial cleaning compositions may be added without departing from the scope of this invention provided they do not interfere with the interaction of the acids and carbonates and the creation of carbon dioxide. These include, but are not limited to, bleaches, optical brighteners, fillers, fragrances, antiseptics, germicides, dyes, stain blockers, preservatives, and similar materials.
[0046] It is also envisioned that the components (carbonate, acid, and water) of the cleaning composition may be applied to the textile simultaneously, e.g. mixed immediately before application, or during application. In the alternative the components of the cleaning composition may be applied, and thus mixed, in any desired order. For example, a solution of acid can be applied directly on the textile followed by the carbonate solution. Alternatively, the carbonate solution could be sprayed first and then the solution containing the acid. Either procedure works well because solutions with a pH which is not neutral tend to clean much better than those that are neutral.
[0047] Thus, while the present invention has been fully described above with particularity and detail in connection with what is presently deemed to be the most practical and preferred embodiment of the invention, it will be apparent to those of ordinary skill in the art that numerous modifications, including, but not limited to, variations in size, materials, shape, form, function and manner of operation, assembly and use may be made, without departing from the principles and concepts of the invention as set forth in the claims.
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Carpeting, upholstery, drapery and other textile fibers are cleaned by applying to the fibers an aqueous, chemically carbonated cleaning solution prepared by mixing a carbonate salt and a low soluble acid with hot water, such that the low soluble acid delayedly reacts with the carbonate salt to produce carbon dioxide before being applied to the textile fibers. The delayed production of carbon dioxide helps prevent the loss of carbon dioxide before the carbon dioxide is lost. The hot water increases cleaning capability of the cleaning solution.
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FIELD OF THE INVENTION
The present invention relates to a construction panel for use in building walls and roofs.
BACKGROUND OF THE INVENTION
Traditional building construction of wood, concrete and/or steel can be relatively expensive and time-consuming to erect. It is sometimes desirable to quickly erect a building at a minimal cost. One alternative in the prior art are so-called "polytunnels" which are simply fabric covered frames creating a semi-circular enclosed space. Polytunnels are often used as temporary structures to provide protection from the elements but are not usually considered permanent. Polytunnels suffer from further disadvantages in that they do not possess high structural strength, provided limited insulative opportunity and have limited useable space as a result of the semi-circular design.
Therefore, a need exists for a low-cost building alternative to traditional wood, concrete and/or steel structures which has an adequate degree of permanence and structural strength. It would be further advantageous if such an alternative included the use of insulating materials to obviate the need to apply separate insulation and allowed for simple and fast construction.
SUMMARY OF THE INVENTION
In one aspect of the invention, the invention is a construction panel for use in a building structure, the panel having a longitudinal dimension and a lateral dimension and comprising a plurality of sub-panels, each sub-panel having a first end and a second end separated by said longitudinal dimension, and comprising:
(a) a plurality of blocks aligned longitudinally and abutting one another; and
(b) stressing means associated with each sub-panel for maintaining the blocks in longitudinal alignment and for creating a longitudinal compressive force in the sub-panel causing the sub-panel to act monolithically;
wherein the sub-panels are arranged and abut one another laterally, and wherein each sub-panel has a convex outer surface and a convex inner surface, the convexity of said surfaces being apparent when the sub-panel is viewed laterally in cross-section.
In the preferred embodiment of the invention, the stressing means comprises, in association with each sub-panel, an outer cable and an inner cable passing in longitudinal orientation along the outer and inner surfaces respectively of the sub-panel, the cables extending between and being anchored to anchor frames associated with the first and second ends of the sub-panel, and both cables are tightened.
The subpanels preferably interlock with each other; therefore, the subpanels may comprise blocks each comprising a projection member, a body and a channel in the body shaped to receive the projection of a laterally adjacent block whereby each subpanel interlocks with the adjacent subpanel or subpanels. A cable groove may be formed on the outer and inner surfaces of each subpanel, which groove overlaps the projections of one subpanel and the body of the adjacent subpanel such that the stressing means assists in attaching one subpanel to the immediately adjacent subpanel or subpanels.
In another aspect of the invention, the invention comprises a construction panel having a longitudinal dimension and a lateral dimension, and having a first end and a second end separated by said longitudinal dimension, said panel comprising:
(a) a plurality of blocks fitted together to form the panel;
(b) wherein each block is shaped such that the panel, when viewed laterally in cross-section, has a convex outer surface and a convex inner surface;
(c) at least two anchor plates associated with said first and second ends of the panel: and
(d) a plurality of tensioned cables running longitudinally along said outer surface and inner surface;
wherein the panel acts monolithically as a result of a compressive force in the panel created by the tensioned cables and the interlocking blocks.
The blocks may be substantially aligned in longitudinal rows where each row interlocks with the immediately adjacent row or rows and the tensioned cables are located in the area of overlap between two adjacent rows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a view of a preferred embodiment of the invention.
FIG. 2 is a view of a portion of a subpanel of the embodiment of FIG. 1.
FIG. 3 is a view of a block of the subpanel of FIG. 2.
FIG. 4 is a view of a block in an alternative embodiment of the invention.
FIG. 5 is a cross-sectional exploded view of the apex beam and tensioning means of the preferred embodiment.
FIG. 6 is a view of the tensioning plate and hooks.
FIG. 7 is a cross sectional view of an assembled roof panel and wall panel.
FIG. 8 is a cutaway view of the lower roof beam.
FIG. 9 is a view of the roof panel.
FIG. 10 is a view of the end beams of the preferred embodiment.
FIG. 11 is an exploded view of the apex flashing.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is a building construction system which comprises a building panel (10) which is particularly useful in constructing a roof but which may also be used to construct walls. The following description is in reference to a preferred embodiment for a roof panel having the approximate dimensions of 100 feet wide by 30 feet in height. Of course, the invention may be practised on a scale smaller or larger than this with the appropriate variations in all other dimensions.
As shown in FIG. 1, a building frame is constructed of conventional structural members: upright center support posts (12), corner support posts (14), an apex beam (16), end beams (18) and lower roof beams (20). The construction of the frame may be by any known or conventional techniques; the only consideration important to the present invention is that the frame be sufficiently strong to support the entire structure, including the forces created by the tensioned cables as described further below.
In this specification, the term "roof plane" shall mean the plane defined by points A, B and C in FIG. 1. A vertical axis shall mean any axis on the roof plane and parallel to axis A-B. A horizontal axis shall mean any axis on the roof plane and parallel to axis B-C.
The roof panel (10) is comprised of a plurality of sub-panels (22) which are elongated vertically and abut each horizontally. The roof panel (10) is attached to the end beams (18), the lower roof beam (20) and the apex beam (16) in a manner that is further described herein.
In the preferred embodiment and as shown in FIG. 2, each subpanel (22) is comprised of a plurality of blocks (24) aligned and abutting one another along a vertical axis. The blocks (24) are approximately 6 feet square in the preferred embodiment. Each block (24) is individually shaped resulting in the subpanel (22) having a cambered upper surface and a cambered lower surface. The camber follows a line D-E which is substantially normal to a horizontal axis. The degree of camber is illustrated by the thicknesses of the blocks (24); the thickest blocks in the middle may be 18 inches thick while the thinnest blocks at the ends of the subpanel may be 8 inches thick. Such thickness is measured on an axis normal to the roof plane.
The blocks (24) are preferably made of a lightweight, low-density material. Expanded polystyrene is ideal and has the additional advantages of high compressive strength, low water absorption and high thermal resistance.
It is preferable that each subpanel (22) interlock with adjoining subpanels (22) in order to provide additional structural strength to the roof panel (10). As shown in FIGS. 2 and 3, this is accomplished by a series of projections (26) and corresponding channels (28) on the sides of subpanels (22) which abut adjoining subpanels. It is convenient to make each individual block (24) interlock with its neighbour in the adjoining subpanel. As may be obvious, the end subpanels (22) or those which abut the end beams will have only projections or only channels as the case may be.
Although it is possible to attach the blocks to one another with glue or other suitable means, it is unnecessary to do so. In the preferred embodiment, the subpanel (22) is made to act monolithically by means of stressing means (30). The stressing means (30) comprises a series of inner cables (32) and outer cables (34) which run along camber lines on the upper and lower surface of the roof panel (10), tensioning hooks (36) and tensioning plates (38). As shown in FIG. 5, the cables (32, 34) are looped over the hooks (36) which pass through the tensioning plate (38) and attach to the apex beam (16) at one end and the lower roof beam (20) at the other end. In the preferred embodiment, the apex and lower roof beams (16, 20) are manufactured to have angled sides which are perpendicular to the roof plane so that the tensioning plates (38) have a parallel surface to attach to.
The tensioning hooks (36) have a threaded portion which allows the cables (32, 34) to be tightened by tightening a nut (40) threaded onto the hook (36). When tightened, the cables (32, 34) create a force compressing the blocks (24) together. This squeezing of the blocks (24) causes the subpanel (32) to act monolithically despite being comprised of separate blocks.
It is further preferable if the camber lines followed by the cables (32, 34) cross portions of adjoining subpanels (22). Therefore, in the preferred embodiment, the cables run along the roof panel (10) in the zones where one subpanel overlaps with another. Placement of each cable is facilitated by a groove formed in each subpanel along the camber line. The grooves are illustrated in FIG. 2 as following lines D-E and F-G. The roof panel (10) will therefore have a corrugated appearance as shown in FIG. 1.
Each tensioning plate (38), shown in FIG. 6, is approximately 12 feet long which is sufficient to tension two subpanels (22). The cables (32, 34) are preferably wire rope; however, any rope or cable having substantial tensile strength may be used.
FIG. 4 illustrates an alternative embodiment of an individual block. Blocks of this configuration are arranged in a "diamond" configuration where each edge of each block is at 45° to the vertical axis if the block is substantially square. The angle may vary if the block is not square but is more of a parallelogram. In this embodiment, the cable grooves again follow the vertical axis and overlap horizontally adjacent blocks. Other alternative configurations of the blocks and the subpanels may be possible; it is intended that all such alternatives by encompassed by the claims herein.
The subpanels (24) may also be used to form a wall panel (50) as shown in FIG. 7. In that case the cables (32, 34) may run from the apex beam (16) to a lower wall beam (52) with tensioning plates (38) and hooks (36) at both ends. Tensioning plates (38) and hooks (36) will not be necessary along the lower roof beam (20) as long as the inner cables (32) pass through the lower roof beam (20) and the outer cables (34) pass over the lower roof beam (20), as shown in FIG. 8. When the cables (32, 34) are tightened, the lower roof beam (20) will act like a tensioning plate to squeeze the blocks (24) together into a subpanel (22).
In order to weatherproof the roof panel (10), it may be necessary to layer a weatherproof fabric or sheet (60) over the panel (10), as shown in FIG. 9. Such a sheet (60) may be held in place by the outer cables (34). In the preferred embodiment, polyethylene sheeting is used. Alternatively, any fabric that is weatherproof and has high resistance to tearing will work.
The preferred embodiment of the invention is assembled using the following method. The groundwork is prepared and levelled in a conventional fashion on the chosen site. A suitable foundation (70) is laid and vertical supports (12, 14) are bolted or set into the foundation (70) to bear the load of the finished structure and any anticipated external forces such as wind and snow accumulation. The vertical supports (12, 14) may be braced as necessary. The apex beam (16), the end beams (18) and the lower roof (20) and wall beams (56) are then secured to the vertical supports (12, 14) to finish the building frame.
Once the building frame is complete, the tensioning plates (28) are affixed to the beams (16, 20) along with the lower tensioning hooks (36). All of the inner tensioning cables (32) are then laid and are tightened somewhat but not fully. The interlocking subpanels (22) may then be laid across the inner cables (32) to form the roof panel (10). The gap between the subpanels (22) and the lower roof beam (20) is covered by flashing preferably made of galvanized sheet metal (not shown).
Next, the fabric sheet (60) is laid across the roof panel (10) and secured along its horizontal edges to the end beams (18). The sheet (60) may be secured to the end beams (18) by an angled bar (62) which is used to sandwich the sheet (60) to the end beam (18), as shown in FIG. 10. The upper and lower edges of the sheet (60) need not be secured as the tightened outer cables (34) will securely keep the sheet (60) in place. Once the fabric sheet is in place, the outer tensioning cables and hooks may be attached to the tensioning plates and roof beams. The inner and outer cables are then tensioned simultaneously.
Once the roof panel (10) is completely formed, the last step is to weatherproof the apex of the roof by using galvanized sheet metal flashing as illustrated in FIG. 11. Flashing (80) shaped to conform to the corrugations of the roof panel (10) are attached to the apex beam (16) to bear down snugly on the sheet (60). A top piece (82) is then used to cover the apex beam (16) and the corrugated flashing (80).
Variations and modifications of the disclosed preferred embodiment and alternative embodiments will be apparent to skilled practitioners. All such variations and modifications are intended to be encompassed by the claims set forth herein.
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A construction panel is formed of a plurality of elongate subpanels where each subpanel comprises a plurality of expanded polystyrene blocks placed end to end. Tensioning cables pass over the inner and outer surfaces of the subpanels between tensioning plates positioned at each end of the subpanels. Tensioning the cables imparts longitudinal compression in the subpanels, such that the blocks of the subpanels act monolithically. The inner and outer surfaces of the subpanels are longitudinally convex. The panel may be corrugated. The subpanels may be interlocking to form the construction panel.
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This is a division of copending application Ser. No. 413,576, filed Aug. 31, 1982, now U.S. Pat. No. 4,517,128.
CROSS REFERENCE TO RELATED APPLICATIONS
Copending U.S. patent application Ser. No. 413,591, filed Aug. 31, 1982, now U.S. Pat. No. 4,446,079, in the name of D. H. Hoskin describes low cost, brine tolerant surfactants including, inter alia, 1,3-dialkoxy-2-propoxypolyethoxypropane sulfonates for enhanced oil recovery.
Copending U.S. patent application Ser. No. 373,550, filed Apr. 30, 1982, now U.S. Pat. No. 4,468,335, in the name of Catherine S. H. Chen and Albert L. Williams describes (branched alkyl)-polyethoxypropane sulfonates and their use in enhanced oil recovery. This Chen et al application is a continuation-in-part of U.S. patent applications Ser. No. 259,215 and Ser. No. 259,216, both filed Apr. 30, 1981, and both now abandoned.
Copending U.S. patent application Ser. No. 259,218, filed Apr. 30, 1981, now U.S. Pat. No. 4,442,042, in the name of Kirk D. Schmitt discloses a method for preparing alkylpolyethoxypropane sulfonates. This Schmitt application is, in turn, related to U.S. application Ser. No. 96,947, filed Nov. 23, 1979, in the name of Catherine S. H. Chen, Kirk D. Schmitt and Albert L. Williams, entitled Method of Making Propane Sulfonates, now U.S. Pat. No. 4,267,123.
The above-mentioned U.S. patent applications and U.S. patents are expressly incorporated herein by reference.
BACKGROUND
This invention is directed to (branched alkyl)-polyethoxyalkyl sulfonates and similar sulfate compounds having an aromatic group on one of the branches of the branched alkyl group, a process for their preparation and a process for their use in enhancing the secondary or tertiary recovery of oil from subterranean oil deposits or reservoirs, particularly from high salinity reservoirs. In particular, these compounds are suitable as single component surfactants in continuous chemical flooding techniques.
In the recovery of oil from oil bearing deposits it is generally possible to recover only a portion of the original oil by so called "primary methods" which utilize only the natural forces present in the reservoir or deposit. Thus a variety of supplemental techniques have been employed in order to increase the recovery of oil from these subterranean reservoirs. The most widely used supplemental recovery technique is water flooding which involves injection of water into an oil bearing reservoir. However, there are problems associated with the water flooding technique and water soluble surfactants have generally been required to be used for this process to be completely successful. Thus the LTWF (Low Tension Water Flood) method using surfactants which function in low salinity (less then 3 percent) is well known. However, it has been found that preflushing the reservoirs with fresh or low salinity water to reduce the salinity so that the low salinity surfactants of the prior art may be used is not always effective, or, the preflushing is effective only for a short duration and the salinity of the fresh water increases over a period of time since it is in contact with reservoir rocks and clays. Either event renders the low salinity surfactants useless and therefore it is of vital importance to have a surfactant which functions at the salinity of the connant water to negate the necessity of preflushing.
Developments for using surfactants to enhance oil recovery may be categorized according to essentially two different concepts. In the first, a solution containing a low concentration of surfactants is injected into the reservoir. The surfactant is dissolved or dispersed in either water or oil. Large pore volumes (about 15-60% or more) of the liquid are injected into the reservoir to reduce interfacial tension between oil and water and thereby increase oil recovery. Specific relationships exist between interfacial tensions of the oil against the flooding media and the percentage recovery obtained by flooding, i.e., the efficiency of flooding increases as the interfacial tension decreases. Oil may be banked with the surfactant solution process but residual oil saturation at a given position in the reservoir will only approach zero after passage of large volumes of this flooding media.
In the second process, a relatively small pore volume (about 3-20%) of a higher concentration surfactant liquid is injected into the reservoir. The high concentration surfactant liquids displace both oil and water and readily displace all the oil contacted in the reservoir. As the high concentration slug moves in the reservoir, it is diluted by formation flood and the process reverts to a low concentration flood; Enhanced Oil Recovery, Van Poolen & Associates, 1980, Tulsa Okla.
Aqueous surfactant liquids for injecting into reservoirs contain two essential components, namely, water and surfactant. An optional third component may be a hydrocarbon. Such three component mixtures of water, surfactant and hydrocarbon may be in the form of a water-external micellar dispersion as discussed in the Jones U.S. Pat. No. 3,506,071. A cosurfactant fourth component (usually alcohol) can be added. Electrolytes, normally inorganic salts, form a fifth component that may be used.
Work is still in progress in the laboratory and in the field to select the optimum method of injecting surfactant to improve oil recovery. The best process for a specific reservoir is the one which has the potential to provide the greatest efficiency and yield regardless of the concentration level of the surfactant. The chemical system, however, to be efficient must be tailored to the specific reservoir.
The prior art with respect to the use of surfactant polymer floods to recover oil from reservoirs has disclosed that for a given amount of surfactant, a small slug process with a high surfactant concentration is more efficient than a large slug process with a low surfactant concentration. The former produces oil earlier and takes a smaller number of pore volumes to complete oil production. This is a favorable condition. However, it has become evident that fluid dispersion and mixing take place in the reservoirs and the slug intake routine cannot be maintained. Deterioration of the surfactant and the mobility control slug can lead to process failure or at least a reduction in process efficiency. For heterogeneous reservoirs where fluid dispersion and mixing takes place to a greater extent it is desirable if not vital to have a continuous flooding process with a surfactant which can move oil even at very low concentrations.
There has now been discovered certain novel surfactants and their use in a continuous flooding process wherein low concentrations of the novel surfactant alone can be used to increase the oil production during secondary water flooding processes or to recover residual tertiary oil where the reservoirs already have been water flooded.
SUMMARY
The present invention relates to novel surfactants which are (branched alkyl)-polyethoxyalkyl sulfonates, and similar sulfate compounds wherein the alkyl sulfonate moiety is replaced by a sulfate moiety, having an aromatic group on one of the branches of the branched alkyl group, processes for their preparation and processes for their use, particularly at low concentrations in enhanced oil recovery. The enhanced oil recovery process is especially adaptable to high salinity reservoirs, e.g., reservoirs having a salinity of from about 4 to 30%.
This surfactant, in amount effective for the intended purpose can be used as a single component surfactant without the addition of any other component or cosurfactant. However, it may be desirable to use mixtures of two or more of the branched surfactants described herein, or to use the surfactant in combination with a sacrificial agent such as lignin sulfonate.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing interfacial tension against crude oil as a function of brine concentration for various two-tailed surfactants.
FIGS. 2 and 3 are graphs showing cumulative oil recovery vs pore volume of injected surfactant slug.
DETAILED DESCRIPTION
The surfactants of this invention may have the formula: ##STR1## where: (i) n and m are from 0 to 3;
(ii) y is from 0 to 5, preferably from 0 to 3, most especially 3;
(iii) x is a rational number (e.g. including fractions) from 2 to 8;
(iv) R 1 is C 4 -C 10 alkyl;
(v) Ar is substituted or unsubstituted phenyl; and
(vi) M is a cation.
Particular examples of Ar when Ar is substituted phenyl include paramethylphenyl and para-tert.-butylphenyl.
It is noted that, when y is 0, the surfactant may be characterized as a sulfate compound, and, when y is 1 or greater, the surfactant may be characterized as an alkyl sulfonate compound.
M is preferably a monovalent cation. Examples of such monovalent cations include ions of alkali metals and nitrogeneous bases. Where M is an alkali metal ion, it may be sodium or potassium. Various nitrogeneous bases, including ammonium or quaternary amines, may be employed. Representative alkylammonium ions include methylammonium, ethylammonium, and normal or isopropylammonium ions, and examples of alkanolammonium ions include monoethanolammonium and triethanolammonium ions.
Sulfonates of this invention can be prepared by methods which in themselves are known in the art. One such method involves the reaction of an alkali metal salt of a (branched alkyl) polyethoxy alcohol with propane sultone. This route provides a convenient laboratory synthesis and gives high yields but is not desirable on a large scale for several reasons. Foremost among them are the facts that (1) such a reaction requires multistep synthesis and purification of propane sultone (2) propane sultone is expensive to purify and its overall yield of 80-90% limits the yield in the preparation of propane sulfonates and (3) propane sultone is a known carcinogen. Therefore, processes involving the use of propane sultone must utilize expensive controls to minimize worker exposure but despite such controls its use will always engender some risk.
An alternative method of synthesis which has potential advantages on a commercial scale without the use of propane sultone can be conducted in accordance with the following reaction sequence. ##STR2## and R 1 , R 2 and x are as defined above and X is halogen or aryl sulfonate (e.g., tosylate).
Where R is such that the allyl ether product of reaction (I) has a solubility in water of less than 0.5% the process can be conducted in two steps in a single reactor without isolation of intermediates in almost 100% yield by control of reaction conditions in steps (I) and (II). Step (I) can be carried out in a completely aqueous system if about 50% NaOH is used as the base and if close contact between the water insoluble allyl halide and alcohol is brought about by inclusion of a certain minimum amount of desired sulfonate final product in the reaction vessel. The initial portion of desired sulfonate final product may be prepared by any suitable conventional route such as e.g., the propane sultone route discussed previously. At the end of the reaction any excess allyl chloride is easily distilled from the reactor. It need not be dried but may be recycled directly, nor must it be separated from an organic solvent since no organic solvent is used.
The preparation of allyl ethers by the reaction of sodium or sodium methoxide with the alcohol followed by reaction with allyl chloride all in an organic solvent such as toluene or tetrahydrofuran (the Williamson ether synthesis) is well known and may be found in many standard textbooks on organic chemistry.
The reaction of NaHSO 3 with simple olefins, step (II), has been much studied. The literature teaches that for simple water-soluble olefins or olefins which can be made soluble by the addition of small amounts of alcohols, all that is required for high conversions to the desired products are conditions in which all reagents are dissolved in a single phase.
In the present method of preparation the (branched alkyl) polyethoxy allyl ethers do not behave this way. Conditions may be found in which all the reagents are dissolved in a single phase in alcohol and water and yet conversion will not exceed 40 or 50%. However, when a minor amount of propane sulfonate product is present in the reaction medium the conversion may be as high as 90% or more. Accordingly, it is advantageous to recycle part of the branched alkoxyalkylpolyethoxypropane sulfonate final product of the reaction so that it is present during reaction. In general, the propane sulfonate product is present in a molar ratio of 1:1 to about 1:10 based on the allyl ether.
In Examples 1-6 which follow, there is described the preparation of four surfactants. Examples 1-5 describe the preparation of various intermediates. More particularly, Examples 1-4 describe the preparation of various alcohols, and Example 5 describes the preparation of tetrahydropyran ether of 2-[2-(2-chloroethoxy)ethoxy]ethanol. Example 6 describes the preparation of four surfactants using the intermediates of Examples 1-5.
EXAMPLE 1
Synthesis of 2-benzyl-1-heptanol
Hydrogenation of 40 g -pentylcinnamaldehyde (Pfaltz and Bauer, Inc.) at 40 psig H 2 in 160 ml ethanol over 2 g 10% Pd/C for 30 min. followed by filtering, stripping and fractional distillation yielded 31 g pale yellow oil bp 115-125/0.2 mm which showed a single peak on a 2'×1/4" 10% SE-30 GC column temperature programmed from 150° to 270° at 6°/min. Carbon-13 NMR was consistent with the assigned structure. ##STR3##
EXAMPLE 2
Synthesis of 2-benzyl-1-nonanol
The alcohol was prepared by hydrogenation of a-heptylcinnamaldehyde exactly as in Example 1. -Heptylcinnamaldehyde was prepared as follows: To a mixture of 53.8 g (0.50 mole) benzaldehyde 50 ml ethanol and 25 ml 10% NaOH at reflux were added 56.8 g (0.40 mole) nonanal dropwise over 20 min. Halfway through the addition of nonanal an additional 25 ml 10% NaOH were added. After two hours at reflux the mixture was cooled, diluted with 100 ml 30°-60° petroleum ether, washed once with 50 ml 5% HCl, once with saturated NaCl brine, filtered through 4A molecular sieves, stripped and fractionally distilled, bp 135°-150°/0.15 mm, to give 56.1 g (61%) whose IR showed aromatic CH stretch from 3000-3100 cm -1 , aldehyde CH at 2705 cm -1 , and an aldehyde C=0 at 1706 cm -1 .
EXAMPLE 3
Synthesis of 1-phenyl-2-decanol
Glassware was dried overnight at 110°, assembled hot under argon, and thoroughly degassed via three cycles of a Firestone valve before use. All reagent transfers were carried out using double ended needle techniques (See, for example, "Organic Synthesis via Boranes", H. C. Brown, Wiley Interscience, N.Y., N.Y., 1975, page 210).
Thus, to 500 ml 1.4 molar benzyl magnesium chloride in THF (Alpha Inorganics) were added 94.6 g nonanal dropwise, with ice cooling, over 1 hour, the mixture kept 1 hour at room temperature, quenched with 20 ml saturated NaCl brine and 500 ml 5% HCl, stripped, and 500 ml diethyl ether added. The organic phase was washed once with 100 ml H 2 O, once wih 200 ml saturated NaCl brine, filtered through 4A molecular sieve, stripped and fractionally distilled to give 122.1 g (78%) water white product bp 111°-113°/0.2 mm whose gas chromatograph on a 10% SP-2100 column programmed from 170° to 270° at 8°/min showed a single peak at 430 sec.
EXAMPLE 4
7-Hydroxymethylpentadecane
For the purposes of comparison, the above 7-Hydroxymethylpentadecane compound was obtained commercially from Pfaltz and Bauer.
EXAMPLE 5
Tetrahydropyran Ether of 2-[2-(2-chloroethoxy)ethoxy]ethanol
The chloroalcohol was freshly distilled from K 2 CO 3 before use because it contained enough HCl to lead to spontaneous exothermic reaction when mixed with dihydropyran. The alcohol (1.5 mole) and dihydropyran (3.0 mole) were mixed in a 3 l E flask, 2.9 l CH 2 Cl 2 added followed by 20 g 4A molecular sieves and 0.18 mole pyridinium p-toluenesulfonate. After stirring overnight the reaction was washed once with 200 ml 50% K 2 CO 3 , filtered, washed once with 200 ml 50% K 2 CO 3 , once with 100 ml saturated NaCl, filtered through 4A sieves and distilled. HPLC confirmed the crude product contained 3% alcohol. The yield was 92% of material bp 70°-80°/1.5 mm Hg.
EXAMPLE 6
Addition of Sodium Triethyleneoxypropane Sulfonate Group to Alcohols
A mixture of 350 ml xylene and 0.500 mole of each of the alcohols of Examples 1-4 was degassed via three cycles of a Firestone valve, refluxed to dryness through a Dean-Stark trap, cooled to 15° in ice and 325 ml 1.6M butyllithium in hexane (Aldrich Chemical Co.) added in 20 minutes followed by 125 ml of the tetrahydropyranyl ether of 2-[2-(2-chloroethoxy)ethoxy]ethanol (Example 5). The hexane was distilled through a Claisen head until the overhead reached 128° then refluxed overnight, cooled to room temperature, quenched with 175 ml saturated NaCl brine plus 80 ml H 2 O, diluted with ether and the phases separated. The organic phase was washed twice with 60 ml H 2 O, once with 175 ml saturated NaCl brine, filtered through 4A molecular sieves and stripped. The residue was dissolved in 700 ml ethanol, 37 g pyridinium p-toluenesulfonate (J. T. Baker Chem. Co.) added, the mixture refluxed 4 hours, cooled, neutralized with 12 g potassium hydroxide in 35 ml H 2 O, stripped, partitioned between 750 ml ether and 200 ml H 2 O. The ether layer was washed once with 90 ml saturated NaCl brine, filtered through 4A molecular sieves, stripped, rapidly distilled on a Kugelrohr then fractionally redistilled. The yield of triethoxylated alcohol at this point ranged from 0.18-0.25 mole (36-50%). The alcohol was dissolved in 4 volumes toluene, degassed via three cycles of a Firestone valve, refluxed to dryness through a Dean-Stack trap, metallic sodium (96% of theory.) added over 10-20 min, reflux, continued until all the sodium dissolved, the mixture cooled to room temperature, then freshly distilled propane sultone (Aldrich Chemical Co. or Eastman) added in 20 min. After 1 hour at room temperature the solvent was removed in vacuo and the product recrystallized once from an acetone/methanol mixture to give 0.11-0.15 mole final product. Carbon-13 NMR peaks characteristic of the sodium triethyleneoxypropane sulfonate group were invariably found as follows: ##STR4##
The four surfactants prepared according to the foregoing Examples may be represented as follows: ##STR5##
EXAMPLE 7
Measurements of Interfacial Tensions
The above represented compounds 2-4 each have a total number of 16 carbon atoms in the hydrophobic tail.
Interfacial tensions (IFT) against West Burkburnett crude oil were measured for 0.1% solutions of each of the surfactants in a synthetic brine containing NaCl, MgCl 2 , and CaCl 2 in weight ratio 18.3:1:3.63 with total dissolved solids content expressed as "% brine". The spinning drop technique [J. L. Cayias, R. S. Schecter, W. H. Wade; Adsorption at Interfaces, Symposium Ser. #8, ACS, 234 (1975)] was used to measure IFT.
Table 1 and FIG. 1 show the results for the three sixteen carbon hydrophobe surfactants and fourteen carbon hydrophobe surfactants of Example 6. It is evident that a two-tailed surfactant is much more brine tolerant, for the same hydrophilic head, if one of the tails incorporates an aromatic group than if both tails are aliphatic.
TABLE 1______________________________________Interfacial Tension at Different SalinitiesIFT Against Crude Oil, mdyne/cm% Brine Surfactant.sup.(a) 1 2 3 4______________________________________30 4.328 0.424 24 14 1622 4 420 2.9 418 7.8 816.6 17 1214 41 4112 6310 268 76 54 322 44______________________________________ .sup.(a) Surfactant Concentration = 0.1%
EXAMPLE 8
Measurement of Interfacial Tension
To show probable efficacy for oil recovery at very low concentrations, such as stripping type enhanced oil recovery process, the IFT against crude oil was measured at 100 ppm surfactant concentration (Table 2). IFT's of 10 mdyne/cm or less are easily achieved over a broad range of concentrations. Since it is generally agreed [L. M. Prince; "Microemulsions", Academic Press, New York, 1977, pg 153] that IFT's of 10 mdyne/cm or less are sufficient to mobilize substantial amounts of oil from reservoir rocks, it is evident that injection of low concentrations of these surfactants will increase oil recovery.
TABLE 2______________________________________Interfacial Tension Against Oil at Different SalinitiesIFT, mdyne/cm% Brine Surfactant.sup.(a) 1 2 3______________________________________30 2.828 5.524 28 59 5822 6.5 6.420 3.3 2.718 6.0 1.616.6 11 7.914 29 29______________________________________ .sup.(a) Surfactant Concentration = 100 ppm
EXAMPLE 9
Measurement of Interfacial Tension
An alternative way to measure the lowering of IFT between oil and water is to measure the amount of oil solubilized into a middle phase when oil and water are equilibrated in contact with one another. Solubilization is defined as the volume of oil in the middle phase divided by the volume of surfactant in the middle phase. Equal volumes of crude oil and surfactant solution were shaken and allowed to equilibrate at least one month (Table 3).
TABLE 3______________________________________Solubilization by Surfactant 2% Brine % 2-BuOH Solubilization at 25° C. 50° C.______________________________________21 0 0 018 0 5.1 2315 0 2.8 9.412 0 1.4 9.421 1 0.5 018 1 2.8 2315 1 .9 1512 1 2.3 5.621 2 0.5 018 2 23 1.915 2 3.3 812 2 1.9 22______________________________________
Solubilization in excess of 5 is considered sufficient to mobilize substantial oil from reservoir rocks. Table 3 indicates that solubilizations greater than 5 exist for a wide range of surfactant/alcohol/brine compositions. Solubilizations for surfactant 2 at 12 and 15% brine at 50° and at 18% brine at 25° exceed 5 at all alcohol concentrations indicating that the surfactant's ability to mobilize oil in a slug process will not be jeopardized by chromatographic separation of alcohol and surfactant.
The exact concentration and temperature at which high solubilizations are obtained can be altered by methods known in the art, namely, varying the number of ethyleneoxy groups or the length of the alkyl chain.
EXAMPLE 10
Oil Recovery
To demonstrate the ability of surfactants of the present invention to recover oil from reservoir rock a 1" by 12" core of 600 m Darcy Berea sandstone was flooded at 25° C. to residual oil content with 18% brine. A 0.20 pore volume slug containing 5% of surfactant 2 and 3% 2-BuOH in 18% brine was injected followed by continuous injection of 18% brine. Thirty percent of the residual oil was produced within one pore volume of the start of injection. The pressure increased 1.5 psig indicating no deleterious viscous phases were formed. The cumulative production of oil as a function of pore volumes of injected fluid is depicted in FIG. 2.
EXAMPLE 11
Oil Recovery
It is known [L. A. Wilson, Jr.; in "Improved Oil Recovery by Surfactant and Polymer Flooding", D. O. Shah and R. S. Schechter, ed., Academic Press, 1976, pg 3] that injection of a thickened water slug following a surfactant slug increases the oil recovery efficiency of the surfactant slug. To demonstrate the compatibility of surfactants of the present invention with this process, a 1" by 12" 600 m Darcy Berea sandstone core was flooded to residual oil saturation at 50° C. with 15% brine. A 0.17 pore volume slug containing 5% of surfactant 2 and 1.5% 2-BuOH (28 cp) was injected followed by continuous injection of a 300 ppm solution of Polytran [Obtained from Jetco Chemicals, Corsicana, Tex. as "Actigum CS-11-L"] in 10% brine (11 cp). FIG. 3 shows the cumulative production of residual oil as a function of pore volumes of fluid injected. The residual oil recovery was increased from 30% at one pore volume in Example 10 to 50% with 66% of the residual oil recovered by two pore volumes.
The compounds of the present invention are felt to be novel surfactants with extreme salt and divalent ion tolerance which produce low IFT against oil over a wide range of temperatures, salt concentrations, and alcohol concentrations. These properties make these compounds suitable for use in many types of chemical waterflooding oil recovery processes contemplated in the literature. They are effective in high concentration slugs with and without alcohol or petroleum sulfonate cosurfactants, with and without polymeric water thickeners, and with and without sacrificial chemicals such as lignosulfonates [Note G. Kalfoglou, U.S. Pat. No. 4,157,115, June 5, 1979].
High concentration slugs of these surfactants with or without added alcohol are moderately viscous which, in itself, is considered beneficial to oil recovery [W. B. Gogarty and J. A. Davis, Jr. SPE Paper No. 3806, Apr. 16-19, 1972].
Very low concentrations of these surfactants have IFT against oil low enough to indicate they will effectively recover oil when injected in a continuous fashion in concentrations from 10 to 500 ppm.
The compounds of the present invention can be synthesized easily and inexpensively by methods well known in the art.
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(Branched alkyl)-polyethoxyalkyl sulfonates, and similar compounds wherein the alkyl sulfonate moiety is replaced by a sulfate moiety, having an aromatic group on one of the branches of the branched alkyl group are provided. These compounds are surfactants which are particularly useful for chemical waterflooding, especially in high brine environments.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention includes a method of manufacturing single-walled carbon nanotubes by promoting self-assembly of single crystals of single-walled carbon nanotubes using field enhanced thermolysis of nano-patterned precursors. With the disclosed method a higher ordering degree of the grown nanotubes than with known methods can be achieved while the synthesis of these highly ordered single crystals of single-walled carbon nanotubes results in extended structures with length dimensions on the micron scale. They are formed from nanotubes that have identical diameter and chirality within each crystal but which may differ between the crystals. With the proposed method single-walled carbon nanotubes can be produced as a highly ordered bulk material on the micron scale which is a first step for the synthesis of bulk macroscopic crystalline material. The invention hence represents a significant advance in the synthesis of crystals containing a high number of well-aligned ordered single-walled carbon nanotubes all of which are physically identical in nature.
2. Description of the Related Art
Carbon nanotubes have been the subject of intense research since their discovery in 1991. One of the most desirable aims of carbon nanotube fabrication is to form large uniform and ordered nano- and microstructures and eventually bulk materials.
The potential applications of single-walled carbon nanotubes range from structural materials with extraordinary mechanical properties down to nanoelectronic components with a potential to circumvent Moore's Law. Single-walled carbon nanotubes can act as ultimate probe tips for scanned probe microscopy with the added ability to chemically functionalize the apex. These nanostructures are also usable for forming microbalances, gas detectors or even energy storage devices. Likewise the use of single-walled carbon nanotubes in the field emission mode for displays or as electrodes for organic light emitting diodes or for electron beam sources in lithography and microscopy are of clear future technological significance.
The growth of single-walled carbon nanotubes traditionally uses harsh conditions such as laser ablation of carbon rods or a direct current arc discharge between carbon electrodes in an inert gas environment, such as described in “Fullerene Nanotubes: C 1,000,000 and Beyond”, Yakobson and Smalley, American Scientist, Vol. 85, No. 4, July-August 1997, pp. 324-337. For both methods the addition of a small quantity of metal catalyst like Co, Ni, Fe, or Mo increases the yield of single-walled carbon nanotubes. To date the resulting material consists however only of an entangled and poorly ordered mat of single-walled carbon nanotubes although each nanotube can be several hundreds of microns long. Furthermore, a wide variation in structures referred to as the zigzag, armchair or chiral forms coexist within the material. U.S. Pat. No. 5,424,054 presents a method for manufacturing hollow fibers having a cylindrical wall comprising a single layer of carbon atoms, but also here the produced fibers have no controlled orientation.
In a recent article “Carbon rings and cages in the growth of single-walled carbon nanotubes” by Ching-Hwa Kiang, Journal of Chemical Physics, Vol. 113, No. 11, 15 September 2000, a growth model for single-walled carbon nanotubes is presented based on an analysis of the experimental results of arc- and laser-grown single-walled carbon nanotubes.
In “Growth of a single freestanding multiwall carbon nanotube on each nanonickel dot”, by Ren et al. in Applied Physics Letters, Vol 75, No. 8, 23. August 1999, pp. 1086-1088, the use of chemical vapor deposition in combination with nanofabricated catalytic patterning or templating has been used to direct the growth of individual single-walled carbon nanotubes on substrates. However, ordered arrays beyond short sections of ordered single-walled carbon nanotubes of tens of nanotubes have not been produced. Likewise, chirality and diameter are not controllable which for many applications is of paramount importance because the physical properties of the nanotubes such as electrical conductivity are extremely structure-sensitive.
SUMMARY OF THE INVENTION
According to a first aspect of the invention there is provided a method of manufacturing single-walled carbon nanotubes comprising the steps of providing on a substrate at least one pillar comprising alternate layers of a first precursor material comprising fullerene molecules and a second precursor material comprising a catalyst, and heating the at least one pillar in the presence of a first magnetic, electromagnetic or electric field. During the heating, crystals comprising single-walled carbon nanotubes grow. The crystal growth direction is determined by the direction of the applied field. The precursor materials can be provided by thermal evaporation. As the fullerene molecules C 60 or C 82 molecules can be preferably used.
It proves an advantageous choice to provide the pillars to have between 5 and 10 layers of the precursor materials deposited upon each other. Each layer may have a thickness between 5 and 30 nm.
The precursor materials can be deposited through a shadow mask comprising one or more apertures. Such a shadow mask has the advantage to be suited for not only providing an aperture for creating one pillar, but with such a shadow mask a large number of such pillars can be fabricated in parallel. Furthermore the fabrication of the apertures in the shadow mask can be done in parallel as well, e.g. by a lithography process.
The substrate can be selected to comprise thermally oxidized silicon or molybdenum in the form of a grid or as a solid film provided on a silicon wafer. The substrate can also be selected to have a rough faceted surface such that it offers crystallization sites, i.e. seed locations from where the crystals respectively the nanotubes can grow.
The substrate ideally is selected to have a surface structure that helps the pillars to stay confined also during the heating step. It is found that the better the confinement of the pillars on the surface, the higher the yield in precisely aligned crystals. The substrate is optimally selected, to not, or only to a negligible extent, participate in the chemical reaction that takes place during the heating step. It is further preferable to have the property to effectively keep the pillars confined thereon. A diffusion of the pillar structure on the surface reduces the yield. Molybdenum or silicon dioxide have been found to be materials for the substrate that meet with both of the above criteria. Particularly molybdenum is found to offer through its surface structure numerous crystallization sites. Instead of a bulk substrate, any layered structure comprising different materials can be used. For the manufacturing method, the upmost layer is the one that influences the process and which herein is referred to as the substrate.
The evaporation of the precursor materials can be performed at a pressure of around 10 −9 Torr, while the substrate can be kept at room temperature. The evaporation can be controlled by using an electromechanical shutter and an in situ balance for monitoring the deposition rate of the precursor materials. The evaporation can be controlled such that the thickness of the layers decreases with their distance from the substrate. This decreasing thickness again increases the yield and it is believed that the reduction in thickness directly leads to the effect that less of the catalyst is transported towards the tip of the growing crystal. Furthermore the evaporation of a catalyst like Ni is technically not so easy which makes it desirable to utilize only the minimum necessary amount for the manufacturing process. Hence the amount of catalyst material can be reduced by the thinner layers. Since it is also believed that the growth of the crystal begins at the base of the pillar, less material transport form the layers which are remote from the substrate is performed with the layers with reduced thickness.
The heating can be performed up to a temperature of essentially 950° C. in a vacuum of essentially 10 −6 Torr or in an essentially inert gas atmosphere, for a time between 3 minutes and an hour. Thereby better results are obtained. A heating time in the minute range is in principle seen sufficient which means that a longer heating does not significantly improve the result.
In the case of applying the first magnetic field, this magnetic field can be oriented essentially normal to the surface of the substrate during heating, such that the growing nanotubes follow the applied field and grow perpendicularly to the substrate surface as well. This field can be concentrated onto the at least one pillar being heated. This proves advantageous, when the heating source is constructed in a way that counteracts the applied field. Since at 950° C. the Curie temperature of a magnet is exceeded, the magnetic field in that heated area would be destroyed. Keeping the magnet away from the heat source such that the heat does not harm the magnet, but directing the field to the pillars allows to keep the magnetic field effective in the pillar area. In the case of growing more than one pillar, the first magnetic field can be applied in a different orientation onto different of the pillars, thereby effecting different crystals growing into different, but controlled, directions. Even crystal intersections can be achieved in this way. After the heating has led to the growth of the single-walled carbon nanotubes, these can be thermally annealed in the presence of a second magnetic field. During this process step, the crystal direction is again determined by the direction of the applied field. When the direction of the second magnetic field differs from the direction of the first magnetic field, the crystal is redirected into the new direction determined by the second applied field.
In the case of applying an electrical field, this electrical field can be directed essentially parallel to the substrate surface in order to have the nanotubes grow orthogonally to the substrate surface.
According to another aspect of the invention a precursor arrangement for manufacturing single-walled carbon nanotubes is provided, which comprises on a substrate at least one pillar comprising alternate layers of a first precursor material comprising fullerene molecules and a second precursor material comprising a catalyst. The layers may have a thickness that decreases with their distance from the substrate. The substrate may comprise thermally oxidized silicon or molybdenum in the form of a grid or as a solid film provided on a silicon wafer. The catalyst may comprise a magnetic material, preferably a metal being selected from the group Ni, Co, Fe, Mo.
According to another aspect of the invention a nanotube arrangement is proposed comprising a substrate and thereupon at least one crystal comprising a bundle of single-walled carbon nanotubes with identical orientation and structure. The nanotube arrangement can be integrated in a display, electrical circuit, switching element or sensor element.
A further aspect of the invention is to provide a nanotube crystal comprising a bundle of straight single-walled carbon nanotubes with essentially identical orientation and structure.
DESCRIPTION OF THE DRAWINGS
Examples of the invention are depicted in the drawings and described in detail below by way of example. It is shown in
FIG. 1 a schematic view of an apparatus for manufacturing single-wall carbon nanotubes in an evaporation step,
FIG. 2 a schematic view of an apparatus for manufacturing single-wall carbon nanotubes in a heating step,
FIG. 3 a schematic view of a single pillar as precursor structure for manufacturing single-wall carbon nanotubes,
FIG. 4 a scanning electron microscope (SEM) micrograph of a crystal containing a bundle of single-wall carbon nanotubes,
FIG. 4 b a magnified portion of the SEM micrograph of FIG. 2 a,
FIG. 4 c a schematic view of a bundle of single-wall carbon nanotubes,
FIG. 5 scanning electron microscope (SEM) micrograph of a typical structure produced by the described method
FIG. 6 an electron diffraction pattern from bundle with single-walled carbon nanotubes.
All the figures are for sake of clarity not shown in real dimensions, nor are the relations between the dimensions shown in a realistic scale.
DETAILED DESCRIPTION OF THE INVENTION
In the following, the various exemplary embodiments of the invention are described.
Crystals of single-walled carbon nanotubes are produced using a method involving nanoscale patterning of solid-state precursor materials. Controlled mixtures of fullerenes, here C 60 molecules and Nickel as catalyst are evaporated through nanometer-scale apertures of a patterned evaporation mask onto a molybdenum substrate. The resulting structures are then thermolysed under vacuum in the presence of a magnetic field. A combination of electron diffraction studies and electron energy loss spectroscopy (EELS) confirms that the produced structures are almost perfect rod-like crystals of single-walled carbon nanotubes oriented normal to the surface of the substrate.
In FIG. 1 a first schematic view of an apparatus for manufacturing single-wall carbon nanotubes is depicted.
A reaction chamber 1 comprises four openings, one being penetrated by a sample-holder 9 for holding a substrate 4 and a patterned evaporation mask 7 , also referred to as shadow mask, the second opening being penetrated by a first tool support 11 , the third opening being penetrated by a second tool support 12 . The fourth opening is provided with a hose 13 for evacuating the reaction chamber 1 and/or filling in some gas, such as an inert gas like Argon. Inert gases are suitable for avoiding the boiling of carbon dioxide from the carbon material provided. The first tool support 11 holds an oscillating quartz 6 serving as a microbalance for controlling the thickness of a deposited layer. The second tool support 12 holds an evaporation source 10 . During operation the evaporation source 10 is emitting material through apertures 14 in the patterned evaporation mask 7 towards the substrate 4 . The evaporation source serves for evaporating here two precursor materials 15 , 16 . Thereof a first precursor material 15 is a fullerene and a second precursor material 16 is a catalyst. The precursor materials 15 , 16 may also comprise additional substances, as long as the crystal growth is achievable.
The evaporation is performed in a way that alternate layers of the precursor materials 15 , 16 are deposited on the substrate 4 . Therefor either the evaporation source 10 provides all the different precursor materials 15 , 16 whose evaporation is controlled in an alternating fashion, or the evaporation source 10 serves only for depositing only one of the precursor materials 15 , 16 and is then exchanged against another evaporation source 10 with the other of the precursor materials 15 , 16 . The depicted solution provides both precursor materials 15 , 16 at the same time in that evaporators for both precursor materials 15 , 16 are put side by side at the evaporation source 10 with an isolation wall between them. A shuttering mechanism is provided for alternately allowing only one of the precursor materials 15 , 16 at each moment in time to arrive through the apertures 14 at the substrate 4 . Thereby underneath each aperture 14 due to the subsequent deposition of layers of the evaporated precursor materials 15 , 16 , pillars 8 can grow on the substrate 4 . For layer thickness control, the sample holder 9 is retracted while the oscillating quartz 6 is moved at the position where the substrate 4 is positioned during the evaporation step. An in situ measurement is performed while the quartz's frequency is monitored. Thus the exact deposition rate can be measured and used for determining the layer thickness for the precursor materials 15 , 16 to be deposited on the substrate 4 .
Once the desired deposition has been achieved and the substrate 4 is patterned with the resulting pillars 8 , the apparatus is modified as depicted in FIG. 2 . The second tool support 12 is altered to now hold a magnet 2 which either itself is pointed or, as depicted here, is combined with a pointed ferrite core 3 , whereby the point is directed towards the substrate 4 . With this arrangement the substrate 4 with the pillars 8 can be heated in the presence of a first magnetic field 17 . The pointed magnet 2 , respectively ferrite core 3 , serves for concentrating the first magnetic field 17 onto the pillars 8 where the reaction converting the pillars 8 into the single-walled carbon nanotubes 19 is taking place. The field 17 provides the driving force for moving the catalyst along the field direction. This also holds true for the case when the field 17 is an electric field or an electromagnetic field.
In FIG. 3 a schematic view of a single pillar 8 as precursor structure for manufacturing the single-wall carbon nanotubes 19 is shown. The precursor structure from which the nanotubes 19 are grown consists here of a hetero structure comprising alternate layers of C 60 molecules being the first precursor material 15 and Nickel being the second precursor material 16 , thermally evaporated. Some 6 or 7 layers with thicknesses of 10-20 nm are deposited on top of each other. The precursor materials 15 , 16 are deposited through the shadow mask 7 , representing a sort of nano-sieve, having several thousand apertures 14 with a diameter of 300 nm and with a pitch of 1 micron. This method of deposition generates small nucleation sites that enable subsequent self assembly of the single-walled carbon nanotube crystals 20 . Although instead of using the shadow mask 7 the material can also be deposited on a substrate 4 with a rough faceted surface, less nanotubes 19 are produced in preference to disordered platelets. In general, some seed location, i.e. nucleation site or crystallization site is the location where the crystal growth initiates.
It is found that in a structure where there is a nucleation site near the pillar 8 , the pillar 8 serves only as material supply for the crystal 20 growing nearby. The pillar 8 has here a diameter of 300 nm but it can generally be stated that the lateral dimensions of the pillar 8 can be selected in a broader range. Although excellent results can be obtained with the 300 nm diameter, a bigger diameter like 500 nm or more should lead to acceptable results as well. The lateral dimensions of the pillars 8 determine the total amount of the precursor materials 15 , 16 that are involved in the growth of the corresponding crystal 20 . Each growing crystal 20 has hence its reservoir of precursor materials 15 , 16 from which it gets its material supplied. The predetermination of the material supply has the effect that the different precursor materials 15 , 16 used in the growth of the corresponding crystal 20 are predetermined in their amount and position. The movement of the molecules of the precursor materials 15 , 16 is hence rather confined within the pillar area and a less chaotic movement leading to a more determined growth process can result therefrom. Also the concentration of the precursor materials 15 , 16 relatively to each other can have a decisive effect, which means that the amount of the second precursor material 16 which is necessary for helping the first precursor material 15 to grow into the desired nanotube form, should neither be substantially exceeded nor substantially fallen below of. Again, the confinement of the precursor materials 15 , 16 in their pillar 8 , leads to a more precise ratio between the two precursor materials 15 , 16 that contribute to the crystal growth of a single crystal 20 .
Since the pillars 8 have also a certain predetermined distance from each other, a mutual disturbing effect of the growing crystals is reduced with respect to a bulk precursor material system. Hence growth of each single crystal 20 at its crystallization point is not or only negligibly interfered with by the growth process of an adjacent crystal 20 . The pillars 8 have hence a distance from each other and this distance reduces the mutual interference of the growth process of the respective crystals, respectively nanotubes 19 .
The pillars 8 have a lateral dimension such that the amount of the precursor materials 15 , 16 is confined to provide the material for a single crystal 20 being a bundle of nanotubes 19 . It is presumed that the stronger the applied field 17 , the larger can be chosen the lateral dimensions of the pillars 8 , since the force that directs the second precursor material 16 is stronger. The pillar shape need not be round or square in but can have any form that is deemed appropriate. For symmetry reasons the round shape is however preferred. The bundle may range from a few to several hundred, thousands or even millions of nanotubes 19 .
It is possible to artificially grow the nucleation sites on the substrate 4 to enable controlled positioning of crystal growth. Such creation of nucleation sites can e.g. be achieved by evaporating through the evaporation mask 7 a material, e.g. tungsten, that can serve as nucleation site on the substrate 4 . Since the evaporation mask 7 has a shadowing effect, an evaporator for the nucleation material which is situated sufficiently apart from the evaporators for the precursor materials 15 , 16 automatically generates the nucleation sites near the pillars 8 . In contrast, the evaporators for the precursor materials 15 , 16 should be situated closely together in order to avoid a lateral misalignment of the various layers in the pillar 8 , in that case, both evaporators are situated simultaneously in the reaction chamber 1 .
During evaporation at a pressure of 10 −9 Torr onto the solid substrate 4 of thermally oxidized silicon or a Mo TEM grid at room temperature, electromechanical shuttering combined with an in situ quartz crystal microbalance to monitor deposition rates, can be used to ensure that both C 60 and Ni can be evaporated sequentially to produce the desired structure.
As shown in FIG. 3, this produces a pillar 8 of precursor materials 15 , 16 at a specific surface site determined by the relative position of the aperture 14 and the substrate surface. The choice of substrate 4 is influenced by the fact that both C 60 and Ni are able to diffuse at high temperatures and the aim is to constrain both materials within the original 300 nm evaporation area. Although good results can be achieved with the silicon dioxide substrate 4 , better results can be obtained with a molybdenum substrate 4 either in the form of a grid for subsequent transmission electron microscopy, or as a solid film sputtered on to a silicon wafer. After evaporation of the C 60 /Ni pillars 8 on the substrate 4 , the arrangement is heated to 950° C. in a vacuum of 10 −6 Torr for a time which is chosen to lie between a few minutes and an hour. Growth of the resulting nanotubes 19 is oriented normal to the substrate surface when the substrate 4 is immersed in the magnetic field 17 oriented parallel to the substrate surface normal during heat treatment. A field strength of ˜1.5 Tesla is suitable to achieve the desired results. The application of an electric, electromagnetic or magnetic field 17 directs the self-assembly and organization of the single-walled carbon nanotube crystals 20 . The electric field can be an AC or DC field. The electromagnetic field can also be an optical near field e.g. of a laser. Also atomic forces or Van der Waals forces may be applied during growth. Also possible is the application of an electronic potential that could change the field emission of tunneling processes such that the electron currents influence the crystal growth as in electromigration.
The material of the second precursor material 16 is directed into the direction of the applied field 17 . Hence the field and the second precursor material 16 interact such that the second precursor material 16 has the property to be movable by the field 17 . Such property can be that the second precursor material 16 is magnetic or bears an electric charge or a combination of both or has any other property that is influenced by the applied field 17 to exert a moving force on the second precursor material 16 .
High-resolution TEM (HREM) studies performed in a JEOL 4000FX microscope operating at 400 kV, for carrying out a detailed diffraction analysis in a 200 kV JEOL 2010 microscope show nanotube bundles to be present with diameters varying between 40 nm and 900 nm with lengths up to 2 microns. The nanotubes 19 are straight and preferentially aligned parallel to the Mo-grid plane. All the nanotubes 19 are single-wall carbon nanotubes 19 forming long and straight bundles. The wall diameters in a bundle are remarkably uniform and range from about 1.4 nm to 2.3 nm in individual bundles. There is an inverse correlation between wall and bundle diameter in that small wall diameters are predominantly observed in large diameter bundles whereas large wall diameters are found in small diameter bundles. Neither multi-wall carbon nanotubes nor isolated single-wall nanotubes are present, the former being excluded on both the observed wall thickness and the absence of a core region.
A typical HRTEM image of a bundle of nanotubes 19 is shown in FIG. 4 a with a higher magnification image showing the internal structure of the nanotube bundle in FIG. 4 b . The bundle is ˜750 nm long and ˜50 nm diameter with a curved end cap.
FIG. 4 b shows the perfect regular arrangement of 1.6 nm diameter single-walled carbon nanotubes 19 in a bundle with no evidence of inhomogeneity or defect. This remarkable structural perfection is a characteristic of all nanotubes 19 produced using the described method.
FIG. 4 c shows a schematic view of a bundle of 7 nanotubes 19 , as they are present in the result depicted in FIGS. 4 a , 4 b , the nanotubes 19 each having a diameter of 1.6 nm.
A scanning electron microscope (SEM) micrograph of a typical structure produced by the described method, depicted in FIG. 5, shows rod-like structures of approximately identical diameter and length with curved end caps have grown normal to the substrate surface. This result is typical of the structures produced with the only variability being the length and width of the rods. To confirm that the rods are carbon nanotube crystals 20 , in the case they are grown on a Molybdenum grid both EELS giving the chemical composition, and electron diffraction, can be carried out. An EELS spectrum of a rod acquired in a VG 501HB STEM operating at 100 kV with a dispersion of 0.1 eV per channel at the Carbon-K edge shows an intense pre-peak at 285 eV just below the main absorption threshold. This pre-peak is a characteristic of the transitions to p* states in sp2-bonded carbon suggesting that graphite-like sheets are present in the nanotube 19 . The spectrum closely resembles previous EELS spectra of carbon nanotubes 19 and confirms that they are indeed made of carbon. Importantly, the presence of Nickel in the EELS spectra is only detected during the growth phase of the nanotube 19 with no evidence of neither Nickel nor Molybdenum in the fully-grown nanotube 19 .
An electron diffraction pattern from a different bundle with single-walled carbon nanotubes 19 diameter 1.98 nm is shown in FIG. 6 . The perfection of the structure is immediately obvious from the sharpness of the diffraction spots. The pattern indicates a highly regular periodicity due to the regular arrangement of nanotubes 19 in the bundle. In fact, more accurately, the bundle has to be considered as a periodic “crystal” of single-walled carbon nanotubes 19 . Since this periodicity leads to strong reflections in the diffraction pattern, the weak diffraction spots and streaks containing the information about the individual nanotubes 19 almost disappear.
Referring to FIG. 6, two primary directions are indicated corresponding to the half single-walled carbon nanotubes wall width of 0.99 nm and orthogonal to this a spacing of 0.28 nm corresponding to the spacing of the graphite hexagons. The weak super reflections have a spacing that corresponds to the double of 0.28 nm.
There is a simple relationship between the diameter and helicity of individual nanotubes 19 specified in terms of a roll up vector (n,m) which arises from considering how an atom-thick graphite sheet can be rolled up to produce a nanotube. The diameter d and chiral angle q are given by:
d= 0.078( n 2 +nm+m 2) 1/2
and q =arc tan ( m /( m+ 2 n ))
From FIG. 6 the chiral angle q is 90° and hence m=n. d is measured as 1.98 nm so that n=m=15 corresponding to a so-called armchair structure. For any crystal 20 of single-walled carbon nanotubes 19 the diffraction pattern indicates that it is made up of physically identical single-walled carbon nanotubes 19 of either chiral or armchair structure. A final structural observation is that relating to the shape of the individual crystals. Previous observations of bundles have demonstrated that the single-walled carbon nanotubes 19 are packed in a hexagonal structure looking towards the end of the bundle. Considering whether the equilibrium cross-sectional shape of a bundle would be circular, hexagonal or more complex in section, a simple argument based on a hexagonally packed structure of identical single-walled carbon nanotubes 19 favors a structure whose faces consist of close packed single-walled carbon nanotubes 19 . This would include a hexagonal cross-section but could equally well be any cross-section consisting of 120° facets. The projected shapes of the bundles and the contrast in the HRTEM images indicate that faceting of the single-walled carbon nanotubes 19 crystals does indeed occur. The characteristics of self-assembled materials can be hence designed through nano-structuring of the reactants in three dimensions combined with programmed environmental changes.
The perfection of the crystals 20 of single-walled carbon nanotubes 19 and the observation that the nanotubes 19 are all physically identical within a given crystal 20 containing up to several million nanotubes 19 is unexpected, based on prior results and synthetic approaches in the field 17 . Nevertheless, the most stable arrangement of bundles of nanotubes 19 meets with thermodynamic expectations of a minimum energy configuration over an extended array of nanotubes 19 in close contact. Minimization of energy also implies that all the nanotubes 19 be identical and straight, permitting maximization of the Van der Waals interactions, minimization of strain, and an expected hexagonal lattice. Evidence of faceting of the crystals 20 is another expectation that is indicated by the obtained results.
The nanotubes 19 respectively bundles thereof grown with the described method can be utilized in a number of devices such as switching devices, displays, or sensors. Depositing a layer of ITO and/or organic LED material on a layer of nanotubes 19 can be used to manufacture a display. Other embodiments comprise nanoelectronic circuits where nanotubes operate as active devices like FETs or as wiring. Also nanotube-based vacuum tube amplifiers and triodes with the nanotube acting as the emitter can be built, whereby the nanotube is used as a tip which provides stable low-voltage operation. Nanomechanical sensors and AFM tips can be supplied with a nanotube as sensor tip. Simply positioning the crystallization point where the later tip shall be located achieves the desired structure. The nanotube can be a movable part in switching devices or be integrated into a GMR head.
Any disclosed embodiment may be combined with one or several of the other embodiments shown and/or described. This is also possible for one or more features of the embodiments. It is obvious that a person skilled in the art can modify the shown arrangements in many ways without departing from the gist of the invention which is encompassed by the subsequent claims.
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The invention is directed to a method of manufacturing single-walled carbon nanotubes comprising the steps of providing on a substrate at least one pillar comprising alternate layers of a first precursor material comprising fullerene molecules and a second precursor material comprising a catalyst, and heating the at least one pillar in the presence of a first magnetic or electric field. It further is directed to a precursor arrangement for manufacturing single-walled carbon nanotubes comprising on a substrate at least one pillar comprising alternate layers of a first precursor material comprising fullerene molecules and a second precursor material comprising a catalyst. A third aspect is a nanotube arrangement comprising a substrate and thereupon at least one crystal comprising a bundle of single-walled carbon nanotubes with essentially identical orientation and structure.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation of copending International Application No. PCT/DE97/02105, filed Sep. 18, 1997, which designated the United States.
BACKGROUND OF THE INVENTION
Field of the Invention
The invention relates to a thermal power plant, including a steam turbine having a turbine rotor directed along a main axis and surrounded by an inner housing. A guide-blade structure, which surrounds the turbine rotor in the circumferential direction and has guide blades, is disposed in the inner housing. The invention also relates to a method for cooling a steam turbine in the ventilation mode, in particular a low-pressure steam turbine.
It is known, for example from a book entitled “Strömungs-maschinen” [Turbo-Machines] by K. Menny, Teubner-Verlag, Stuttgart, 1985, Section 3.4.6“Naβdampfstufen” [Wet-Steam Stages], that condensation of action steam takes place in steam turbines, in particular in so-called wet-steam stages. During an expansion of the steam in the steam turbine, supercooled steam occurs if there is a fall below a boundary curve with the wet-steam region, for example in the case of condensing turbines. The temperature of the supercooled steam is lower than a saturation temperature associated with the steam point. At specific supercooling, spontaneous condensation commences, in which small mist droplets occur that may settle on guide blades in the form of a water film or individual strands of water. The water film breaks away from trailing edges of the guide blades and forms secondary drops having a diameter of up to about 400 μm. Those steam droplets which break away may lead to a stripping of material, if they impinge on the moving blades, particularly when the drops have a diameter on the order of magnitude of 50 to 400 μm (so-called drop impact erosion). In order to avoid such drop impact erosion, the water film is often sucked away directly on the guide-blade surface. For that purpose, a hollow guide blade has slots which connect its interior to the condenser of the steam turbine.
German Published, Non-Prosecuted Patent Application DE-OS 19 51 922 specifies a device for preventing the formation of droplets in the low-pressure stages of steam turbines. Droplets are prevented from forming by feeding hot steam to the guide blades of the last guide-blade rows through an outer ring. The hot steam is conducted through the hollow guide blades to an inner ring and is conducted out of it again through a geodetically low-lying outflow conduit. The guide blades are to be heated to such an extent by feeding hot steam that condensation cannot take place at all.
Austrian Patent 250 402 describes introducing steam from preceding stages into guide-blades and feeding it into the steam flow again through slots in the guide blades. The avoidance of the formation of condensate on guide blades is likewise dealt with in U.S. Pat. No. 3,306,576, wherein hot steam is fed to a hollow guide blade and passing out of it through bores into the steam flow. The hot steam heats the steam flow to such an extent that the saturation temperature is exceeded at least locally and no condensation takes place.
A steam turbine blade which has a hollow structure and has an orifice for diverting steam into a main steam flow, is likewise described in the abstract of Japanese Patent Application 54-14 1908, Patent Abstracts of Japan, Jan. 18, 1980, Vol. No. 4.
European Patent 0 602 040 B1, corresponding to German Published, Non-Prosecuted Patent Application DE 41 29 518 A1and corresponding U.S. Pat. No. 5,490,386, describes a method for cooling a low-pressure steam turbine in the ventilation mode, wherein the rotor of the steam turbine is rotated, without being subjected to steam to be expanded. In a low-pressure turbine working in the ventilation mode, a steam atmosphere prevails, having a static pressure which corresponds to the pressure prevailing in the condenser connected to the low-pressure turbine. The friction of the turbine blades on the steam (ventilation) may lead to a considerable amount of heat being generated, with the result that the turbine may be heated to a high, possibly even inadmissibly high temperature. In order to avoid that from occurring, cooling measures are employed, in which, for example, condensate is injected, while at the same time being atomized, into the outlet or, if the cooling capacity to be applied has to be particularly high, into the inlet of the turbine. The condensate evaporates, with its temperature thereby being lowered, and as a result, the ventilating turbine is cooled. If injection takes place at the outlet, the cooling effect is often restricted to parts of the turbine in the vicinity of the outlet. If injection takes place at the inlet, condensate which agglomerates in the region of the inlet may put the blading of the turbine at risk due to surging. Therefore, according to European Patent 0 602 040 B1, corresponding to German Published, Non-Prosecuted Patent Application DE 41 29 518 A1 and corresponding U.S. Pat. No. 5,490,386, steam is fed into the steam turbine through a tapping point located between the outlet and the inlet of the steam turbine. Cooling in the turbine thereby first benefits the radially outer ends of the blades. The ends are subjected to the highest load as a result of the friction on the steam located in the turbine. The cooling effect is thus restricted essentially to those regions of the turbine in which it is desired. The cooling of other components of the turbine, for example, of the turbine shaft, is avoided.
Besides steam, condensate is additionally fed to a tapping conduit connected to the tapping point, in particular by injecting condensate into the steam transfer conduit and/or into the tapping conduit through the use of a condensate transfer conduit. The condensate is preferably mixed with the steam in an atomizer nozzle and is injected from that atomizer nozzle into the tapping conduit. A particularly high cooling effect is achieved by a condensate which is distributed into fine droplets and the droplet diameters of which are smaller than about 0.1 mm. The cooling process is controlled through a temperature measuring point located between the tapping point and the outlet, the feed of the steam or the feed of the steam/condensate mixture for tapping being regulated as a function of the measured temperature. The quantity of steam or steam/condensate mixture fed to the tapping conduit is approximately on the order of magnitude of 1% of the steam stream when the steam turbine is operating in the power mode. The steam used for cooling comes from a condensate container which serves for collecting, heating and degassing the condensate. Steam from the condensate container, to which hot steam is usually fed for the purpose of degassing the condensate, is saturated due to the coexistence of steam. Condensate, if appropriate, is even mixed with finely distributed condensate, and is therefore particularly suitable for injection into the ventilating turbine. Furthermore, steam may be extracted from a steam discharge conduit, through the use of which the steam is conducted past the low-pressure turbine in the ventilation mode. Such a steam discharge conduit conducts the steam, for example, from a high-pressure steam turbine preceding the low-pressure steam turbine or from a configuration formed of a high-pressure steam turbine and of a medium-pressure steam turbine, around the low-pressure steam turbine, to a heating device or the like, where the steam is possibly cooled and condensed. In order to obtain a steam/condensate mixture, the steam to be fed to the tapping point may be extracted from such a heating device. The steam may likewise be extracted from a high-pressure or medium-pressure steam turbine preceding the low-pressure steam turbine, directly or indirectly, for example from a preheater or the like fed by the turbine. Such steam normally has a sufficiently high characteristic pressure, so that feeding into the ventilating steam turbine can take place without separate pumps or the like.
SUMMARY OF THE INVENTION
It is accordingly an object of the invention to provide a thermal power plant having a steam turbine and a method for cooling a steam turbine in a ventilation mode, which overcome the hereinafore-mentioned disadvantages of the heretofore-known devices and methods of this general type, in which the steam turbine can be cooled simply and effectively in a ventilation mode and/or in which condensation on guide-blades can be avoided, or at least reduced, simply and effectively.
With the foregoing and other objects in view there is provided, in accordance with the invention, a thermal power plant, comprising a steam turbine including a turbine rotor directed along a main axis, an inner housing surrounding the turbine rotor, a guide-blade structure disposed in the inner housing and surrounding the turbine rotor in circumferential direction, the guide-blade structure having guide blades, and at least one of the guide blades having a cavity formed therein, having an outer surface and having at least one orifice conduit branching off from the cavity and opening to the outer surface; a fluid conduit connected to the cavity for feeding cooling fluid; a condensate vessel; and a closeable transfer conduit connected between the condensate vessel and the fluid conduit.
In an idling and/or low-power mode (ventilation mode), the blades of the last blade rows of a low-pressure steam turbine, in particular, become heated. In such a ventilation mode, a meander flow having an insignificant effective backflow is formed. Feeding finely atomized water or wet steam, generally cooling fluid, through the orifice conduit into the steam turbine gives rise, upstream of the outlet, to a cooling of the-guide blades and moving blades. Evaporation of water droplets thus brings about effective cooling, particularly of the last low-pressure blade rows which are heated to the greatest extent in the ventilation mode. In this case, through the use of a change-over of the feed of fluid into the fluid conduit, the steam turbine can, on one hand, be heated locally by applying a hot fluid in a regular power mode, in order to avoid the action steam condensing on the guide blades connected to the fluid conduit, and, on the other hand, be cooled by applying a cooling fluid, for example water or wet steam, in a ventilation mode. The orifice conduit is preferably constructed, on the outer surface, as a hole, in particular with an approximately circular or elliptic crosss-ection.
A fluid, preferably superheated steam, may be fed into the action steam stream through the cavity and through the orifice conduit which, in particular, is a bore. Feeding steam through a multiplicity of fine orifice conduits and heating the guide blades as a result thereof produces a steam cushion which prevents the agglomeration of large drops on the blade surface. Admixing hot steam in the vicinity of the outer surface of the guide blade in particular reduces the wet-steam fraction which would otherwise be very high, for example on the last low-pressure guide-blade row of a low-pressure steam turbine. The risk of drop impact erosion is at least markedly reduced thereby. The hollow guide blade is preferably disposed in one of the last guide-blade rows, in particular the antepenultimate, the penultimate or the last guide-blade row.
In accordance with another feature of the invention, the guide blades of the steam turbine are connected to an outer-ring chamber for conducting the fluid that is required in each case, with the fluid conduit opening into the outer-ring chamber. As a result, all of the guide blades of a guide-blade row can be fed with the fluid in a simple way.
In accordance with a further feature of the invention, in order to provide the discharge of condensation water, the outer-ring chamber has a drainage conduit in its low region.
In accordance with an added feature of the invention, the fluid conduit is connected to the outer-ring chamber in a geodetically high region.
In accordance with an additional feature of the invention, in guide blades are connected to an inner-ring chamber in order to simplify the construction, to increase thermal mechanical stability and to conduct the cooling fluid or heating fluid. Thus, particularly in the case of guide blades having cavities which extend from the outer-ring chamber to the inner-ring chamber, it is also possible to feed the fluid into the individual guide-blades both from the inner-ring chamber and from the outer-ring chamber.
In accordance with yet another feature of the invention, the steam turbine can be connected, during operation in a power mode, to a plant component carrying hot steam, for example a high-pressure steam turbine, and/or, in a ventilation mode, to a plant component carrying water, in particular condensate, or wet steam, for example a condenser, a preheater, a heat exchanger, etc. Corresponding connecting conduits between the fluid conduit and the corresponding plant components can be cut in and cut out through corresponding actuators or shut-off valves. It is also possible to provide a central actuator which is connected to various feed conduits for hot fluid and cooling fluid and which is connected to the fluid conduit. Depending on the particular requirement, a fluid having a desired pressure and temperature state can be fed to the fluid conduit from a feed conduit or a plurality of feed conduits through this actuator.
In accordance with yet a further feature of the invention, the orifice conduit opens on the outer surface of the guide blade, preferably on the suction side in the region of the onflow edge. As a result, in the ventilation mode, cooling fluid spreads from the onflow edge over the entire surface of the suction side of the guide blade towards the flow-off edge, as a cooling film as it were. In the power mode, the hot fluid is likewise mixed with the action steam in a region around the surface of the guide blade, thereby effectively avoiding, or at least markedly reducing, the formation of relatively large condensate droplets.
With the objects of the invention in view there is also provided a method for cooling a steam turbine in a ventilation mode, which comprises providing a turbine rotor directed along a main axis; providing an inner housing surrounding the turbine rotor; providing a guide-blade structure in the inner housing surrounding the turbine rotor in circumferential direction; providing a hollow guide blade of the guide-blade structure; and feeding a fluid, in particular wet steam or condensate, through at least the hollow guide blade into the inner housing, in a ventilation mode.
This leads to effective cooling of the blades, particularly in the case of the last blade rows of a low-pressure steam turbine. With regard to carrying out the method, reference may also be made to European Patent 0 602 040 B1, corresponding to German Published, Non-Prosecuted Patent Application DE 41 29 518 A1 and corresponding U.S. Pat. No. 5,490,386.
In accordance with a concomitant mode of the invention, the hollow guide blade is preferably disposed in one of the last three guide-blade rows.
Furthermore, a reduction in the condensation of action steam on a guide blade of a steam turbine in the power mode is possible if, in this case, a hot fluid, in particular hot steam, is fed to the cavity of the guide blade. The hot fluid flows out through orifice conduits on the outer surface of the guide blade and is mixed with the action steam there and, if appropriate, on the entire outer surface of the guide blade. On one hand, the hot fluid causes the guide blade to be heated and, on the other hand, mixing with the action steam leads to heating of the action steam. Both effects contribute to a marked reduction, if not even to a complete avoidance, of the formation of condensate droplets on the guide blade. The risk of drop impact erosion on moving blades disposed downstream of the guide blade is thereby virtually eliminated.
Other features which are considered as characteristic for the invention are set forth in the appended claims.
Although the invention is illustrated and described herein as embodied in a thermal power plant having a steam turbine and a method for cooling a steam turbine in a ventilation mode, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic circuit diagram of a power station system with a low-pressure steam turbine;
FIG. 2 is an enlarged, fragmentary, longitudinal-sectional view of a low-pressure steam turbine;
FIG. 3 is a further enlarged, cross-sectional view of the last guide-blade row of a low-pressure steam turbine;
FIG. 4 is an even further enlarged, fragmentary, perspective view of a guide blade; and
FIG. 5 is a cross-sectional view of a guide blade according to FIG. 4 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the figures of the drawings in detail and first, particularly, to FIG. 1 thereof, there is seen a diagrammatic illustration of a thermal power plant with a high-pressure steam turbine 17 a , a low-pressure steam turbine 1 , a condenser 18 a and a condensate container 36 , in which further components of the thermal power plant, for example a boiler or a generator, are not illustrated. The components of the thermal power plant which are illustrated are connected to one another through the use of steam connecting conduits 28 or condensate conduits 29 . A condensate pump 37 is inserted into the condensate conduit 29 . A change-over device 30 is located between the high-pressure steam turbine 17 a and the low-pressure steam turbine 1 , in the steam connecting conduit 28 . Hot steam flowing off from the high-pressure steam turbine 17 a can be diverted through a further steam connecting conduit 28 to a heating heat exchanger 31 with the aid of the change-over device 30 , which is conventionally formed by flaps. Thus, the low-pressure steam turbine 1 is not subjected to hot steam, depending on the setting of the change-over device 30 . The steam conducted past the low-pressure steam turbine 1 is condensed in the heating heat exchanger 31 and flows as condensate to the condensate container 36 .
The low-pressure steam turbine 1 is rigidly coupled to the high-pressure steam turbine 17 a , so that non-illustrated rotors of the two steam turbines 1 and 17 a run synchronously. If the steam flowing off from the high-pressure steam turbine 17 a is conducted past the low-pressure steam turbine 1 , that is to say the latter rotates idly, friction occurs in the low-pressure steam turbine 1 due to the static pressure which prevails therein and which corresponds to the pressure of the steam in the condensate container 36 . A fluid conduit 7 for introducing fluid into the low-pressure steam turbine 1 is disposed between an inlet 33 , which serves for subjecting the turbine to action steam, and an outlet 34 , through which the steam expanded in the low-pressure steam turbine 1 is conducted to the condenser 36 . The fluid conduit 7 is connected to a cavity 6 of a guide blade 5 a seen in FIGS. 2, 3 and 4 . The condensate is heated in the condensate container 36 through the use of steam which is fed from the high-pressure steam turbine 17 a through the use of a hot-steam conduit 32 .
A steam-filled steam space 42 is located in the condensate container 36 above a condensate level. Steam is extracted from this steam space 42 and is fed to the fluid conduit 7 through a steam transfer conduit 38 . Furthermore, condensate is fed from the condensate container 36 to the fluid conduit 7 through a condensate transfer conduit 39 . A branch-off of the hot-steam conduit 32 is connected to the fluid conduit 7 through a corresponding valve 27 . The steam transfer conduit 38 and the condensate transfer conduit 39 likewise each have a valve 27 and are connected to the fluid conduit 7 . All of the valves 27 are connected to a temperature measuring point 40 in the low-pressure team turbine 1 through a control line 41 . As a result, the quantity of fed-in condensate and steam from the steam space 42 and of hot steam from the high-pressure steam turbine 17 a can be fed in a regulated manner into the fluid conduit 7 and, through the guide blade 5 a , into the low-pressure steam turbine 1 . Regulated cooling of the low-pressure steam turbine 1 in the ventilation mode, without work output being expended, and a feed of hot steam into the guide blade 5 a to reduce the condensation of action steam, can thus be carried out.
Insofar as there is no condensate container 36 available for the extraction of steam or condensate, steam may be extracted, for example, from the heating heat exchanger 31 or from a non-illustrated preheater which is assigned to the high-pressure steam turbine 17 a.
FIG. 2 shows a portion of a double-flow low-pressure steam turbine 1 with a turbine rotor 3 which is directed along a main axis 2 and which carries moving blades 24 . The turbine rotor 3 is mounted in a turbine bearing 22 and is sealed off relative to an inner housing 4 of the steam turbine 1 through the use of a rotor gasket 23 . Guide blades 5 , which are connected to the inner housing 4 , and the moving blades 24 of the rotor 3 , are disposed alternately in the axial direction. The guide blades 5 , in particular the guide blade 5 a of the last low-pressure guide-blade row (guide-blade structure 11 seen in FIG. 3) are constructed, for example, as hollow guide blades inclined in the axial direction and curved in the circumferential direction. The guide blades 5 , 5 a of a guide-blade row are welded to a likewise hollow outer ring having an outer-ring chamber 12 of the inner housing 4 and are welded to an inner ring having an inner-ring chamber 16 adjacent the rotor 3 and surrounding the latter and are thus connected to one another. Action steam 19 flows through the low-pressure steam turbine 1 in the axial direction and is directed vertically and conducted out of the steam turbine 1 through an exhaust-steam port 20 . The guide blade 5 a has orifice conduits 9 a , 9 b seen in FIGS. 4 and 5, through which fluid 8 can be fed into the region of flow of the action steam 19 .
The orifice conduits 9 b are disposed in the vicinity of an onflow edge 26 , on the suction side, preferably essentially facing the outer-ring chamber 12 . The orifice conduits 9 a are disposed on a delivery side.
FIG. 3 shows a cross-section through the guide-blade structure 11 of the last guide-blade row of the steam turbine 1 . The fluid conduit 7 , which can be shut off through the use of a valve 27 , opens out into a geodetically high region or outer-ring chamber 15 of the outer-ring chamber 12 . The guide blades 5 a , which are welded to the outer-ring chamber 15 , extend radially in the direction of the main axis 2 of the turbine rotor 3 . They are welded to the inner-ring chamber 16 surrounding the turbine rotor 3 . The guide-blade structure 11 is produced from two exactly fitting halves which are joined to one another along a parting plane 25 . A drainage conduit 14 is provided in a geodetically lowest region 13 of the outer-ring chamber 12 .
In the ventilation mode, condensate and/or wet steam can be introduced into the outer-ring chamber 12 through the fluid conduit 7 . This steam 8 passes through the cavity 6 seen in FIGS. 4 and 5 into the guide blade 5 a . The cavity 6 preferably extends from the outer-ring chamber 12 through the entire guide blade 5 a along a center line 21 as far as the inner-ring chamber 16 . The orifice conduits 9 b and 9 a , in particular bores, are provided on the suction side and the delivery side as is seen in FIGS. 4 and 5, and connect the cavity 6 to an outer surface 10 of the guide blade 5 a . The fluid 8 , the wet steam and/or the condensate, flows out of the guide blade 5 a from these orifice conduits 9 a , 9 b . When the steam turbine 1 is in the ventilation mode, the outflowing fluid 8 causes the guide blade 5 a to be cooled, in particular with a cooling film forming over its outer surface 10 . When the steam turbine 1 is in the power mode, hot steam is fed to the cavity 6 through the fluid conduit 7 , the hot steam is mixed with the action steam 19 on the outer surface 10 and, particularly when this is saturated steam, leads to a marked increase in temperature of the action steam 19 . Moreover, the fed hot steam causes the guide blade 5 a to be heated, so that the formation of condensate droplets, particularly on the flow-off edge of the guide blade 5 a , is markedly reduced, if not even completely avoided.
The invention is distinguished by the fact that guide blades, in particular one or more of the last three guide-blade rows of a low-pressure steam turbine, have a cavity, from which orifice conduits lead onto the surface of the respective guide blade. In the ventilation mode, cooling fluid, in particular wet steam or condensate, and, in a power mode, hot steam, can be fed to this cavity through a fluid conduit. In the ventilation mode, this effectively achieves cooling of the guide blade by simple measures and, in the power mode, heating of the guide blade and heating of the action steam, with the formation of condensate on the guide blade, is avoided.
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A thermal power plant includes a steam turbine having guide blades. At least one of the guide blades has a cavity. The cavity is connected to a fluid conduit for feeding fluid and to orifice conduits opening on an outer surface of the guide blade. A method for cooling a steam turbine in a ventilation mode is also provided.
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BACKGROUND OF THE INVENTION
[0001] 1. Technical Field
[0002] The present invention relates to a microprocessor monitoring apparatus for monitoring an operating status of a CPU (Central Processing Unit), while performing reset operation on the CPU.
[0003] 2. Description of the Related Art
[0004] In an apparatus with a microprocessor, a program may go out of control due to hardware failure, etc. and a hardware timer circuit called a watchdog timer is provided to detect such runaway of the program (for example, see Japanese Laid-Open Patent Publication No. H10-269109). A reset signal is input to the watchdog timer (hereinafter, abbreviated as WDT) from a monitored program at predetermined intervals, and when the reset signal is not input due to runaway of the monitored program, the WDT restarts the microprocessor.
[0005] Further, when a program (firmware) that the microprocessor executes is rewritten for the reason of updating the apparatus function, modifying a bug, or the like, in order to execute a new program, it is necessary to restart the microprocessor after the rewrite so as to execute the main program from the first line.
[0006] Conventionally, since a restart dedicated circuit is provided to restart, the circuit has become larger. Therefore, it is an object of the present invention to provide a method for enabling a microprocessor to be restarted after rewriting a program without providing a dedicated circuit and an apparatus using the method.
BRIEF SUMMARY OF THE INVENTION
[0007] To attain the above-mentioned object, in the invention, a timer means for counting a predetermined clock is controlled by following first mode and second mode. It is a feature that in the first mode the timer means is reset (count-cleared) at predetermined intervals by a program to monitor an operating status of the program, and that in the second mode the microprocessor is restarted without resetting the timer means at predetermined intervals by the program. The configuration will specifically be described. The apparatus has a microprocessor, storing means for storing a program that the microprocessor executes, timer means for timing, and control means for controlling the timer means. Then, the control means is provided with the first mode for resetting the timer means at predetermined intervals by the program and monitoring an operating status of the program, and the second mode for restarting the microprocessor without resetting the timer means at predetermined intervals by the program.
[Advantageous Effect of the Invention]
[0008] The invention enables a single timer means to monitor an operating status of a microprocessor and perform restarting operation, and thus, enables the circuit configuration to be reduced in size and simplified. In other words, the timer means that has conventionally been used only as a monitoring apparatus of the microprocessor is configured to restart the microprocessor, and the need is thereby eliminated to provide a restart dedicated circuit.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0009] FIG. 1 is a configuration explanatory view of an image reading system according to the invention;
[0010] FIG. 2 is a configuration diagram of an image reading apparatus in the apparatus of FIG. 1 ;
[0011] FIG. 3 is a hardware configuration block diagram in the apparatus of FIG. 1 ;
[0012] FIG. 4 is a configuration schematic view of a program in ROM according to the invention;
[0013] FIG. 5 contains schematic views of program monitoring operation, and FIG. 5( a ) shows a first mode (program monitoring mode), and FIG. 5( b ) shows a second mode (program non-monitoring mode);
[0014] FIG. 6 shows a program rewrite flow;
[0015] FIG. 7 is an explanatory view of program states of FIG. 6 ; and
[0016] FIG. 8 shows another program rewrite flow different from in FIG. 6 .
DETAILED DESCRIPTION OF THE INVENTION
[0017] The present invention will be described using an image reading system as an example. As shown in FIG. 1 , the image reading system has a scanner 10 that is an image reading apparatus for reading an image of an original document, and a personal computer (hereinafter, abbreviated as “PC”) 20 that is an upper apparatus of the scanner 10 and that transmits various commands to the scanner. The PC 20 and scanner 10 are connected via an interface such as USB, SCSI, Ethernet and PCIe, and the PC has incorporated application program as a user interface for the scanner and driver program to operate the scanner.
[0018] Further, the PC 20 is connected to a network, and is configured to acquire a new program via the network in rewriting the program of the scanner 10 and transmit the new program to the scanner 10 . In addition, the scanner 10 maybe a complex apparatus provided with various functions such as a printer and facsimile, and any apparatus is applicable which is provided with a watchdog timer circuit described later.
[0019] Further, this Embodiment describes the example of using the separate PC 20 as an upper apparatus of the scanner 10 i.e. an apparatus to issue commands to the scanner 10 , but the scanner 10 maybe internally provided with a command transmitting section (application and driver) that has the same function as that of the PC 20 to exchange commands and image data inside the scanner. In this case, the scanner itself is provided with a display section such as a display, and is configured to enable a user to set various reading conditions on a setting screen in the display section.
[Configuration of the Scanner]
[0020] As shown in FIG. 2 , the scanner 10 has a platen 15 supported on the upper surface of a casing 5 to mount an original document, and an image reading unit 17 for reading the original document on the platen 15 . In the image reading unit 17 , in order to read an image of the original document on the platen while moving along the platen 15 , a traveling belt 18 coupled to a motor Mc is coupled to a carriage 19 . A light source 21 irradiates the original document on the platen 15 with light, the reflected light from the document is guided to a condenser lens 23 via a mirror 22 , the condenser lens 23 forms an image on a reading sensor (CCD) 24 so as to perform photoelectric conversion, and reading of the document image is thereby performed.
[0021] As shown in FIG. 3 , the PC 20 and scanner 10 are connected via a port 1 , and the PC 20 is connected to the network. The scanner 10 is provided with a CPU 30 that is a microprocessor to perform various computation processing, flash memory as ROM 31 that is a storing means for storing programs that the CPU 30 executes, RAM 32 that is memory to temporarily store data, etc. during various processing, clock oscillator 33 that issues a clock, and watchdog timer circuit (hereinafter, referred to as a WDT circuit) 35 to perform monitoring of the program, and further, is connected to the light source 21 , motor Mc and CCD 24 via a port 2 .
[0022] As shown in FIG. 4 , the ROM 31 stores a boot program Pb having an initial program Pn and rewrite program Pk, and main program Pm. The initial program Pn is a program to execute initial processing such as clearing the RAM 32 and initializing various kinds of hardware when the apparatus is turned on, and the boot program Pb is a program that is executed when the boot program itself or main program Pm is rewritten. The main program Pm is a program for the scanner 10 to execute various kinds of processing after the initial processing. In addition, for simplicity in description, FIG. 4 shows the rewrite program Pk and initial program Pn as separate programs, but the programs are configured as an integrated continuous program.
[0023] Meanwhile, the WDT circuit 35 is provided with a counter (CNT) 36 to count up, counter register 37 to perform various settings of the counter 36 , clock selecting section 38 for inputting a clock with a predetermined frequency corresponding to the setting of the counter register 37 to the counter 36 , and reset control 39 for generating a reset signal to reset the control system including the CPU 30 when the count number of the counter 36 reaches a beforehand defined predetermined value (the overflow occurs). The counter register 37 has an ON/OFF setting area (count operation is started in the case of “1”, while being halted in the case of “0”, and the count value is initialized to zero) Ar 1 to select and set start/halt of the count operation of the counter 36 , and a frequency setting area Ar 2 to select and set the frequency of the clock to input to the counter 36 , and the clock selecting section 38 selects and inputs the clock with a predetermined frequency according to the settings in the frequency setting area Ar 2 . The counter 36 causes an overflow after counting the beforehand defined predetermined number of clocks.
[0024] Accordingly, the time (overflow time T) elapsed before the overflow is variable according to the frequency of the clock output from the clock selecting section 38 , and the overflow time T is shorter as the frequency is increased.
[Monitoring of the Program by the WDT Circuit]
[0025] Monitoring of the program by the WDT circuit 35 is performed as described below.
[0026] As shown in FIG. 5( a ) (first mode), a program (monitored program) monitored by the WDT circuit 35 is configured to reset the count value of the counter (CNT) 36 at predetermined intervals, and the above-mentioned overflow time T is set to be a time slightly longer than the reset interval of the counter value by the program. Accordingly, when the monitored program goes out of control and the counter value is not reset within the overflow time T, the counter 36 causes an overflow. In response to the overflow, the reset control 39 outputs a control reset signal, and the CPU 30 is reset.
[0027] In this Embodiment, as shown in FIG. 5( a ), the main program Pm is configured to reset the counter 36 at predetermined intervals so as to be monitored by the WDT circuit 35 . Accordingly, after the initial processing is executed according to the initial program Pn after powering on the apparatus, the main program Pm is executed, and during the execution of the main program Pm, the WDT circuit 35 operates in the first mode for monitoring the program as described above.
[0028] The second mode of the WDT circuit 35 that is executed in rewriting the program will be described with reference to the flowchart of FIG. 6 . In addition, in this Embodiment, descriptions are given assuming that both of the boot program Pb and main program Pm are rewritten as an example. When a user or service person selects rewrite of the program on a predetermined screen of the PC 20 , the PC 20 transmits a rewrite command to the scanner 10 , and the scanner 10 receives this command (ST 001 ). The CPU 30 receiving the rewrite command shifts the program to execute to the rewrite program on the ROM 31 from the main program Pm, and performs the following processing.
[0029] The CPU 30 sets the ON/OFF setting area Ar 1 of the counter register 37 at 0, and halts the count operation of the counter 36 of the WDT circuit 35 (ST 002 ). By this means, the WDT circuit 35 is in a state of not monitoring any program. Then, in ST 003 , the rewrite program is copied to the RAM 32 (in addition, thereafter, the rewrite program and main program each before being rewritten are respectively referred to as an old rewrite program Pk 0 and old main program Pm 0 , and new rewrite program and main program are respectively referred to as a new rewrite program PkN and new main program PmN.)
[0030] In ST 004 , the PC 30 acquires the new main program PmN and new boot program PbN from the PC 20 to write. More specifically, after erasing the old main program Pm 0 stored on the ROM 31 , the CPU 30 receives the new main program PmN and new boot program PbN transmitted from the PC 20 . Then, the new main program PmN is written in the area where the old main program Pm 0 has been stored, and the new boot program PbN is written in an area different from the area where the old boot program Pb 0 is stored. This state is shown in FIG. 7 .
[0031] Next, the CPU 30 sets the ON/OFF setting area Ar 1 of the counter register 37 at 1, and resumes the count operation of the counter 36 (ST 005 ). In addition, at this point, as described above, since the overflow time T is determined by the frequency of the clock input to the counter 36 , the frequency of the clock is selected and set such that the time is sufficient for erasing of the old boot program and movement of the new boot program as described later.
[0032] ST 006 is executed by the old rewrite program Pk 0 on the RAM 32 , the old boot program Pb 0 on the ROM 31 is erased, while the new boot program PbN acquired in ST 004 is written in the area where the old boot program Pb 0 has been stored. In addition, the count operation of the counter 36 of the WDT circuit 35 is resumed in ST 005 , but runs in the second mode of not monitoring the program.
[0033] In other words, as shown in FIG. 5 ( b ), the old rewrite program Pk 0 on the RAM 32 executed in ST 006 is not configured to reset the count value at predetermined intervals, and does not undergo monitoring of the WDT circuit 35 . Accordingly, the counter 36 is not reset by the old rewrite program Pk 0 and causes an overflow, the reset control 39 outputs a control reset signal, and the CPU 30 is reset. In other words, after executing the new initial program PnN, the new main program PmN is executed.
[0034] Thus, the old rewrite program Pk 0 on the RAM 32 is configured not to reset the count value of the counter regularly, the counter 36 is thereby caused to intentionally result in overflow, and the CPU 30 is thus automatically reset after rewriting the program. In other words, by using the WDT circuit 35 as a circuit to reset the CPU 30 (using in the second mode), it is made possible to reset the CPU 30 without using a dedicated circuit.
[0035] In addition, in this Embodiment, the counter 36 is resumed at timing between the ST 004 and ST 006 , but is resumed at any timing such that the counter 36 causes an overflow after the end of processing of ST 006 .
[0036] Further, in this Embodiment, after receiving the rewrite command, the count operation of the counter 36 of the WDT circuit 35 is temporarily halted in ST 002 . Even when the old rewrite program Pk 0 on the ROM 31 is also configured to reset the counter 36 at predetermined intervals as the main program, and is monitored by the WDT circuit 35 during the processing of ST 003 and ST 004 , such a program arises that it takes time to acquire the new program from the PC 20 in ST 004 , the CPU 30 is reset due to the overflow, and that the new program is not acquired, and to avoid the problem, the count operation is temporarily halted.
[0037] Referring to FIG. 8 , described next is Embodiment 2 for avoiding such a problem and automatically performing reset of the CPU 30 after rewriting the program using the WDT circuit 35 as in Embodiment 1.
Embodiment 2
[0038] The count operation of the counter 36 is halted in Embodiment 1, and in Embodiment 2, the program is subjected to rewrite processing while maintaining the count operation. Only parts different from Embodiment 1 will be described below.
[0039] After receiving a rewrite command in ST 001 , the overflow time T of the counter 36 is changed in ST 002 ′. The old rewrite program on the ROM 31 is beforehand configured to reset the counter 36 at predetermined intervals by dividing the processing of ST 004 or the like, and the overflow time T is changed in ST 002 ′ in accordance with the reset period of the counter 36 . By this means, the overflow does not occur during the processing of ST 003 and ST 004 , and it is possible to acquire a new program.
[0040] Next, the overflow time T of the counter 36 is changed again in ST 005 ′. As in Embodiment 1, the old rewrite program Pk 0 on the RAM 32 executed in ST 006 is not configured to reset a counter value at predetermined intervals as shown in FIG. 5( b ), and is not monitored by the WDT circuit 35 even when the counter 36 operates. Accordingly, in ST 005 ′, the overflow time T of the counter 36 is set so as to cause an overflow after completing the processing of ST 006 .
[0041] Thus, in Embodiment 2, the WDT circuit 35 operates in the second mode after ST 005 ′. As described above, as in Embodiment 2, by using the WDT circuit 35 as a circuit to reset the CPU 30 (using in the second mode), it is made possible to reset the CPU 30 without using a dedicated circuit.
[0042] In addition, this application claims priority from Japanese Patent Application No. 2009-028261 incorporated herein by reference.
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To provide a method for enabling a microprocessor to be restarted after rewriting a program without providing a dedicated circuit and an apparatus using the method, a timer means for counting a predetermined clock is controlled in the following first and second mode, where in the first mode, the timer means is rest (count-cleared) at predetermined intervals by a program so as to monitor an operating status of the program, and in the second mode, the microprocessor is restarted without resetting the timer means at predetermined intervals by the program.
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BACKGROUND OF THE INVENTION
This invention relates to an organopolysiloxane composition for viscous fluid coupling. More specifically, this invention relates to a viscous fluid coupling organopolysiloxane composition which is stable for long periods of time and so does not suffer from torque variations at high temperatures and high shear forces.
Because the fluid used for viscous fluid coupling must have properties such as an appropriate viscosity, high flash point, stability against oxidation, stability against thermal decomposition and an insignificant temperature dependence on the part of the viscosity, fluid dimethylpolysiloxanes have generally been used heretofore in this application.
However, by themselves, dimethylpolysiloxane fluids tend to deteriorate after a certain period of time, i.e., suffer from an increase in viscosity or gelation, due to the violent shear forces and frictional heat generated in fluid coupling. Accordingly, they lose their fluid coupling function.
Thus, Japanese Patent 55-18457[18457/80] proposes a working fluid comprising a fluid organopolysiloxane which contains a polysiloxane possessing the N-phenylaminophenyl group and with a degree of polymerization of ≦40. This working fluid is relatively stable with regard to gelation and viscosity increases at high temperatures and high shear forces.
However, the preceding method suffers from the problem that long-term use in fluid coupling causes a decline in the organopolysiloxane's viscosity due to the high shear forces. A gradual decline in the torque transmission ratio occurs and the fluid coupling function is lost.
SUMMARY OF THE INVENTION
The object of the present invention is to overcome the aforementioned problems by providing a viscous fluid coupling organopolysiloxane composition which is stable on the long-term and which does not undergo torque variations even at high shear forces.
Said object is achieved by a viscous fluid coupling organopolysiloxane composition which is characterized by a composition comprising: An organopolysiloxane composition for viscous fluid coupling, comprising: (i) a liquid organopolysiloxane having the average unit formula R a SiO.sub.(4-a)/2 wherein R is a monovalent hydrocarbon radical and a is 1.7 to 2.3; and (ii) a reaction product of (A) an organopolysiloxane having the formula R' b SiO.sub.(4-b)/2 wherein R' is a monovalent hydrocarbon group and b is 1.4 to 2.3 with (B) from 0.01 to 10 parts by weight of an aromatic aminophenol per 100 parts of said organopolysiloxane (A), in the presence of(C) from 0.001 to 1.0 part by weight of a quaternary phosphonium hydroxide per 100 parts of said organopolysiloxane (A), wherein the viscosity of said component (ii) is within 20 percent of the viscosity of said component (i) and said component (ii) is present in such quantity that the aromatic aminophenyl groups of said aromatic aminophenol constitutes from 0.01 to 2.00 percent by weight of the total weight of (i) plus (ii). Said object is also achieved when the reaction product (ii) is prepared in the presence of from 0.001 to 1.0 part by weight of a quaternary phosphonium hydroxide per 100 parts of said organopolysiloxane (A) and in the presence of from 0 to 20 parts by weight of an organopolysiloxane cyclic having the general formula ##STR1## per 100 parts of said organopolysiloxane (A), wherein R is a monovalent hydrocarbon group and n is a integer having a value of 3 to 6.
DETAILED DESCRIPTION OF THE INVENTION
By way of explanation of the present invention, the component (i) used in the present invention is the principal component of this composition and is to have the average unit formula
R.sub.a SiO.sub.(4-a)/2.
In this formula, R is a monovalent hydrocarbon group and is exemplified by alkyl groups such as methyl, ethyl, propyl and butyl; substituted alkyl groups such as 2-phenylethyl, 2-phenylpropyl and 3,3,3-trifluoropropyl; alkenyl groups such as vinyl and propenyl; and aryl and substituted aryl groups such as phenyl, tolyl and xylyl. Alkyl and aryl groups are preferred and methyl and phenyl groups are particularly preferred. Furthermore, this component may contain a small quantity of silicon-bonded hydrogen atoms, silicon-bonded hydroxyl groups or silicon-bonded alkoxy groups. In the above formula, a may range from 1.7 to 2.3.
The structure of this component may be straight chain, branched chain, cyclic or network, but straight chain or branched chain is preferred. The terminal group is preferably an organosiloxy group such as a trialkylsiloxy or alkenyldialkylsiloxy group, or an alkoxy or hydroxyl group.
The viscosity of this component is not specifically restricted, but is preferably 100 to 1,000,000 cS at 25° C. from the standpoint of torque transmission, and is more preferably 1,000 to 100,000 cS.
Concrete examples of this component are trimethylsiloxy group-terminated dimethylpolysiloxanes, dimethylvinylsiloxy group-terminated dimethylpolysiloxanes, trimethylsiloxy group-terminated dimethylsiloxane-methylvinylsiloxane copolymers, trimethylsiloxy group-terminated dimethylsiloxane-methylphenylsiloxane copolymers, trimethylsiloxy group-terminated methylphenylpolysiloxanes, hydroxyl group-terminated dimethylpolysiloxanes, hydroxyl group-terminated dimethylsiloxane-methylphenylsiloxane copolymers, and copolymers composed of trimethylsiloxane units and SiO2 units. Also usable are mixtures of a single type, or two or more types, with different structures and/or different numbers of siloxane units.
The component (ii) used by the present invention is the product of the reaction of (A) organopolysiloxane with (B) aromatic aminophenol in the presence of (C) quaternary phosphonium hydroxide. Moreover, its viscosity must be within ±20% of the viscosity of component (i). Its function is to suppress any decline in the torque transmission ratio by the organopolysiloxane composition of the present invention at high shear forces.
The organopolysiloxane (A) used to produce component (ii) is organopolysiloxane with the average unit formula
R.sup.1.sub.b SiO.sub.(4-b)/2.
In this formula, R 1 is a monovalent hydrocarbon group and its examples are the same as for R in component (i) and b is 1.4 to 2.3.
The structure of this component may be straight chain, branched chain, cyclic or network, but straight chain or branched chain is preferred. The terminal is preferably an organosiloxy group such as a trialkylsiloxy or alkenyldialkylsiloxy group, or an alkoxy group or hydroxyl group.
The viscosity of the organopolysiloxane of the present component must exceed at least -20% of the viscosity of component (i). The reason for this is that the reaction of this component with component (B) results in a small decline in viscosity, with the result that the viscosity of the reaction product might otherwise not exceed -20% of the viscosity of component (i).
Concrete examples of this component are the same as for component (i).
Concrete examples of the aromatic aminophenol (B) used to produce component (ii) are ##STR2##
The quaternary phosphonium hydroxide (C) used to produce component (ii) has the formula
R.sup.2.sub.4 POH
wherein R 2 may be an alkyl group such as methyl, ethyl, propyl, butyl or octyl. Alternatively, R 2 may be an aryl group such as phenyl. Mixtures of R 2 groups are also suitable herein, leading to such compounds as methyltriphenylphosphonium hydroxide, for example.
The reaction product comprising component (ii) is produced by reacting organopolysiloxane (A) with aromatic aminophenol (B) in the presence of quaternary phosphonium hydroxide (C).
The reaction ratio between organopolysiloxane (A) and aromatic aminophenol (B) is preferably in the range of 0.01 to 10 parts by weight component (B) per 100 parts by weight component (A) and more preferably in the range of 0.1 to 5 parts by weight component (B) per 100 parts by weight component (A) from the standpoint of reducing the quantity of unreacted component (A) and/or component (B).
The use ratio of component (C) is preferably in the range of 0.001 to 1.0 part by weight component (C) per 100 parts by weight component (A) and more preferably in the range of 0.01 to 0.1 part by weight component (C) per 100 parts by weight component (A).
The reaction temperature is preferably 130°-280° C. and more preferably 150°-250° C.
The reaction atmosphere is the ambient or an inert gas atmosphere.
During this reaction, the reaction mixture first undergoes a gradual decline in viscosity, followed by a nearly constant value, and the reaction is taken to be complete at this point.
Furthermore, a small quantity of organopolysiloxane cyclic can be added to accelerate the reaction. In this case, the cyclic component is preferably stripped off at elevated temperatures under reduced pressures after the reaction.
Also, when unreacted component (A) and/or component (B) remains in the reaction product, they are removed after the reaction by means such as, for example, filtration, in order to obtain a homogeneous, transparent liquid reaction product.
The viscosity of this reaction product must be within ±20% of the viscosity of component (i) from the standpoint of preventing any decline in the torque transmission ratio of the composition of the present invention. It is preferably within ±10% and more preferably within ±5%.
Component (ii) is to be added in a quantity such that the total weight of aromatic aminophenyl groups in component (ii) is 0.01 to 2.00 wt %, and preferably 0.05 to 1.00 wt %, based on the total weight of component (i) plus component (ii).
The composition of the present invention is produced by simply mixing component (i) and component (ii) in the prescribed ratio.
The present invention will be explained in detail using examples of execution. In the examples, "part" denotes "part by weight" and "%" denotes "wt %" and the viscosity is the value measured at 25° C.
EXAMPLE 1
To 100 parts trimethylsiloxy group-terminated dimethylpolysiloxane with a viscosity of 12,500 cS were added 0.6 parts N-phenylaminophenol and 0.03 parts tetrabutylphosphonium hydroxide, followed by mixing at room temperature to obtain a homogeneous dispersion. This mixture was reacted at a temperature of 200° C. under a nitrogen atmosphere. The viscosity reached a nearly constant value 2 hours after the start of the reaction and the reaction product was then cooled to room temperature. The reaction product was then combined with diatomaceous earth and subsequently purified by filtration. The obtained reaction product was a light-yellow, transparent liquid with a viscosity of 5,500 cS.
Ten parts of this reaction product was added to 100 parts of a trimethylsiloxy group-terminated dimethylpolysiloxane with a viscosity of 4,900 cS followed by mixing to homogeneity at room temperature in order to obtain an organopolysiloxane oil with a viscosity of 5,000 cS and an N-phenylaminophenyl group content of 0.05%.
This organopolysiloxane oil was filled into a fluid-coupling device which was then operated continuously at 6,500 rpm and the variation in the output rpm was measured.
The results are reported in Table 1.
COMPARISON EXAMPLE 1
A trimethylsiloxy group-terminated dimethylpolysiloxane with viscosity of 5,000 cS was filled into the fluid-coupling device, which was then continuously operated at 6,500 rpm and the variation in the output rpm is measured.
The results are reported in Table 1.
COMPARISON EXAMPLE 2
To 100 parts trimethylsiloxy group-terminated dimethylpolysiloxane with a viscosity of 5,000 cS was added 0.5 parts organopolysiloxane with the formula ##STR3## and this was then mixed at room temperature to homogeneity.
This organopolysiloxane oil was filled into the fluid-coupling device, which was subsequently continuously operated at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
EXAMPLE 2
To 100 parts trimethylsiloxy group-terminated dimethylpolysiloxane with a viscosity of 1,800 cS was added 10 parts dimethylsiloxane cyclic tetramer. This was mixed at room temperature to homogeneity, then heated to 200° C., 0.8 part N-phenylaminophenol and 0.05 part tetrabutylphosphonium hydroxide were added and this was then reacted at the same temperature under a nitrogen atmosphere. The viscosity reached a nearly constant value 20 minutes after the start of the reaction and the dimethylsiloxane cyclic tetramer was then removed at 200° C./10 mmHg. The reaction product was cooled to room temperature, combined with diatomaceous earth and then purified by filtration. The obtained reaction product was a light-yellow, transparent liquid with a viscosity of 1,000 cS.
Twenty parts of this reaction product was added to 100 parts trimethylsiloxy group-terminated dimethylpolysiloxane with a viscosity of 1,000 cS, followed by mixing at room temperature to homogeneity to obtain an organopolysiloxane oil with a viscosity of 1,000 cS and a 0.13% content of N-phenylaminophenyl groups.
This organopolysiloxane oil was filled into the fluid-coupling device, which was subsequently continuously operated at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
Example 3
To 100 parts of trimethylsiloxy group-terminated dimethylsiloxane-diphenylsiloxane copolymer with a viscosity of 10,000 cS (10 mol% diphenylsiloxane units) were added 2.0 parts N-naphthylaminophenol and 0.01 part methyltriphenylphosphonium hydroxide and this was then mixed at room temperature to obtain a homogeneous dispersion. The resulting mixture was then reacted in air at 150° C. The viscosity reached a nearly constant value 2 hours after the start of the reaction and the reaction mixture was then cooled to room temperature, combined with diatomaceous earth and purified by filtration. The obtained reaction product was a light-yellow, transparent liquid with a viscosity of 2,520 cS.
One hundred parts of this reaction product was added to 100 parts of a trimethylsiloxy group-terminated dimethylsiloxane-diphenylsiloxane copolymer with a viscosity of 2,500 cS (10 mol% diphenylsiloxane units) and this was then mixed at room temperature to homogeneity to obtain an organopolysiloxane oil with a viscosity of 2,510 cS and a 0.89% content of N-naphthylaminophenyl groups.
This organopolysiloxane oil was filled into the fluid-coupling device which was then operated continuously at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
Comparison Example 3
A trimethylsiloxy group-terminated dimethylsiloxanediphenylsiloxane copolymer with a viscosity of 2,500 cS and a diphenylsiloxane unit content of 10 mol % was filled into the fluid-coupling device, which was then run continuously at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
EXAMPLE 4
One hundred parts hydroxyl group-terminated dimethylpolysiloxane with a viscosity of 30,000 cS was combined with 5 parts dimethylsiloxane cyclic tetramer and this was mixed at room temperature to homogeneity. After heating to 250° C., 1.5 parts N-(N-phenylamino phenyl)aminophenol and 0.02 part tetramethylphosphonium hydroxide were added and a reaction was carried out at this temperature under a nitrogen atmosphere. The viscosity reached a nearly constant value 10 minutes after the start of the reaction and the dimethylsiloxane cyclic tetramer was then stripped at 250° C./10 mmHg. The reaction product was cooled to room temperaturecombined with diatomaceous earth and then purified by filtration. The obtained reaction product was a light-yellow, transparent liquid with a viscosity of 13,400 cS.
Ten parts of this reaction product was added to 100 parts hydroxyl group-terminated dimethylpolysiloxane with a viscosity of 12,500 cS and this was then mixed at room temperature to homogeneity in order to obtain an organopolysiloxane oil with a viscosity of 12,600 cS and a 0.13% content of N-(N-phenylaminophenyl)aminophenyl groups.
This organopolysiloxane oil was filled into the fluid-coupling device, which was then run continuously at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
COMPARISON EXAMPLE 4
To 100 parts hydroxyl group-terminated dimethylpolysiloxane with a viscosity of 12,500 cS was added 0.6 part organopolysiloxane with the formula ##STR4## and this was then mixed at room temperature to homogeneity.
This organopolysiloxane oil was filled into the fluid-coupling device which was subsequently run continuously at 6,500 rpm and the variation in output rpm was measured.
The results are reported in Table 1.
TABLE 1__________________________________________________________________________ Initial Fluid Viscosity Viscosity Output RPM After 300 HoursNo. (cS) 1 Hour 50 Hours 100 Hours 300 Hours of Operation (cS)__________________________________________________________________________Example 1 5000 4150 4110 4090 4080 4940Example 2 1000 2840 2830 2810 2820 992Example 3 2510 3010 2990 2970 2950 2420Example 4 12600 4750 4740 4800 4920 13900Comparison 5000 4160 4390 gelation -- --Example 1Comparison 5000 4140 3880 3690 3890 4750Example 2Comparison 2500 3000 2820 2680 2420 1910Example 3Comparison 12500 4750 4620 4520 gelation --Example 4__________________________________________________________________________
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A composition for viscous fluid coupling is described. The composition comprises a liquid organopolysiloxane and a reaction product of a liquid organopolysiloxane with an aromatic aminophenol in the presence of a quaternary phosphonium hydroxide. The composition is characterized by a long term stability, undergoing little torque variation even at elevated temperatures and high shear forces.
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[0001] This invention is a divisional application of U.S. patent application Ser. No. 12/378,670 filed Feb. 18, 2009, which is a divisional application of U.S. patent application Ser. No. 11/246,825 filed Oct. 7, 2005, now U.S. Pat. No. 7,517,409, which is a divisional application of U.S. patent application Ser. No. 10/649,288 filed Aug. 27, 2003, now U.S. Pat. No. 7,160,574, and claims the benefit of priority to U.S. Provisional Patent Application 60/406,602 filed Aug. 28, 2002.
FIELD OF INVENTION
[0002] This invention relates to piping repair and restoration, and in particular to methods, systems and apparatus for cleaning and providing barrier protective coatings to the interior walls of small metal and plastic type pipes such as drain lines, hot water lines, cold water lines, potable water lines, natural gas lines, HVAC piping systems, drain lines, and fire sprinkler system lines, and the like, that are used in multi-unit residential buildings, office buildings, commercial buildings, and single family homes, and the like.
BACKGROUND AND PRIOR ART
[0003] Large piping systems such as those used in commercial buildings, apartment buildings, condominiums, as well as homes and the like that have a broad base of users commonly develop problems with their pipes such as their water and plumbing pipes, and the like. These problems can include leaks caused by pipe corrosion and erosion, as well as blockage from mineral deposits that develop over time where materials build up directly inside the pipes. Presently when a failure in a piping system occurs the repair method may involve a number of applications. Those repair applications may involve a specific repair to the area of failure such as replacing that section of pipe or the use of a clamping devise and a gasket. In some cases the complete piping system of the building may need to be replaced.
[0004] In the case of pipes where the water flow has been impeded by rust build up or by a deposit build up such as calcium and other minerals, various methods for the removal of the rust or other build up have been used. However the damage caused by the rust or from other deposits to the pipe wall cannot be repaired unless the pipe is replaced.
[0005] Traditional techniques to correct for the corrosion, leakage and blockage problems have included replacing some or all of a building's pipes. In addition to the large expense for the cost of the new pipes, additional problems with replacing the pipes include the immense labor and construction costs that must be incurred for these projects.
[0006] Most piping systems are located behind finished walls or ceilings, under floors, in concrete or underground. From a practical viewpoint simply getting to the problem area of the pipe to make the repair can create the largest problem. Getting to the pipe for making repairs can require tearing up the building, cutting concrete and/or having to dig holes through floors, the foundation or the ground. These labor intensive repair projects can include substantial demolition of a buildings walls and floors to access the existing piping systems. For example, tearing out the interior walls to access the pipes is an expected result of the demolition.
[0007] Once the walls and floors have been opened, then the old pipes are usually pulled out and thrown out as scrap, which is then followed by replacement with new pipes. These prior techniques do little if nothing to reuse, refix, or recycle the old pipes.
[0008] In addition, there are usually substantial costs for removing the debris and old pipes from the worksite. With these projects both the cost of new pipes and the additional labor to install these pipes are required expenditures. Further, there are additional added costs for the materials and labor to replumb these new pipes along with the necessary wall and floor repairs that must be made to clean up for the demolition effects. For example, getting at and fixing a pipe behind drywall is not completing the repair project. The drywall must also be repaired, and just the drywall type repairs can be extremely costly. Additional expenses related to the repair or replacement of an existing piping system will vary depending primarily on the location of the pipe, the building finishes surrounding the pipe and the presence of hazardous materials such as asbestos encapsulating the pipe. Furthermore, these prior known techniques for making piping repair take considerable amounts of time that can include many months or more to be completed which results in lost revenue from tenants and occupants of commercial type buildings since tenants cannot use the buildings until these projects are completed.
[0009] Finally, the current pipe repair techniques are usually only temporary. Even after encountering the cost to repair the pipe, the cost and inconvenience of tearing up walls or grounds and if a revenue property the lost revenue associated with the repair or replacement, the new pipe will still be subject to the corrosive effects of fluids such as water that passes through the pipes.
[0010] Over the years many attempts have been proposed for cleaning water type pipes with chemical cleaning solutions. See for example, U.S. Pat. Nos. 5,045,352 to Mueller; 5,800,629 to Ludwig et al.; 5,915,395 to Smith; and 6,345,632 to Ludwig et al. However, all of these systems require the use of chemical solutions such as liquid acids, chlorine, and the like, that must be run through the pipes as a prerequisite prior to any coating of the pipes. The National Sanitation Foundation (NSF) specifically does not allow the use of any chemical agent solutions for use with cleaning potable water piping systems. Thus, these systems cannot be legally used in the United States for cleaning out water piping systems.
[0011] Other systems have been proposed that use dry particulate materials as a cleaning agent that is sprayed from mobile devices that travel through or around the pipes. See U.S. Pat. Nos. 4,314,427 to Stolz; and 5,085,016 to Rose. However, these traveling devices require large diameter pipes to be operational and cannot be used inside of pipes that are less than approximately 6 inches in diameter, and would not be able to travel around narrow bends. Thus, these devices cannot be used in small diameter pipes found in potable water piping systems that also have sharp and narrow bends.
[0012] The proposed systems and devices referenced above generally require sectioning a small pipe length for cleaning and coating type applications, or limiting the application to generally straight elongated pipe lengths. For large building such as multistory applications, the time and cost to section off various piping sections would be cost prohibitive. None of the prior art is known to be able to service an entire building's water type piping system at one time in one complete operation.
[0013] Thus, the need exists for solutions to the above problems with fixing existing piping systems in buildings.
SUMMARY OF THE INVENTION
[0014] A primary objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes in buildings without having to physically remove and replace the pipes.
[0015] A secondary objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes by initially cleaning the interior walls of the pipes.
[0016] A third objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes by applying a corrosion protection barrier coating to the interior walls of the pipes.
[0017] A fourth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes in buildings in a cost effective and efficient manner.
[0018] A fifth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes which is applicable to small diameter piping systems from approximately ⅜″ to approximately 6″ in piping systems made of various materials such as galvanized steel, black steel, lead, brass, copper or other materials such as composites including plastics, as an alternative to pipe replacement.
[0019] A sixth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes which is applied to pipes, “in place” or insitu minimizing the need for opening up walls, ceilings, or grounds.
[0020] A seventh objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes which minimizes the disturbance of asbestos lined piping or walls/ceilings that can also contain lead based paint or other harmful materials.
[0021] An eighth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where once the existing piping system is restored with a durable epoxy barrier coating the common effects of corrosion from water passing through the pipes will be delayed if not stopped entirely.
[0022] A ninth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes to clean out blockage where once the existing piping system is restored, users will experience an increase in the flow of water, which reduces the energy cost to transport the water. Additionally, the barrier epoxy coating being applied to the interior walls of the pipes can create enhanced hydraulic capabilities again giving greater flow with reduced energy costs.
[0023] A tenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where customers benefit from the savings in time associated with the restoration of an existing piping system.
[0024] An eleventh objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where customers benefit from the economical savings associated with the restoration of an existing piping system, since walls, ceilings floors, and/or grounds do not always need to be broken and/or cut through.
[0025] A twelfth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where income producing properties experience savings by remaining commercially usable, and any operational interference and interruption of income-producing activities is minimized.
[0026] A thirteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where health benefits had previously accrued, as the water to metal contact will be stopped by a barrier coating thereby preventing the leaching of metallic and potentially other harmful products from the pipe into the water supply such as but not limited to lead from solder joints and from lead pipes, and any excess leaching of copper, iron and lead.
[0027] A fourteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the pipes are being restored in-place thus causing less demand for new metallic pipes, which is a non-renewable resource.
[0028] A fifteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes using a less intrusive method of repair where there is less building waste and a reduced demand on expensive landfills.
[0029] A sixteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the process uses specially filtered air that reduces possible impurities from entering the piping system during the process.
[0030] A seventeenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the equipment package is able to function safely, cleanly, and efficiently in high customer traffic areas.
[0031] An eighteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the equipment components are mobile and maneuverable inside buildings and within the parameters typically found in single-family homes, multi unit residential buildings and various commercial buildings.
[0032] A nineteenth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the equipment components can operate quietly, within the strictest of noise requirements such as approximately seventy four decibels and below when measured at a distance of approximately several feet away.
[0033] A twentieth objective of the invention is to provide methods, systems and devices for repairing interior walls of pipe where the barrier coating material for application in a variety of piping environments, and operating parameters such as but not limited to a wide temperature range, at a wide variety of airflows and air pressures, and the like.
[0034] A twenty first objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the barrier coating material and the process is functionally able to deliver turnaround of restored piping systems to service within approximately twenty four hours or less or no more than approximately ninety six hours for large projects.
[0035] A twenty second objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the barrier coating material is designed to operate safely under NSF(National Sanitation Foundation) Standard 61 criteria in domestic water systems, with adhesion characteristics within piping systems in excess of approximately 400 PSI.
[0036] A twenty third objective of the invention is to provide methods, systems and devices for repairing interior walls of pipes where the barrier coating material is designed as a long-term, long-lasting, durable solution to pipe corrosion, pipe erosion, pinhole leak and related water damage to piping systems where the barrier coating extends the life of the existing piping system.
[0037] A twenty fourth objective of the invention is to provide methods, systems and devices for both cleaning and coating interiors of pipes having diameters of up to approximately 6 inches using dry particulates, such as sand and grit, prior to coating the interior pipe walls.
[0038] A twenty fifth objective of the invention is to provide methods, systems and devices for both cleaning and coating interiors of pipes having diameters of up to approximately 6 inches in plural story buildings, without having to section off small sections of piping for cleaning and coating applications.
[0039] A twenty sixth objective of the invention is to provide methods, systems and devices for cleaning the interiors of an entire piping system in a building in a single pass run operation.
[0040] A twenty seventh objective of the invention is to provide methods, systems and devices for barrier coating the interiors of an entire piping system in a building in a single pass run operation.
[0041] The novel method and system of pipe restoration prepares and protects small diameter piping systems such as those within the diameter range of approximately ⅜ of an inch to approximately six inches and can include straight and bent sections of piping from the effects of water corrosion, erosion and electrolysis, thus extending the life of small diameter piping systems. The barrier coating used as part of the novel process method and system, can be used in pipes servicing potable water systems, meets the criteria established by the National Sanitation Foundation (NSF) for products that come into contact with potable water. The epoxy material also meets the applicable physical criteria established by the American Water Works Association as a barrier coating. Application within buildings ranges from single-family homes to smaller walk-up style apartments to multi-floor concrete high-rise hotel/resort facilities and office towers, as well as high-rise apartment and condominium buildings and schools. The novel method process and system allows for barrier coating of potable water lines, natural gas lines, HVAC piping systems, hot water lines, cold water lines, drain lines, and fire sprinkler systems.
[0042] The novel method of application of an epoxy barrier coating is applied to pipes right within the walls eliminating the traditional destructive nature associated with a re-piping job. Typically 1 riser system or section of pipe can be isolated at a time and the restoration of the riser system or section of pipe can be completed in less than one to four days (depending upon the building size and type of application) with water restored within approximately 24 to approximately 96 hours. For hotel and motel operators that means not having to take rooms off line for extended periods of time. Too, for most applications, there are no walls to cut, no large piles of waste, no dust and virtually no lost room revenue. Entire building piping systems can be cleaned within one run through pass of using the invention. Likewise, an entire building piping system can be coated within one single pass operation as well.
[0043] Once applied, the epoxy coating creates a barrier coating on the interior of the pipe. The application process and the properties of the epoxy coating ensure the interior of the piping system is fully coated. Epoxy coatings are characterized by their durability, strength, adhesion and chemical resistance, making them an ideal product for their application as a barrier coating on the inside of small diameter piping systems.
[0044] The novel barrier coating provides protection and extended life to an existing piping system that has been affected by erosion corrosion caused from internal burrs, improper soldering, excessive turns, and excessive water velocity in the piping system, electrolysis and “wear” on the pipe walls created by suspended solids. The epoxy barrier coating will create an approximately 4 mil or greater covering to the inside of the piping system.
[0045] There are primarily 3 types of metallic piping systems that are commonly used in the plumbing industry—copper, steel and cast iron. New steel pipes are treated with various forms of barrier coatings to prevent or slow the effects of corrosion. The most common barrier coating used on steel pipe is the application of a zinc based barrier coat commonly called galvanizing. New copper pipe has no barrier coating protection and for years was thought to be corrosion resistant offering a lifetime trouble free use as a piping system.
[0046] Under certain circumstances that involved a combination of factors of which the chemistry of water and installation practices a natural occurring barrier coating would form on the inside of copper pipes which would act as a barrier coating, protecting the copper piping system against the effects of corrosion from the water.
[0047] In recent history, due to changes in the way drinking water is being treated and changes in installation practices, the natural occurring barrier coating on the inside of copper pipe is not being formed or if it was formed is now being washed away. In either case without an adequate natural occurring barrier coating, the copper pipe is exposed to the effects of corrosion/erosion, which can result in premature aging and failure of the piping system.
[0048] With galvanized pipe the zinc coating wears away leaving the pipe exposed to the effects of the corrosive activity of the water. This results in the pipe rusting and eventually failing.
[0049] The invention can also be used with piping systems having plastic pipes, PVC pipes, composite material, and the like.
[0050] The novel method and system of corrosion control by the application of an epoxy barrier coating to new or existing piping systems is a preventative corrosion control method that can be applied to existing piping systems in-place.
[0051] The invention includes novel methods and equipment for providing barrier coating corrosion control for the interior walls of small diameter piping systems. The novel process method and system of corrosion control includes at least three basic steps: Air Drying a piping system to be serviced; profiling the piping system using an abrasive cleaning agent; and applying the barrier coating to selected coating thickness layers inside the pipes. The novel invention can also include two additional preliminary steps of: diagnosing problems with the piping system to be serviced, and planning and setting up the barrier coating project onsite. Finally, the novel invention can include a final end step of evaluating the system after applying the barrier coating and re-assembling the piping system.
[0052] Further objects and advantages of this invention will be apparent from the following detailed description of the presently preferred embodiments which are illustrated schematically in the accompanying drawings.
BRIEF DESCRIPTION OF THE FIGURES
[0053] FIG. 1 shows the general six steps that is an overview for applying the barrier coating.
[0054] FIGS. 2A , 2 B, 2 C and 2 D shows a detailed process flowchart using the steps of FIG. 1 for providing the barrier coating.
[0055] FIG. 3 shows a side view of a multi-story story building using the novel barrier coating corrosion control method and system of the invention.
[0056] FIG. 4 shows a side view of the novel exhaust air diffuser used in the barrier coating control system in FIG. 3 .
[0057] FIG. 5A shows a perspective view of the novel portable air distribution manifold used in the barrier coating control system in FIG. 3 .
[0058] FIG. 5B shows a side view of the novel Pressure Generator System (Sander) 500 used in the barrier coating control system of FIG. 3 .
[0059] FIG. 5C is an enlarged view of the front control panel for use with the pressure generator system 500 of FIG. 5B .
[0060] FIG. 6A shows a side view of the novel Abrasive Reclaim Separator Module (Pre-Filter) used in the barrier coating control system of FIG. 3 .
[0061] FIG. 6B shows an end view of the novel Abrasive Reclaim Separator Module (Pre-Filter) used in the barrier coating control system of FIG. 3 .
[0062] FIG. 7A shows a side view of the novel Dust Collector System 700 (Filter) used in the barrier coating control system of FIG. 3
[0063] FIG. 7B shows an enlarged side cross-sectional view of the mounted Cartridge Filters used in the Dust Collector System of FIG. 7A .
[0064] FIG. 8A shows a perspective view of the novel Portable Epoxy Metering and Dispensing Unit 800 (Epoxy Mixer) used in the barrier coating control system of FIG. 3
[0065] FIG. 8B shows another perspective view of the novel Portable Epoxy Metering and Dispensing Unit 800 (Epoxy Mixer) used in the barrier coating control system of FIG. 3
[0066] FIG. 8C shows an enlarged view of the foot dispenser activator a part of the novel Portable Epoxy Metering and Dispensing Unit 800 (Epoxy Mixer) used in the barrier coating control system of FIG. 3
[0067] FIG. 8D is an enlarged view of the mixing tubes and mixing head of FIG. 8B .
[0068] FIG. 9 shows a side view of the novel Main Air Header and Distributor 200 (Header) used in the barrier coating control system of FIG. 3
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0069] Before explaining the disclosed embodiments of the present invention in detail it is to be understood that the invention is not limited in its application to the details of the particular arrangements shown since the invention is capable of other embodiments. Also, the terminology used herein is for the purpose of description and not of limitation.
[0070] FIG. 1 shows the general six steps for a project overview for applying the barrier coating to an existing piping system, which include step one, 10 program diagnosis, step two, 20 project planning, step three, 30 drying piping system, step four 40 , profiling the piping system, step five, 50 barrier coating interior walls of the pipes in the piping system, and final step six 60 evaluation and return to operation of the piping system.
Step One—Problem Diagnosis 10
[0071] For step one, 10 , several steps can be done to diagnose the problem with a piping system in a building, and can include:
(a) Interview onsite engineering staff, property mangers, owners or other property representatives as to the nature of the current problem with the piping system. (b) Evaluation of local and on-site water chemistry being used in the piping system for hardness and aggressive qualities. (c) Engineering evaluation, if necessary, to determine extent of present damage to the wall thickness of the piping and overall integrity of the piping system. (d) Additional on-site testing of piping system, if necessary, identifying leaks or the nature or extent of leaking. (e) Corrosion control proposal development for client, including options for pipe and fitting replacement where necessary.
[0077] After completion of step one, 10 , the project planning and setup step 20 can be started.
Step Two—Project Planning and Setup 20
[0078] For step two, 20 , several steps can be followed for planning and setup for restoring the integrity of the piping system in a building, and can include:
(a) Complete contract development with client, after the diagnosis contract has started. (b) Commence project planning with site analysis crew, project management team, and on-site engineering/maintenance staff (c) Plan delivery of the equipment and supplies to the worksite. (d) Complete equipment and supply delivery to worksite. (e) Commence and complete mechanical isolation of the piping system. (f) Commence and complete set up of hosing and equipment.
Step Three—Air Drying—Step 1 Method of Corrosion Control 30
[0085] For step three, 30 , the piping system to be prepared for the coating by drying the existing pipes, and can include:
(a) Piping systems are mapped. (b) Isolations of riser systems or pipe sections are prepared and completed. (c) The isolated piping system to receive the barrier coating is adapted to be connected to the barrier coating equipment. (d) The isolated riser system is drained of water. (e) Using moisture and oil free, hot compressed air, a flushing sequence is completed on the riser system to assure water is removed. (f) Riser system is then dried with heated, moisture and oil free compressed air. (g) Length of drying sequence is determined by pipe type, diameter, length complexity, location and degree of corrosion contained within the piping system, if any. (h) Inspections are completed to assure a dry piping system ready for the barrier coating.
Step Four—Piping System Profiling—Step 2 of Method of Corrosion Control 40
[0094] For step four, 40 , the piping system is to be profiled, and can include:
(a) Dried pipes can be profiled using an abrasive agent in varying quantities and types. The abrasive medium can be introduced into the piping system by the use of the moisture and oil free heated compressed air using varying quantities of air and varying air pressures. The amount of the abrading agent is controlled by the use of a pressure generator. (b) The abraded pipe, when viewed without magnification, must be generally free of all visible oil, grease, dirt, mill scale, and rust. Generally, evenly dispersed, very light shadows, streaks, and discolorations caused by stains of mill scale, rust and old coatings may remain on no more than approximately 33 percent of the surface. Also, slight residues of rust and old coatings may be left in the craters of pits if the original surface is pitted. (c) Pipe profiling is completed to ready the pipe for the application of the barrier coating material. (d) Visual inspections can be made at connection points and other random access areas of the piping system to assure proper cleaning and profiling standards are achieved. (e) An air flushing sequence is completed to the riser system to remove any residuals left in the piping system from the profiling stage.
Step Five—Corrosion Control Epoxy Sealing and Protection of the Piping—Step 3 of the Method of Corrosion Control 50
[0100] For step five, 50 , the piping system is to barrier coated and can include:
(a) Piping system can be heated with hot, pre-filtered, moisture and oil free compressed air to an appropriate standard for an epoxy coating application. (b) Piping system can be checked for leaks. (c) Corrosion control barrier coating material can be prepared and metered to manufacturer's specifications using a proportionator. (d) Corrosion control barrier coating material can be injected into the piping system using hot, pre-filtered, moisture and oil free compressed air at temperatures, air volume and pressure levels to distribute the epoxy barrier coating throughout the pipe segment, in sufficient amounts to eliminate the water to pipe contact in order to create an epoxy barrier coating on the inside of the pipe. (e) The epoxy barrier coating can be applied to achieve coating of approximately 4 mils and greater. (f) Once the epoxy barrier coating is injected warm, pre-filtered, moisture and oil free compressed air can be applied over the internal surface of the pipe to achieve the initial set of the epoxy barrier coating. (g) Confirm that all valves and pipe segments support appropriate air flow indicating clear passage of the air through the pipe i.e.: no areas of blockage. Allow the barrier coating to cure to manufacturer's standards.
Step Six—System Evaluation and Re-Assembly 60
[0108] The final step six, 60 allows for restoring the piping system to operation and can include:
(a) Remove all process application fittings. (b) Examine pipe segments to assure appropriate coating standards. (c) Re-confirm that all valves and pipe segments support appropriate air flow. (d) Install original valves, fittings/fixtures, or any other fittings/fixtures as specified by building owner representative. (e) Reconnect water system, and water supply. (f) Complete system checks, testing and evaluation of the integrity of the piping system. (g) Complete a water flush of system, according to manufacturer's specifications. (h) Evaluate water flow and quality. (i) Document riser schedule, and complete pipe labeling.
[0118] FIGS. 2A , 2 B, 2 C and 2 D show a detailed process flowchart using the steps of FIG. 1 for providing the barrier coating. These flow chart figures show a preferred method of applying a novel barrier coating corrosion control for the interior of small diameter piping systems following a specific breakdown of a preferred application of the invention.
[0119] FIG. 3 shows a side view of a ten story building setup for using the novel method and system of the invention. Components in FIG. 3 will now be identified as follows:
[0000]
IDENTIFIER
EQUIPMENT
100
395, 850, 1100, 1600 CFM Compressors Outfitted with
Aftercooler, Water separator, Fine Filter and Reheater
200
Main Air Header and Distributor (Main Header)
300
Exhaust Air Diffuser (Muffler)
400
Portable Air Distribution Manifold (Floor Header)
500
Pressure Generator System (Sander)
600
Reclaim Separator Module (Pre-Filter)
700
Dust Collector System (Filter)
800
Portable Epoxy Metering and Dispensing Unit
(Epoxy Mixer)
900
Epoxy Barrier Coating
[0120] Referring to FIG. 3 , components 100 - 800 can be located and used at different locations in a ten story building. The invention allows for an entire building piping system to be cleaned in one single pass through run without having to dismantle either the entire or multiple sections of the piping system. The piping system can include pipes having diameters of approximately ⅜ of an inch up to approximately 6 inches in diameter with the piping including bends up to approximately ninety degrees or more throughout the building. The invention allows for an entire building piping system to have the interior surfaces of the pipes coated in one single pass through run without having to dismantle either the entire or multiple parts of the piping system. Each of the components will now be defined.
100 Air Compressor
[0121] The air compressors 100 can provide filtered and heated compressed air. The filtered and heated compressed air employed in various quantities is used, to dry the interior of the piping system, as the propellant to drive the abrasive material used in cleaning of the piping system and is used as the propellant in the application of the epoxy barrier coating and the drying of the epoxy bather coating once it has been applied. The compressors 100 also provide compressed air used to propel ancillary air driven equipment.
200 Main Air Header and Distributor
[0122] An off the shelf main header and distributor 200 shown in FIGS. 3 and 9 can be one Manufactured By:Media Blast & Abrasives, Inc. 591 W. Apollo Street Brea, Calif. 92821 The components of the main header and distributor of FIG. 9 are labeled as follows.
Description of Main Header Equipment Describing Each Component:
[0000]
12 & 14 Gauge Steel Construction
Approximate Dimensions: 28″w×27″l×53″h
Ford Grabber Blue Powder-coating
Air Pressure Gauge 205
Regulator Adjustment 210
Air Pressure Regulator 215
Moisture Bleeder Valve 220
2 2″ NPT Inlet With Full Port Ball Valve 225
14-1″ Side-Mounted Ball Valves—Regulated Air 230
4-1″ Top Mounted Ball Valves—Unregulated Air 235
1-2″ Top Mounted full port Ball Valve—Unregulated Air 240
1-2″ Top Mounted Full Port Ball Valve—Regulated Air 245
1.9 Cubic Feet Pressure Pot 250
Insulated Cabinet 255
Two Inflatable Tires 260
Push/Pull Handles 265
[0139] Referring to FIGS. 3 and 9 , the Main Header 200 provides safe air management capability from the air compressor for both regulated and unregulated air distribution (or any combination thereof) to the various other equipment components and to both the piping system risers and fixture outlets for a range of piping configurations from a single family home to a multi-story building. The air enters through the 2″ NPT inlet, 225 to service the pressure vessel. The main header 200 can manage air capacities ranging to approximately 1100 CFM and approximately 125 psi.
[0140] There are many novel parts and benefits with the Main Header and Distributor 200 . The distributor is portable and is easy to move and maneuver in tight working environments. Regulator Adjustment 210 can easily and quickly manage air capacities ranging to approximately 1600 CFM and approximately 200 psi, and vary the operating airflows to each of the other ancillary equipment associated with the invention. The Air Pressure Regulator 210 and the Method of Distributing the air allows both regulated and unregulated air management from the same equipment in a user-friendly, functional manner. The approximately 1″ Valving 230 , 235 , 245 allows accommodation for both approximately 1″ hosing and with adapters, and hose sizes of less than approximately 1′ can be used to meet a wide variety of air demand needs on a job site. The insulated cabinet 255 , surrounding air works dampens noise associated with the movement of the compressed air. The insulated cabinet 255 , helps retain heat of the pre-dried and heated compressed air, the pre-dried and heated compressed air being an integral part of the invention. The insulated cabinet 255 , helps reduce moisture in the pressure vessel and air supply passing through it. Finally, the valving of the pressure vessel allows for delivery (separate or simultaneous) of regulated air to the side mounted air outlet valves 230 , the top mounted regulated air outlet valves 245 , as well as the top mounted unregulated air outlet valves 235 and 240 .
[0141] FIG. 4 shows a side view of the novel exhaust air diffuser 300 used in the barrier coating control system in FIG. 3 .
300 Exhaust Air Diffuser (Muffler)
[0142] Referring to FIGS. 3 and 4 , an exhaust air diffuser and muffler 300 that can be used with the invention can be one Manufactured By:Media Blast & Abrasives, Inc. 591 W. Apollo Street, Brea, Calif. 92821.
[0000] Description of Muffler 300 components:
12 & 14 Gauge Steel Construction Approximate Dimensions: 34″w×46″1×76″h Ford Grabber Blue Powder-coating Vented Access Panels on Both Sides of Unit 305 Vented End Panels 310 Dust Drawer with Removable Pan 315 Canvas Dust Bag Diffusers 320 2″ NPT Inlet 325 4″×8″ Expansion Chamber 330 Overhead Plenum 335 Two Swivel Casters 340 Two Locking Casters 350 Push/Pull Handles 360
[0156] Referring to FIGS. 3 and 4 , the Air Diffuser/Muffler 300 allows the safe, wholesale dumping of unregulated or regulated air from the compressor off of the Main Header 200 through the approximately 2″ NPT inlet, into the expansion chamber and canvas dust bag diffusers for the purpose of controlling the air temperature in the piping system during the drying phase, the pipe warming phase, the epoxy application phase and the initial curing phase of the epoxy barrier coating material after it is injected into the piping system. The Air diffuser 300 can eliminate the need to operate the air filter 600 during various stages of the process, promoting energy efficiency as the filter 600 is an air assisted and electrically powered piece of invention.
[0157] There are many novel parts and benefits to the Exhaust air diffuser 300 . The diffuser's portability allows for easy to move and maneuver in tight working environments. Vented access panels 305 allow for safe and even distribution of the air upon venting, prevents the build up of backpressure of the venting air and reduces the noise of the venting air. A Dust Drawer with Removable Pan 315 allows for easy clean out of the expansion chamber. A Canvas Dust Bag Diffuser 320 assures quiet, customer friendly discharge of air. An approximately 2″ NPT Inlet 325 allows full range of air diffusion from approximately 1″ to approximately 2″ discharge hoses. A 4″×8″ Expansion Chamber 330 allows for rapid dispersing of the air upon entering the Air Diffuser 300 . The expansion chamber 330 permits the compressed air that enters the diffuser 300 to expand allowing for a more efficient and safe passage to exit, which reduces the noise of the air upon departure and helps reduce the build up of backpressure of the exiting air from the piping system. The Air Diffuser 300 promotes the rapid unrestricted movement of the compressed air in volumes greater than approximately 1100 CFM and can operate with air pressures greater than approximately 120 PSI. When used in conjunction with the heated, pre-filtered compressed air of the compressor 100 , the use of the Air Diffuser 300 creates a more efficient movement of the heated air, which results in a cost savings by drying the pipes faster, drying the epoxy faster, which in turn saves manpower, fuel and reduces the operational time of the compressor 100 .
[0158] FIG. 5A shows a preferred portable air distribution manifold 400 that can be used in the exemplary setup shown in FIG. 3
400 Portable Air Distribution Manifold
[0159] Referring to FIGS. 3 and 5A , an on off-the-shelf manifold 400 can be one Manufactured By: M & H Machinery 45790 Airport Road, Chilliwack, BC, Canada Description of Manifold 400 Components:
Main Air Cylinder 2½″×12″ Schedule 40 Steel Construction Ford Grabber Blue Paint Finishes 4-1″ Welded Nipples Placed at a 45° Angle to the Base Cylinder; Male Threaded 410 1″ NPT Female Threaded Portals at Each End of Cylinder 420 2 Metal Legs for Support and Elevation of Manifold 430 Pressure Rated Vessels to 125 PSI or Greater 440 Attached for Air Control, 1″ Full Port Ball Valves NPT; Female Threaded 450 All Hose End Receptors are NPT 1″; Female Threaded 460
[0168] As part of the general air distribution system set up, the floor manifolds 400 can be pressure rated vessels designed to evenly and quietly distribute the compressed air to at least 5 other points of connection, typically being the connections to the piping system. Airflow from each connection at the manifold is controlled by the use of individual full port ball valves.
[0169] There are many novel parts and benefits to the Air Manifold 400 . The portability of manifold 400 allows for easy to move and maneuver in tight working environments. The elevated legs 430 provide a stable base for unit 400 as well as keep the hose end connections off the floor with sufficient clearance to permit the operator ease of access when having to make the hose end connections. The threaded nipples 410 placed at approximately 45° angle allow for a more efficient use of space and less restriction and constriction of the airline hoses they are attached to. Multiple manifolds 400 can be attached to accommodate more than 5 outlets. The manifolds can be modular and can be used as 1 unit or can be attached to other units and used as more than 1.
[0170] FIG. 5B shows a perspective view of the novel pressure generator sander system 500 used in the barrier coating control system in FIG. 3 . FIG. 5C shows the front control panel of the sander system.
500 Pressure Generator System-Sander
[0171] Referring to FIGS. 3 , 5 B and 5 C, a pressure generator sander 500 that can be used with the invention can be one Manufactured By: Media Blast & Abrasives, Inc.591 W. Apollo Street Brea, Calif. 92821.
Description of Sander 500 Components:
[0000]
12 & 14 Gauge Steel Construction
Approximate Dimensions: 20″w×24″l×42″h
Ford Grabber Blue Powder-coating
1-1″ NPT Inlets 505
1-1″ NPT Outlet 510
3—Air Breather Mufflers 515
Pop-up Valve gasket 520
Pop-up Valve 525
Hand Port Gasket 530
Pressure Pot with Hand Port and Hopper 535
Filler Lid with Latches 540
Mixing Valve 545
Remote Regulator 550
Process Valve 555
Toggle Switch 560
Air Pressure Gauge 565
Regulator Adjustment 570
Pulse Button 580
Wheel Assembly 585
2—Inflatable Tires 590
[0192] The pressure generating sander system 500 can provide easy loading and controlled dispensing of a wide variety of abrasive medium in amounts up to approximately 1.3 US gallons at a time. The pressure generator sander can include operational controls that allow the operator to easily control the amount of air pressure and control the quantity of the abrasive medium to be dispersed in a single or multiple application. The abrasive medium can be controlled in quantity and type and is introduced into a moving air steam that is connected to a pipe or piping systems that are to be sand blasted clean by the abrasive medium. The sand can be introduced by the pressure generator sander system 500 by being connected to and be located outside of the piping system depicted in FIG. 3 . The novel application of the sander system 500 allows for cleaning small pipes having diameters of approximately ⅜″ up to approximately 6″.
[0193] Table 1 shows a list of preferred dry particulate materials with their hardness ratings and grain shapes that can be used with the sand generator 500 , and Table 2 shows a list of preferred dry particulate particle sieve sizes that can be used with the invention.
[0000]
TABLE 1
PARTICULATES
Material
Hardness Rating
Grain Shape
Diamond
10
Cubical
Aluminium Oxide
9
Cubical
Silica
5
Rounded
Garnet
5
Rounded
Walnut shells
3
Cubical
[0000]
TABLE 2
PARTICULATE SIZE
SIEVE SIZE OPENING
U.S. Mesh
Inches
Microns
Millimeters
4
.187
4760
4.76
8
.0937
2380
2.38
16
.0469
1190
1.19
25
.0280
710
.71
45
.0138
350
.35
[0194] There are many novel parts and benefits to the use of the Pressure Generator Sander System 500 . The portability allows for easy to move and maneuver in tight working environments. The sander 500 is able to accept a wide variety of abrasive media in a wide variety of media size. Variable air pressure controls 570 in the sander 500 allows for management of air pressures up to approximately 125 PSI. A mixing Valve 545 adjustment allows for setting, controlling and dispensing a wide variety of abrasive media in limited and controlled quantities, allowing the operator precise control over the amount of abrasive medium that can be introduced into the air stream in a single or multiple application. The filler lid 540 , incorporated as part of the cabinet and the pressure pot allows the operator to load with ease, controlled amounts of the abrasive medium into the pressure pot 535 . The pulse button 580 can be utilized to deliver a single sized quantity of the abrasive material into the air stream or can be operated to deliver a constant stream of abrasive material in to the air stream. All operator controls and hose connections can be centralized for ease of operator use.
[0195] FIG. 6A shows a side view of the novel Abrasive Reclaim Separator Module (Pre-Filter) 600 used in the barrier coating control system of FIG. 3 . FIG. 6B shows an end view of the novel Abrasive Reclaim Separator Module (Pre-Filter) 600 used in the barrier coating control system of FIG. 3 .
600 Abrasive Reclaim Separator Module (Pre-filter)
[0196] Referring to FIGS. 3 , 6 A and 6 B, an off-the-shelf pre-filter that can be used with the invention can be one Manufactured By:Media Blast & Abrasives, Inc. 591 W. Apollo Street Brea, Calif. 92821
Description of Pre-Filter 600 Components:
[0000]
12 & 14 Gauge Steel Construction
Approximate Dimensions: 23″w×22″1×36″h
Ford Grabber Blue Powder-coating
Dust Drawer with Removable Pan 610
2-2″ NPT Inlets 620
Approximate Dimensions: 13¼″w×13¼″l×17″h Cyclone Chamber/Separator 630
8″ Air and Dust Outlet with Flexible Duct to Air Filter 640
Two Inflatable Tires 650
Push/Pull Handle 660
[0206] During the pipe profiling stage, the Pre-Filter 600 allows the filtering of air and debris from the piping system for more than two systems at a time through the 2—approximately 2″ NPT inlets 620 . The cyclone chamber/separator 630 captures the abrasive material and large debris from the piping system, the by products of the pipe profiling process. The fine dust particles and air escape through the approximately 8″ air and dust outlet 640 at the top of the machine and are carried to the dust collection equipment 700 , which filters, from the exhausting air, fine particulates, that may not have been captured with the Pre-Filter 600 .
[0207] There are many novel parts and benefits to the Pre-Filter 600 . The pre-filter has portability and is easy to move and maneuver in tight working environments. The Dust Drawer with Removable Pan 610 allows for easy clean out of the abrasive media and debris from the pipe. The Cyclone Chamber/Separator 630 slows and traps the abrasive media and debris from the piping system and air stream, and prevents excess debris from entering into the filtration equipment. The 2—approximately 2″ NPT Inlet 620 allows a full range of air filtration from two separate riser or piping systems. Use of the approximately 8″ or greater flex tube 640 as an expansion chamber results in reducing the air pressure of the air as it leaves the pre-filter 600 and reduces the potential for back pressure of the air as it departs the pre-filter and enhances the operational performance of the air filter. When used in conjunction with the air filter 700 , the Pre-filter 600 provides a novel way of separating large debris from entering the final stage of the filtration process. By filtering out the large debris with the pre-filter 600 this promotes a great efficiency of filtration of fine particles in the final stages of filtration in the air filter 700 . The approximately 8″ air and dust outlet 640 to the air filter 700 from the pre-filter 600 permits the compressed air to expand, slowing it in velocity before it enters the air filter 700 , which enhances the operation of the air filter 700 . Process cost savings are gained by the use of the pre-filter 600 by reducing the impact of filtering out the large amounts of debris at the pre-filter stage prior to air entering the air filter 700 . This provides for greater operating efficiencies at the air filter 700 a reduction in energy usage and longer life and use of the actual fine air filters 760 used in the air filter 700 .
700 Dust Collection Filter
[0208] Referring to FIGS. 3 , 7 A and 7 B, an off-the-shelf example if a filter 700 used with the invention can be one Manufactured By:Media Blast & Abrasives, Inc. 591 W. Apollo Street, Brea, Calif. 92821.
Description of Air Filter 700 Components:
[0000]
12 & 14 Gauge Steel Construction
Approximate Dimensions: 24″w×32″l×65″h
Ford Grabber Blue Powder-coating
Dust Drawer with Removable Pan and Tightening Knobs 705
1-¾ NPT Inlet 710
2.0 HP Baldor Motor, Volts 115/230 715
8″ Air and Dust Inlet with Flexible Duct to Pre-Filter 720
Ball Vibrator Muffler 725
2—Locking Wheels 730
2—Swivel and Locking Wheels 735
Pushbutton Switch 740
Mushroom Head Switch 745
Selector Switch 750
Tightening Knob 755
2—Corrugated Cartridge Filters, approximately 99.98% Efficient, Collecting 0.5 Micron Particles (based on SAE-J726 test) 760
Cartridge Mounting Rods 765
Cartridge Mounting Plates 770
Filter Tightening Knobs 775
Filter Ball Tightening Knobs 780
Sliding Air Control Exit Vent 785
[0229] During the pipe profiling stage, the filter or dust collector 700 is the final stage of the air filtration process. The dust collector 700 filters the passing air of fine dust and debris from the piping system after the contaminated air first passes through the pre-filter 600 (abrasive reclaim separator module). During the epoxy coating drying stage the filter 700 is used to draw air through the piping system, keeping a flow of air running over the epoxy and enhancing its drying characteristics. The filter 700 creates a vacuum in the piping system which is used as method of checking for airflow in the piping system, part of the ACE DuraFlo process. The dust collector 700 can be capable of filtering air in volumes up to approximately 1100 CFM.
[0230] There are many novel parts and benefits to the Air Filter 700 . The air filter has portability and is easy to move and maneuver in tight working environments. The Dust Drawer with Removable Pan 705 allows for easy clean out of the abrasive media and debris from the filtration chamber. The 8″ flexible duct 640 (from FIG. 6A permits the compressed air to expand and slow in velocity prior to entering the dust collector 700 , enhancing efficiency. The sliding air control exit vent 785 permits use of a lower amperage motor on start up. The reduced electrical draw enables the dust collector 700 to be used on common household electrical currents while still being able to maintain its capacity to filter up to approximately 1100 CFM of air. The air filter 700 keeps a flow of air running over the epoxy and enhancing its drying and curing characteristics. The dust collector 700 creates a vacuum in the piping system, which is used as method of checking for airflow in the piping system.
800 Portable Epoxy Metering and Dispensing Unit
[0231] Referring to FIGS. 3 , 8 A, 8 B and 8 C, a metering and dispensing unit 800 used with the invention can be one Manufactured by:Lily Corporation, 240 South Broadway, Aurora, Ill. 60505-4205.
Description of Metering and Dispensing Unit 800 Components:
[0000]
Aluminum Frame And Cabinet Construction
Approximate Dimensions: 48″L×48″H×22″W
Blue and Black Anodized Finishes
Electrical Powered Space Heating Element and Thermostat 805
Temperature Gauge 810
1-3 Gallon Stainless Steel Pressure Pot for Resin Part A 815
1-3 Gallon Stainless Steel Pressure Pot for Catalyst Part B 820
Pressure Valve For Each Tank 825
Side Door Access Panel 830
Parts and Tool Drawer 835
Aluminum Removable Cover To Access Pressure Pots 840
Adjustable Cycle or Shot Counter 845
4 Wheels—Swivel and Locking 850
Coalescing Air Filter 855
Air Pressure Regulator and Gauge 860
Foot Dispenser Activator 865
Abort Switch 870
On/Off Control Switch 875
Compressed Air Driven Epoxy Meter and Pump Adjustable for Dispensing Up To 14.76 Oz of Mixed Epoxy Per Single Application. Multiple Applications Can Dispense Up To 75 Gallons of Epoxy Per Hour. 880
Threaded Epoxy Mixing Head To Accommodate Disposable Epoxy Mixing Tubes 887 , 885
Push/Pull Handle 890
Epoxy Carrying Tube Hanger 895
[0254] The Portable Epoxy Metering and Dispensing Unit 800 can store up to approximately 3 US gallons of each of A and B component of the two mix component epoxy, and can dispense single shots up to approximately 14.76 oz, in capacities up to approximately 75 US gallons per hour.
[0255] The unit 800 can be very mobile and can be used both indoors and outdoors, and it can operate using a 15 Amp 110 AC electrical service i.e.: regular household current and approximately 9 cubic feet (CFM) at 90 to 130 pounds per square inch. The unit 800 requires only a single operator.
[0256] The epoxy used with the unit 800 can be heated using this unit to its recommended temperature for application. The epoxy can be metered to control the amount of epoxy being dispensed.
[0257] There are many novel parts and benefits to the Epoxy Metering and Dispensing Unit 800 , which include portability and is easy to move and maneuver in tight working environments. The heated and insulted cabinet, all epoxy transit hoses, valves and pumps can be heated within the cabinet. The Top filling pressurized tanks 815 and 820 offers ease and access for refilling. Epoxy can be metered and dispensed accurately in single shot or multiple shots having the dispensing capacity up to approximately 14.76 ounces of material per shot, up to approximately 75 gallons per hour. The position of mixing head 885 , permits a single operator to fill the portable epoxy carrying tubes 887 in a single fast application. The drip tray permits any epoxy overspill at the time of filling to be contained in the drip tray, containing the spill and reducing cleanup. The epoxy carrying tube hanger 895 allows the operator to fill and temporarily store filled epoxy tubes, ready for easy distribution. The pump 880 and heater 805 combination allows for the epoxy to metered “on ratio” under a variety of conditions such as changes in the viscosity of the epoxy components which can differ due to temperature changes which effect the flow rates of the epoxy which can differ giving the operator an additional control on placement of the epoxy by changing temperature and flow rates. Unit 800 overall provides greater operator control of the characteristics of the epoxy in the process.
900 Epoxy Barrier Coating
[0258] Referring to FIGS. 3 and 8A , 8 B and 8 C, a preferred epoxy barrier coating that can be used with the invention can be one Manufactured by: CJH, Inc. 2211 Navy Drive, Stockton, Calif. 95206. The barrier coating product used in this process can be a 2-part thermo set resin with a base resin and a base-curing agent.
[0259] The preferred thermo set resin is mixed as a two-part epoxy that is used in the invention. When mixed and applied, it forms a durable barrier coating on pipe interior surfaces and other substrates. The barrier coating provides a barrier coating that protects those coated surfaces from the effects caused by the corrosive activities associated with the chemistry of water and other reactive materials on the metal and other substrates.
[0260] The epoxy barrier coating can be applied to create a protective barrier coating to pipes ranging in size approximately ⅜″ to approximately 6″ and greater. The barrier coating can be applied around bends intersections, elbows, t's, to pipes having different diameters and make up. The barrier coating can be applied to pipes in any position e.g.: vertical or horizontal, and can be applied as a protective coating to metal pipes used in fire sprinkler systems and natural gas systems. Up to approximately 4 mils thick coating layers can be formed on the interior walls of the pipes. The barrier coating protects the existing interior walls and can also stop leaks in existing pipes which have small openings and cracks, and the like, of up to approximately ⅜ th ″ in diameters in size.
[0261] Although the process of application described in this invention includes application of thermo set resins other types of thermo set resins can be used.
[0262] For example, other thermo set resins can be applied in the process, and can vary depending upon viscosity, conditions for application including temperature, diameter of pipe, length of pipe, type of material pipe comprised of, application conditions, potable and non potable water carrying pipes, and based on other conditions and parameters of the piping system being cleaned and coated by the invention.
[0263] Other thermo set type resins that can be used include but are not limited to and can be one of many that can be obtained by numerous suppliers such as but not including: Dow Chemical, Huntsmans Advances Material, formerly Ciba Giegy and Resolution Polymers, formerly Shell Chemical.
[0264] Although the novel invention can be applied to all types of metal pipes such as but not limited to copper pipes, steel pipes, galvanized pipes, and cast iron pipes, the invention can be applied to pipes made of other materials such as but not limited to plastics, PVC(polyvinyl chloride), composite materials, polybutidylene, and the like. Additionally, small cracks and holes in plastic type and metal pipes can also be fixed in place by the barrier coating.
[0265] Although the preferred applications for the invention are described with building piping systems, the invention can have other applications such as but not limited to include piping systems for swimming pools, underground pipes, in-slab piping systems, piping under driveways, various liquid transmission lines, tubes contained in heating and cooling units, tubing in radiators, radiant in floor heaters, chillers and heat exchange units, and the like.
[0266] While the invention has been described, disclosed, illustrated and shown in various terms of certain embodiments or modifications which it has presumed in practice, the scope of the invention is not intended to be, nor should it be deemed to be, limited thereby and such other modifications or embodiments as may be suggested by the teachings herein are particularly reserved especially as they fall within the breadth and scope of the claims here appended.
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Methods and process steps for mapping, cleaning and providing barrier coatings to interior walls of piping systems. An entire piping system can be cleaned in one single pass by dry particulates forced by air and the piping system coated in one single pass. Pipes can be protected from water corrosion, erosion and electrolysis. Pipes having diameters of approximately ⅜″ up to approximately 6″ are treatable. Piping systems such as potable water lines, natural gas lines, HVAC, drains, and fire sprinkler systems in homes, apartments, high-rise hotel/resorts, office towers, high-rise apartment and condominiums and schools, can be treated. The coating forms an approximately 4 mils or greater covering inside the pipes. Buildings can return to service within approximately 24 to approximately 96 hours.
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CROSS RELATED APPLICATIONS
This application is a divisional of application Ser. No. 11/746,935 filed May 10, 2007 now U.S. Pat. No. 7,766,269 which is a divisional of application Ser. No. 11/357,027 filed Feb. 21, 2006 now U.S. Pat. No. 7,472,855 and claims the benefit of provisional application Ser. No. 60/743,108, filed Jan. 9, 2006, both of which are incorporated by reference in their entirety.
This invention relates generally to refiners for removing contaminants from fiber materials, such as recycled or recovered paper and packaging materials. In particular, the present invention relates to refiner stator plates and especially to the outer row of teeth on the stator plates.
Refiner plates are used for imparting mechanical work on fibrous material. Refiner plates having teeth (in contrast to plates having bars) are typically used in refiners which serve to deflake, disperge or mix fibrous materials with or without addition of chemicals. The refiner plates disclosed herein are generally applicable to all toothed plates for dispergers specifically and refiners in general.
Disperging is primarily used in de-inking systems to recover used paper and board for reuse as raw material for producing new paper or board. Disperging is used to detach ink from fiber, disperse and reduce ink and dirt particles to a favorable size for downstream removal, and reduce particles to sizes below visible detection. The disperger is also used to break down stickies, coating particles and wax (collectively referred to as “particles”) that are often in the fibrous material fed to refiner. The particles are removed from the fibers by the disperger become entrained in a suspension of fibrous material and liquid flowing through the refiner, and are removed from the suspension as the particles float or are washed out of the suspension. In addition, the disperger may be used to mechanically treat fibers to retain or improve fiber strength and mix bleaching chemicals with fibrous pulp.
There are typically two types of mechanical dispergers used on recycled fibrous material: kneeders and rotating discs. This disclosure focuses on disc-typed disperger plates that have toothed refiner stator plates. Disc-type dispergers are similar to pulp and chip refiners. A refiner disc typically has mounted thereon an annular plate or an array of plate segments arranged as a circular disc. In a disc-type disperger, pulp is fed to the center of the refiner using a feed screw and moves peripherally through the disperging zone, which is a gap between the rotating (rotor) disk and stationary (stator) disk, and the pulp is ejected from the disperging zone at the periphery of the discs.
The general configuration of a disc-type disperger is two circular discs facing each other with one disc (rotor) being rotated at speeds usually up to 1800 ppm, and potentially higher speeds. The other disc is stationary (stator). Alternatively, both discs may rotate in opposite directions.
On the face of each disc is mounted a plate having teeth (also referred to as pyramids) mounted in tangential rows. A plate may be a single annular plate or an annular array of plate segments. Each row of teeth is typically at a common radius from the center of the disc. The rows of rotor and stator teeth interleave when the rotor and stator discs are opposite each other in the refiner or disperger. The rows of rotor and stator teeth intersect a plane in the disperging zone that is between the discs. Channels are formed between the interleaved rows of teeth. The channels define the disperging zone between the discs.
The fibrous pulp flows alternatively between rotor and stator teeth as the pulp moves through successive rows of rotor and stator teeth. The pulp moves from the center inlet of the disc to a peripheral outlet at the outer circumference of the discs. As fibers pass from rotor teeth to stator teeth and vice-versa, the fibers are impacted as the rows of rotor teeth rotate between rows of stator teeth. The clearance between rotor and stator teeth is typically on the order of 1 to 12 mm (millimeters). The fibers are not cut by the impacts of the teeth, but are severely and alternately flexed. The impacts received by the fiber break the ink and toner particles off of the fiber and into smaller particles, and break the stickie particles off of the fibers.
Two types of plates are commonly used in disc-type dispergers: (1) a pyramidal design (also referred to as a tooth design) having an intermeshing toothed pattern, and (2) a refiner bar design. A novel pyramidal tooth design has been developed for a refiner plate and is disclosed herein.
FIGS. 1 a , 1 b and 1 c show an exemplary pyramidal plate segment having a conventional tooth pattern. An enhanced exemplary pyramidal toothed plate segment is shown in commonly-owned U.S. Patent Application Publication No. 2005/0194482, entitled “Grooved Pyramid Disperger Plate.” For pyramidal plates, fiber stock is forced radially through small channels created between the teeth on opposite plates, as shown in FIG. 1 c . Pulp fibers experience high shear, e.g., impacts, in their passage through dispergers caused by intense fiber-to-fiber and fiber-to-plate friction.
With reference to FIGS. 1 a , 1 b and 1 c , the refiner or disperger 10 comprises disperger plates 14 , 15 which are each securable to the face of one of the opposing disperger discs 12 , 13 . The discs 12 , 13 , only portions of which are shown in FIG. 1 c , each have a center axis 19 about which they rotate, radii 32 and substantially circular peripheries.
A plate may or may not be segmented. A segmented plate is an annular array of plate segments typically mounted on a disperger disc. A non-segmented plate is a one-piece annular plate attached to a disperger disc. Plate segment 14 is for the rotor disc 12 and plate segment 15 is for the stator disc 13 . The rotor plate segments 14 are attached to the face of rotor disc 12 in an annular array to form a plate. The segments may be fastened to the disc by any convenient or conventional manner, such as by bolts (not shown) passing through bores 17 . The disperger plate segments 14 , 15 are arranged side-by-side to form plates attached to the face of the each disc 12 , 13 .
Each disperger plate segment 14 , 15 has an inner edge 22 towards the center 19 of its attached disc and an outer edge 24 near the periphery of its disc. Each plate segment 14 , 15 has, on its substrate face concentric rows 26 of pyramids or teeth 28 . The rotation of the rotor disc 12 and its plate segments 14 apply a centrifugal force to the refined material, e.g., fibers, that cause the material to move radially outward from the inner edge to the outer edge 24 of the plates. The refined material predominantly move through the disperging zone channels 30 formed between adjacent teeth 28 of the opposing plate segments 14 , 15 . The refined material flows radially out from the disperging zone into a casing 31 of the refiner 10 .
The concentric rows 26 are each at a common radial distance (see radii 32 ) from the disc center 19 and arranged to intermesh so as to allow the rotor and stator teeth 28 to intersect the plane between the discs. Fiber passing from the center of the stator to the periphery of the discs receive impacts as the rotor teeth 28 pass close to the stator teeth 28 . The channel clearance between the rotor teeth 28 and the stator teeth 28 is on the order of 1 to 12 mm so that the fibers are not cut or pinched, but are severely and alternately flexed as they pass in the channels between the teeth on the rotor disc 12 and the teeth on the stator disc 13 . Flexing the fiber breaks the ink and toner particles on the fibers into smaller particles and breaks off the stickie particles on the fibers.
FIGS. 2 a and 2 b show a top view and a side cross-sectional view, respectively, of a standard tooth geometry 34 used in the outer row of a stator plate. The tooth 34 has a pyramidal design consisting of strait sides 36 that taper to the top 38 of the tooth. The sides of the standard tooth 28 are each substantially parallel to a radial 32 of the plate.
A primary role of the disperger plate is to transfer energy pulses (impacts) to the fibers during their passage through the channels between the discs. The widely accepted toothed plate typically includes the square pyramidal tooth geometry with variations in edge length and tooth placement to achieve desired results.
Refiner material passing between the discs can be accelerated to a high velocity due to the centrifugal forces imparted by the rotor disc. Some of the refiner material exits the discs 12 , 13 at a high velocity and are flung radially against the refiner casing 31 . The high velocity impacts of refiner material against the casing have caused abrasive wear and damaging cavitation to the casing. There is a long felt need for a means to reduce the wear and damage on refiner and disperger casing due and, particularly, to reduce the wear and damage caused by refiner material impacts against the casing.
BRIEF DESCRIPTION
This disclosure proposes a modified stator tooth geometry, such as an angled tooth, for the outermost row of a stator plate. The modified tooth geometry is intended to achieve a longer life of the casing by reducing impacts against the casing due to high velocity particles exiting the plates of the refiner.
A refiner stator plate has been developed having a plurality of concentric rows of teeth wherein an outer row is at or near an outer periphery of the plate segment. The teeth in the outer row include leading sidewalls, wherein the sidewalls are at an angle to radii of the plate segment. plate is preferably a stator plate for a disperger. The angle of the sidewalls of the outer row may be opposite to a direction of rotation of a rotor plate. The angle of the sidewalls is in a range of 10 to 60 degrees with respect to a radial, and preferably in a range of 15 to 45 degrees. The sidewalls may be planar, V-shaped having a straight radial inward surface and a slanted radial outward surface, or curved along their lengths.
Further, the angled sidewall of the teeth of the outer stator row are arranged to project normal (in other words, tangential) to a radial a distance at least equal to a gap between adjacent teeth of the outer stator row. In addition, the angled sidewall may include an angled wall portion and a radially aligned wall portion. Further, the outer row of teeth may have substantially perpendicular rear walls.
A refiner or disperger has been developed comprising a rotor disc including a rotor plate including concentric rows of rotor teeth; a stator disc arranged opposite to the rotor disc in a disperger, wherein the stator disc includes a stator plate, wherein the stator plate includes concentric rows of stator teeth intermeshing with the rotor teeth and an outer row of the stator teeth include sidewalls angled in opposition to the rotation of the rotor disc so as to deflect particles flowing between the teeth of the outer row.
A method of refining pulp material between opposing discs in a refiner has been developed, the method comprising: feeding the pulp material to an inlet of at least one of the discs; rotating one disc with respect to the other disc while pulp material is moved between the discs due to centrifugal force; refining the pulp material by subjecting the material to impacts caused by rows of teeth on the rotating disc intermeshing with rows of teeth on the other disc; deflecting the pulp material as the material flows through an outer row of teeth on the other disc, wherein the outer row of discs comprise teeth having a sidewall angled to deflect pulp material moving radially between the teeth.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1( a ) and 1 ( b ) are a front view and cross-sectional side view, respectively, of a toothed stator plate segment conventionally used in disc-type dispergers.
FIG. 1( c ) is a side cross-sectional view of a stator and rotor disperger plates and discs with channels therebetween.
FIGS. 2 a and 2 b are a top down view and a side perspective view, respectively, of a conventional tooth geometry for the outer teeth row of stator disperger plate.
FIGS. 3 a and 3 b are a top down view and a side perspective view, respectively, of an angled tooth for the outer row of a stator disperger plate, wherein the sidewalls of the tooth are each angled with respect to a radius of the disc.
FIGS. 4 a and 4 b are a front plan view and a side cross-sectional view, respectively, of a disperging stator plate segment utilizing the angled tooth geometry for the outer row of teeth.
FIG. 5 is a top down perspective view of an alternative angled tooth geometry for an outer row of a stator plate.
FIG. 6 is a top down perspective view of another alternative angled tooth geometry for an outer row of a stator plate.
DETAILED DESCRIPTION
A novel arrangement of teeth for a toothed refiner stator plate has been developed in which the outer peripheral row of teeth are angled to deflect refiner material, e.g., pulp, moving through the disperging zone. The deflection reduces the velocity of refiner material particles that would otherwise move along a radial line at a high speed from between the refiner discs and into the casing. This novel arrangement of outer row stator teeth may be applied to any type of toothed refiner plate and especially disc-type dispergers.
The outer row of stator teeth are angled to control the feed of the pulp exiting the disperging zone and out from between the discs. In particular, the leading sidewall of the stator teeth in the outer row of teeth are angled to slant the teeth so as to deflect particles moving along a substantially radial line between the outer row of stator teeth. Deflecting refiner material reduces the velocity of the exiting refiner material and minimizes the impact of the refiner material on the walls of the refiner casing.
The angled outer row of stator teeth prevent pulp from following a direct radial path from the last row of stator teeth and into the casing where high velocity pulp can damage the casing wall. The angle of the outer row of stator teeth and the length of the angled portion of these teeth are selected such that the refiner material, e.g. pulp, passing through the disperging zone is deflected by the angled sidewalls of the last row of stator teeth. The outer row teeth are slanted, at least along a portion of the teeth, such that the slanted portion of the teeth project tangentially a distance at least equal to the gap between adjacent teeth. The deflection prevents refiner materials from being flung at high velocity radially from the discs and into the refiner casing.
FIGS. 3 a and 3 b show a top view and a side perspective view, respectively, of an angled stator tooth 40 where the sides of the tooth are angled with respect to a radial 32 of the disc center. The stator tooth 40 is preferably positioned at the outer row of the stator plate. One or both of the sidewalls 42 of the tooth 40 form an angle 44 with respect to a radius 18 of the disc. Further, the sidewalls 42 taper towards the top 46 of the tooth. The base 48 of the tooth is at the substrate of the plate. The front wall 50 of the tooth faces radially inward and the rear wall 52 of the tooth faces radially outward. The front and rear faces may each be aligned substantially tangent to the row and plate. The front wall may slope towards the top of the tooth. The rear wall, preferably, is generally perpendicular to the substrate of the plate.
The slant (angle 44 ) of the outer row of stator teeth deflects refiner material as it passes through the outer row of stator teeth. The deflection is intended to slow the refiner material, pulp and entrained particles, as it leaves the channel between the disc and before the refiner material enters the casing of the disperger or refiner. By reducing the velocity of the refiner material, less damage is done to the casing as a result of refiner material hitting the casing.
FIGS. 4 a and 4 b are a font view and a side-cross-sectional view, respectively, of an exemplary stator plate 54 that is mounted on a disperger disc. The stator plate is opposite a rotor plate and a disperging zone is formed by the channels between the two opposing plates. The rotational direction (arrow 55 ) for the rotor plate is counter-clockwise (which appears clockwise from the view point of FIG. 4 a which shows a stator plate segment).
The stator disperger plate segment 54 includes rows 56 , 58 , 60 , 62 , 64 and 66 of teeth 68 . The inner teeth rows ( 56 , 58 , 60 , 62 and 64 ) may have a pyramidal shape such as shown in FIGS. 2 a and 2 b . The sidewalls of the inner rows of teeth may be aligned with a radius of the disc, or may be slanted with respect to the radius. Similarly, the rotor plate (not shown) may have rows of teeth that interleave with the row of stator teeth, when the plates are arranged in the refiner.
The outer row 66 of stator teeth 40 have sidewall angles that are angled either in the same direction as or opposite to the rotation 55 of the rotor. It should make no difference to casing protection whether the last row of stator teeth are slanted towards or against the rotational direction. Slanting the outer row of stator teeth in a direction opposite to direction places the teeth in a “holdback” position, and slanting the teeth in the same direction of rotation is a “feeding position.”Further, the sidewall angle of the teeth 40 may be between 10° to 60°, and preferably in a range of 15° to 45°, with respect to a radial of the plate and disc. The angle ( 44 in FIG. 3 a ) of the sidewalls of the last row 66 of stator teeth 40 is selected to deflect refiner material moving through the row and to allow the flow without too much obstruction.
The rear wall ( 52 in FIG. 3 b ) extends to the outer periphery 24 of the stator plate. The sidewall of the teeth 40 are extended as a result of the rear wall being substantially normal to the substrate 72 of the stator plate 54 . Extending the sidewalls provides additional sidewall area to deflect the refiner material. The length and angle of the sidewall should be sufficient such that a fast moving particle cannot move along a radial through the gap between the teeth without hitting the sidewall of a tooth. Accordingly, the projection of the width of the sidewall along a tangential direction should be at least as wide as the gap between the teeth of the last stator row.
The sidewalls on both sides of the outer row stator teeth 40 preferably form the same angles with respect to radii. The leading sidewall (facing the rotational direction of the rotor) deflects pulp. The trailing sidewall is on the opposite side of the tooth and faces a leading sidewall of an adjacent stator tooth. Maintaining the same angles on both sides of the teeth ensures that the gap between teeth remains constant along the length of the teeth. Accordingly, the leading and trailing sidewalls of the stator tooth are preferably symmetrical.
FIG. 5 shows a top down perspective view of an alternative tooth 70 for the last row of the stator plate. The alternative tooth has a double angled sidewall 72 that includes a radial sidewall section 78 and an angled wall section 80 . The radial sidewall section 78 is substantially aligned with a radial of the stator plate. The angled wall section 80 is offset from a radial by an angle 10 to 60 degrees and preferably between 15 to 45 degrees. The length and angle of the angled sidewall 80 are arranged to deflect all refined material moving along a radial and between teeth in the last row of stator teeth. In particular, the tangential projection 81 of the length of the sidewall 80 spans the width of the gap between adjacent teeth in the last stator row.
FIG. 6 shows a top down perspective view of another alternative tooth 84 for the last row of the stator plate. The alternative tooth has a curved sidewall 86 that starts as a substantially radial sidewall section 88 and progressively turns to an angled wall section 90 . The inward radial sidewall section 88 is substantially aligned with a radial of the stator plate. The length and curvature of sidewall 86 are arranged to deflect all refined material moving along a radial and between teeth in the last row of stator teeth. In particular, the tangential projection of the length of the sidewall 86 should span the width of the gap between adjacent teeth in the last stator row.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
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A method of refining celluosic fiber material between opposing discs in a refiner including: feeding the fiber material to between the discs; rotating at least one of the discs to propel the fiber material radially outward and between the discs; refining the refining material by passing the material through rows of intermeshing teeth on the opposing discs; and deflecting the refining material as the material flows through an outer row of teeth on one of discs, wherein the teeth in the outer row have a leading sidewall angled to deflect pulp material moving radially between the teeth.
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BACKGROUND OF THE INVENTION
[0001] The present application relates to ornamental wheel covers, in particular to wheel cover assemblies that are suitable for affixing to vehicles such as heavy trucks, or rigs, and the like.
[0002] The motor vehicular transport industry today is a vibrant part of the economy, and many large transport trucks and rigs are privately owned. Indeed, many a large rig is the effective home of its private owner, providing onboard computers, communication systems, televised entertainment, and sleeping quarters. Ornamentation of the exterior has become an important aspect of personal ownership. Accordingly, the fitting of ornamental wheel covers over the wheels of large rigs and trucks has become widespread in recent years.
[0003] Unfortunately, the devices and methods used to attach ornamental cover assemblies over the wheels of large vehicles suffer from various shortcomings. Commonly, some devices for attaching ornamental covers over wheels have relied upon outwardly extending threaded lugs which are typically provided on the axle for attaching the wheel to the hub. Although this method uses structure present on the vehicle which is clearly intended for affixation of structure (such as a wheel), the method has the disadvantage of making the integrity of the wheel attachment structure dependent upon the viability of a foreign structure that was not part of the vehicle manufacturer's original wheel attachment design. The addition of foreign structure to the original wheel attachment assembly may lead to shortcomings, and indeed, may lead to denial of insurance coverage where the shortcomings are attributable to structure foreign to the original vehicle design. Additional problems may arise should the vehicle be subject to inspection by local, state, or federal authorities. Some inspectors may require that ornamental wheel covers be removed to present a clear view of the wheel attachment system. Removal of the covers may require the vehicle to be jacked up, on a wheel by wheel basis, to take the load off each wheel while the covers are being removed, causing considerable inconvenience.
[0004] One method for attaching wheel covers over wheels that has been used to avoid relying on structure dedicated to wheel attachment is to launch a cover attachment assembly from a hub's oil or grease hub cap attachment structure, rather than the wheel attachment structure. One such device that has been developed provides a number of threaded rods, each rod having a stop nut toward each end. A first stop nut is set at a desired position along the length of the rod, allowing the rod to be inserted, at one end, to a desired depth into a threaded hole in the hub that would otherwise receive one of the half dozen or so bolts for holding down a hub cap. (Three such threaded rods might be provided in triangulated formation, displacing three of the regular hub cap hold-down bolts.) At the other end of each rod, a second stop nut may be adjusted to permit an ornamental wheel cover to be set to the correct orientation in relation to the wheel. In this way, any loading applied to the ornamental wheel cover is transmitted via the rods back to the grease hub, and the wheel attachment structure is left unaffected by any impact or load upon the ornamental wheel cover.
[0005] However, a shortcoming in the foregoing structure is that it is flimsy, in that an impact on the ornamental wheel cover may permanently bend or buckle the rods out of original alignment, leaving the wheel cover in a disfigured spatial relationship to the wheel, defeating the purpose of the ornamentation.
[0006] Another shortcoming found in the prior art relates to the bolts or studs used to affix the wheel cover over the wheel. Typically, an ornamental wheel cover sized to fit a large truck, and configured to survive the kind of occasional impact load that can be expected in this context, may be made of cast aluminum, and may weigh about 15 to 30 pounds. It has been found that a wheel cover having such a large weight may suffer from inadequate torsional and shear attachment to the wheel hub where insufficient attachment means are provided. Where a single central stud is provided for attachment, the rotational momentum of a heavy wheel cover may cause the cover to incline to rotate independently when the vehicle is brought to a sudden stop, because the wheel cover does not have its own braking system and may not be connected over the wheel other than at a central stud. Added to the problem of rotational momentum may be the problem of shear, which may be additionally incurred when the cover is impacted by collision with a curb, bollard or the like.
[0007] Accordingly, there is a need for an improved structure and method of affixing ornamental wheel covers over wheels of vehicles such as trucks. The present invention addresses these and other needs.
SUMMARY OF THE INVENTION
[0008] According to a preferred embodiment of the invention, there is described a wheel covering system that provides a sturdy and robust system for attaching an ornamental wheel cover over a wheel of a large vehicle such as a truck or rig, coverable of withstanding the kind of impact load that a wheel cover might experience over its lifetime, yet being easy to attach, and avoiding connection with the wheel attachment system of the axle hub.
[0009] In a preferred embodiment, the wheel covering system is configured for attachment to a vehicle hub in which the hub has a plurality of threaded lugs for attaching a wheel, and on which a hub cap is attached to the hub by a plurality of threaded bolts. The system includes an ornamental cover having a center point and is configured to be positioned adjacent the wheel, the cover having two holes, each hole offset an equal distance from the center point. A mounting member is provided for connecting the cover over the wheel. The mounting member is configured to be removably attached to two diametrically opposite sides of the hub cap without being in contact with the threaded lugs. The mounting member has a distal end and a proximal end, in which the distal end defines a plurality of holes configured to receive at least some of the threaded bolts that hold down the hub cap. (The terms “distal” and “proximal” as referred to herein are from the perspective of one installing the covering system, thus meaning inward and outward of the vehicle respectively.) These holes are for permitting both the mounting member and the hub cap to be attached to the hub, the mounting member spanning across the outside of the hub cap. The proximal end of the mounting member includes two outwardly extending threaded studs for insertion into the two holes of the ornamental cover, to permit removable attachment of the cover to the mounting member. Thus, the invention avoids any connection to the threaded lugs which are used for attaching the wheel to the hub.
[0010] In a further aspect, the wheel covering system includes a feature in which the ornamental cover has a third hole at the center point, and the proximal end of the mounting member includes a spindle positioned to be inserted through the third hole. Preferably, the spindle may be longer than the flanking studs. Thus, the spindle advantageously facilitates attachment of the cover over the wheel because, when the mounting member has been attached to the hub, it permits the operator to slip the cover over the spindle first, then, by rotating the cover somewhat, to match the two offset holes in the cover with the studs and push the cover over the spindle and studs. The central hole may have a conical portion to facilitate this action. The studs and spindle provide a high degree of redundancy to secure the connection and provide a factor of safety against rotational and shear forces that may be exerted during braking or in a collision.
[0011] In other aspects of the covering system, the ornamental cover has a recess for housing the studs. A bolt-on cap closes off the recess, providing a smooth outer surface to the cover when completely mounted. Preferably, the recess has a floor that is flat, and the proximal end of the mounting member is flat. Thus, the floor of the recess is configured to be compressed against the proximal end of the mounting member by nuts screwed onto the threaded studs, and this provides a secure and wobble free attachment of the cover to the mounting member.
[0012] In one embodiment of the invention, principally for steering and trailing axles, the mounting member includes a cylindrical portion, an external flange attached to the distal end of the mounting member, and a circular plate attached to the proximal end of the mounting member. Preferably, the cylindrical portion is between 3 and 4 mm thick, to provide a sufficiently light but robust mounting member for connecting the cover to hub. A plurality of holes are formed in the flange to receive the hub cap bolts, whereby both the mounting member and the hub cap may be attached to the hub, the mounting member covering the hub cap. The threaded studs are attached to the circular plate at the proximal end of the mounting member. Preferably, the mounting member includes a slot configured to receive a valve of the hub cap. In this way, the oil or grease level may be maintained without removing the mounting member from the hub. Additionally, the mounting member may include an orifice positioned to allow inspection, through the mounting member, of the oil or grease level in the hub cap. Thus, the oil or grease level may be checked without removing the mounting member from the hub.
[0013] In a second embodiment, principally for drive axles, the mounting member is configured to provide attachment of an ornamental cover to a hub having an axle mounting cap. The mounting member of this embodiment also does not contact threaded lugs on the hub that are intended for attaching a wheel to the axle. However, here, the mounting member is formed from an initially flat plate having two ends. The plate is bent to a configuration adapted to span across the axle mounting cap and to be fixed to the axle mounting cap at the two ends. In this embodiment, the thickness of the plate is preferably between 4 mm and 5 mm to provide desirable stiffness and strength. This configuration also overcomes shortcomings in the prior art, and provides a sufficiently robust configuration for a wheel covering system that can be expected to experience impact loads during its lifetime.
[0014] These and other advantages of the invention will become more apparent from the following detailed description thereof and the accompanying exemplary drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a perspective view of a typical wheel attached to an hub of a truck.
[0016] FIG. 2 is a vertical sectional view of a mounting member used in the present invention.
[0017] FIG. 3 is a plan view of the mounting member of FIG. 2 .
[0018] FIG. 4 is the wheel of FIG. 1 , including the mounting member of FIGS. 2 and 3 .
[0019] FIG. 5 is a vertical sectional view of the wheel in FIG. 4 , including a wheel covering system having features of the present invention.
[0020] FIG. 5A is an expanded view of the central portion of FIG. 5 .
[0021] FIG. 6 is a perspective view of a typical drive wheel attached to a different kind of hub of a truck.
[0022] FIG. 7 is a vertical sectional view of an embodiment of a mounting member suitable for use with the wheel and hub of FIG. 6 .
[0023] FIG. 8 is a plan view of the mounting member of FIG. 7 .
[0024] FIG. 9 is the wheel of FIG. 6 , including the mounting member of FIGS. 7 and 8 .
[0025] FIG. 10 is a vertical sectional view of the wheel in FIG. 9 , including a wheel covering system attached.
[0026] FIG. 10A is an expanded view of the central portion of FIG. 10 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0027] With reference to the drawings which are by way of example and not limitation, a wheel cover assembly and attachment system is disclosed having features of the wheel covering system of the present invention. In setting forth the features of the present invention, there will first be described a cover assembly of a preferred embodiment that is structured for incorporation with the wheel covering system of the present invention. Second, there will be described one kind of heavy truck hub structure that a wheel cover assembly will commonly encounter for attachment. Third, there will be described one preferred embodiment of an attachment system structured for incorporation with the wheel covering assembly of the present invention in the context of the described truck hub. Fourth, there will be described a further type of heavy truck hub structure that a wheel cover assembly may commonly encounter for attachment. Fifth, there will be described variations to the embodiments of the wheel cover assembly and attachment systems earlier described.
[0028] Turning now to a first embodiment of a wheel cover assembly of the present invention, as best seen in FIG. 5 , an ornamental outer cover adapted for attachment according to the present invention is generally indicated by the numeral 20 . Where the cover 20 is intended for attachment to a large vehicle such as a truck or rig, it is beneficially made of cast aluminum, and may weigh as much as about 15 to 30 pounds. This substantial weight gives the cover 20 considerable durability, able to withstand the occasional impact that is inevitable over the lifetime of a cover.
[0029] In a preferred embodiment, the cover 20 has openings (not shown in the figures) that give the cover a visible depth to one viewing the cover attached to a wheel. To enhance this visible depth, a second cover element is provided, being a foil sheet 24 specially made to have enhanced reflective properties on one side, preferably out of aluminum or stainless steel and in the range of 0.5 to 1 mm thick. The foil sheet 24 is placed distal to the outer cover 20 with the reflective side facing the exterior. In this way, one viewing the cover 20 looks through the openings in the cover 20 onto the reflective foil sheet 24 with the effect that the foil obstructs the view onto the unattractive structural details of the wheel attachment system, and reflects light to give an overall attractive ornamental appearance. The combination of cover 20 and foil 24 is referred to as a cover assembly, in this and in further embodiments.
[0030] In a preferred embodiment, an outer circumferential rim of the inner foil 24 may be configured to contact the ornamental cover 20 along an outer circumferential line 26 ( FIG. 5 ), and also along an inner circumferential line 28 (seen in FIG. 5A ). Matching holes may be drilled into the foil 24 and cover 20 along both the inner and outer lines of contact 26 , 28 at points spaced apart, so that tapping screws 29 may be inserted through the foil 24 and screwed into the cover 20 , to fixedly attach the foil 24 to the cover 20 along two circumferential lines. This attachment of foil to cover has the advantage of making the wheel assembly easy to manipulate as a single object, facilitating installation, removal, storage, and transport.
[0031] Prior to turning to the structure for connecting the cover assembly to the vehicle wheel, there will be described with reference to FIGS. 1 , 4 , and 5 certain features commonly found on large trucks that may provide the foundation for a device and method of connection of the present wheel covering system. Typically, the front axle 40 of a truck is the steering axle, and its terminal end commonly includes a number of features. An outer cylinder 44 acts as a hub and includes a number of lug bolts 46 ( FIGS. 1 , 4 , and 5 ) protruding outwardly to be inserted through receiving holes 48 in the wheel 50 and to be covered by hex-head nuts 52 that will be tightened to a specified torque for proper operation and safety of the wheel in motion.
[0032] For the steering axle, there are commonly found three types of axle caps, (1) oil, (2) grease, and (3) non-serviceable. One of such axle caps 54 (also referred to as hub caps) of a kind typically found on a steering axle is commonly attached to the proximal end of the outer cylinder 44 . The outer cylinder and hub cap rotate with the axle 40 . This oil or grease hub cap will typically have a transparent window 56 ( FIG. 1 ) to enable a vehicle operator to inspect the oil or grease level, and an oil valve 57 for introducing oil into the oil hub cap. The axle cap 54 is fixed to the axle 40 by a plurality of hub cap bolts 58 inserted through an external flange 60 on the hub cap, and into threaded hub cap holes 62 in the axle.
[0033] Turning now to a mounting member and mechanism configured to match and attach the cover assembly in the present invention, it has been determined that affixing the mounting member directly from the exterior of the axle cap 54 rather than from the lugs 46 of the outer cylinder 44 may be effectively achieved, as will be described, to produce a robust and effective connection coverable of safely holding a heavy cover assembly of about 40 pounds under acceleration, deceleration, and impact loads, and that overcome shortcomings in the art.
[0034] In a preferred embodiment, and as best seen in FIGS. 2 and 3 , a mounting member 70 or connector is provided for operation as a structural connection between the hub 44 and the cover assembly 20 , 24 for operation of the wheel covering assembly of the present invention. The mounting member 70 includes a cylindrical portion 72 that, in a preferred embodiment, is fabricated to include a spun or cast steel cylinder which, in a preferred embodiment is 3-4 mm thick. A capping portion 74 takes the form of a flat steel disc that may be welded to the proximal edge of the cylindrical portion 72 . An external flange 76 is made as a flat steel annulus that may be welded to the distal edge of the cylindrical portion 72 . Holes 78 are drilled into the flange 76 to correspond with the locations of the bolts 58 holding the hub cap 54 to the axle 40 . When the mounting member 70 is attached to a steering hub according the present invention, the bolts 58 are removed from the hub cap 54 , the mounting member 70 is positioned to straddle the hub cap 54 , and the bolts 58 are replaced to attach both the hub cap 54 and the mounting member 70 to the hub 44 , as exemplified in FIG. 5 , thus capturing the mounting member 70 on top of the hub cap 54 . (If required, a new set of bolts slightly longer than those removed from the hub cap may be used.) A slot 77 may be machined in the mounting member 70 to penetrate both the flange 76 and the cylindrical portion 72 , as best seen in FIGS. 2 and 3 , the slot being sized to receive the oil hub cap valve 57 which, when the mounting member is attached, may protrude outwardly from under the mounting member 70 so as to remain available to receive oil for refilling the oil cap.
[0035] On the covering portion 74 of the mounting member, two threaded lugs 80 are fixed to receive corresponding holes 100 (best seen in FIG. 5A ) in the cover 20 . The two threaded lugs 80 are preferably spaced equidistant from the center of the covering portion 74 , diametrically opposite one another. Moreover, on the center of the covering portion 74 a threadless guide spindle 82 may be fixed, preferably having a length that is about half an inch longer than the flanking threaded lugs 80 and having a diameter that is about the same as the lugs, preferably 10-14 mm. The cover 20 has three mating holes 100 to receive the spindle first, and then the flanking lugs. Covering nuts 86 are screwed down onto the lugs 80 to secure the cover assembly onto the mounting member 70 . Preferably, the covering nuts 86 are configured to have a unique circumferential profile so that the manufacturer may provide a mating socket for use by a vehicle owner. Such unique profile and mating socket, in effect, provides a key to the owner, making it extremely difficult for miscreants to remove the cover assembly without permission. A closing cap 88 may be inserted into a recess 90 in the cover 20 to protect and conceal the spindle, lugs, the covering nuts, and related assembly. The closing cap 88 may be held in the recess 90 by two bolts 89 configured to pass through the cover 20 and mate with two threaded holes 91 ( FIG. 2 ) in the covering portion 74 for securing the closing cap 88 flush with the external surface of the cover 20 . In a preferred embodiment, the floor 91 of the recess 90 is flat, thus allowing a stable and wobble free connection to be formed between the cover 20 and the mounting member 70 when the covering nuts are tightened to compress the floor against the mounting member.
[0036] Thus, under a preferred embodiment, the mounting member 70 includes two threaded lugs 80 and an additional spindle 82 for attaching the cover assembly to the hub. In light of the considerable weight of the cover assembly, two lugs and corresponding nuts provide a degree of redundancy and safety in case one of the nuts should come loose. Furthermore, by providing two lugs offset from the center, the capacity to withstand the rotational momentum applied by the cover assembly is greatly increased. It will be appreciated that the weight of the cover assembly, perhaps in the vicinity of 40 pounds, is much greater than in the case of a regular passenger automobile, and thus unbalanced angular momentum of the cover assembly caused by sudden braking may be substantial. The provision of a redundant second lug and nut combination, offset from the center of the cover, is advantageous in dealing with such momentum.
[0037] Moreover, in addition to the rotational forces exerted by the cover assembly, an additional force may be exerted as a shear force when the cover 20 is subject to an impact such as may be applied when hitting a curb, bollard, or other object, a not uncommon experience in the lifetime of a wheel cover. The ability of the wheel covering system to withstand these forces is greatly enhanced by the addition of the central spindle 82 , so that three separate protrusions (the two lugs 80 and the spindle 82 ) are provided to withstand shear forces caused by impact.
[0038] An additional advantage provided by the central spindle 82 in combination with two lugs 80 is firstly that the spindle provides a guide pin to facilitate installing the cover assembly. A feature of the cover 20 provided to facilitate installation on the hub is that the central hole 100 on the cover 20 may be configured to terminate, on the inside face, in a conical taper 101 ( FIG. 5A ). Thus, because the spindle 82 is about half an inch longer than the flanking lugs 80 , the installer is able to locate the central spindle 82 in the central hole 100 by sliding the cover past the spindle. When the spindle falls into the cone 101 , the installer knows that he has found the correct hole, and pushes the cover assembly inwards so that its significant weight is taken by the spindle 82 . Then, by rotating the cover assembly somewhat, the installer may easily align the lugs 80 with their corresponding holes 100 , and push the cover assembly onto the lugs 80 before installing and tightening the covering nuts 86 . The longer spindle feature eliminates the difficulty of having to simultaneously manually support the full weight of the cover assembly and find the correct cover alignment with respect to the two lugs 80 before the cover assembly may be pressed over the lugs.
[0039] In a further aspect, the mounting member 70 may include an aperture 83 cut into the proximal end of the mounting member (seen in FIG. 3 ), to enable the vehicle operator to view the oil or grease level in the hub via the window 56 in the oil or grease hub cap 54 . The aperture 83 must be at the topmost point of its rotational travel for the vehicle operator to correctly assess the adequacy of the grease level. Thus, if the aperture is not at the topmost point of its travel when the vehicle is at rest, it may be necessary to roll the vehicle forward somewhat to bring the aperture 83 up to the topmost point of its travel before an inspection can be conducted.
[0040] It will be appreciated that the structure described has the further advantage of allowing a vehicle operator to remove a wheel by removing only the cover assembly. The mounting attachment 70 may remain in place on the hub while the wheel is removed, thereby avoiding the inconvenience of having to remove structure in addition to the wheel when changing or repairing a wheel.
[0041] Turning now to another embodiment of the present invention there is now described with reference to FIGS. 6-10 a wheel covering system having alternative features of the present invention. It is a common aspect of large trucks or rigs that they may have three (or more) sets of axles. The front axle is generally the steering axle, commonly having features such as those described above. Behind the front axle is a typically a drive axle, followed by a trailing axle. One variation between a steering axle and a drive axle is that a drive axle may have two wheels on each side, in which the geometry of the outer driving wheel differs from the geometry of the single steering wheel. Whereas a steering wheel is commonly configured to present a radially inner disc portion 51 generally flush with the outside profile of the wheel 50 , as exemplified in FIGS. 1 , 4 , 5 , an outer driving wheel is commonly configured to present a radially inner disc portion 51 ′ generally flush with the inside profile of the wheel 50 ′ as exemplified in FIGS. 6 , 9 , 10 . Additionally, the outer drive axle commonly does not have a large oil or grease inspection cover (as a steering wheel may have), but rather may have a flat or bulbous plate sealing the hub, as exemplified in FIG. 6 . In light of these variations of the geometry of the various hub to wheel configurations typical in a large vehicle, a further embodiment of the present invention is described.
[0042] Turning to FIGS. 6-10 , there is described an alternative attachment system for attaching an ornamental wheel cover to a drive axle of a large truck. Where numerals are shown to be “primed,” they refer to the same element as in the former embodiment, with any modifications made to suit the present embodiment. As in the case of the embodiment of the steering wheel covering system exemplified in FIGS. 1-5 , the drive wheel covering system of the present embodiment includes an ornamental cover 20 ′ which may similarly have openings (not shown in the figures), a foil 24 ′ shaped to fill in a larger void in the wheel distal to the cover 20 ′ and having a reflective surface facing the exterior of the cover to create visible depth in the cover. As in the former embodiment, the foil may be screwed onto the cover by screws 29 ′ tapping into the cover 20 ′ along two circumferential lines 26 ′, 28 ′ (outer and inner), thus forming a single cover assembly that can be readily manipulated into place over the wheel, stored, and transported.
[0043] The mounting member 70 ′ in this second embodiment is exemplified best in FIGS. 7-8 . The mounting member is not formed from a cylinder as in the previous embodiment, but in this case may be fabricated from a flat metal plate which is then bent to a shape suitable for spanning over a bulbous axle cap 54 ′ covering the driving wheel hub 44 ′, as exemplified in FIGS. 7-8 , and 10 . Preferably, as in the previous embodiment, the proximal surface 74 ′ of the mounting member is flat, and vertical, when in use. In a preferred embodiment, the thickness of the flat metal plate is between 5 and 6 mm, to provide suitable stiffness and strength without excessive weight. The extremities of the plate may be shaped to conform to the circular perimeter of the hub 44 ′. Holes 78 ′ are provided in the extremities of the plate and positioned to match locations of the axle cover bolts 58 ′ holding down the bulbous axle cap 54 ′ on the hub. The mounting member 70 ′ of this embodiment similarly includes two threaded lugs 80 ′ positioned at a proximal end, offset from the center of the mounting member, and a threadless spindle 82 ′ at the center, as in the previous embodiment, for installation of the cover assembly of the present embodiment in a similar way. It has been found that the bent plate mounting member 70 ′ embodiment, although not as stiff as the cylindrical mounting member 70 of the previous embodiment, provides an inexpensive yet adequate and robust solution to connecting an ornamental wheel cover over a drive wheel of a truck and overcomes shortcomings in the prior art without adding excessive weight. As in the previous embodiment, the cover assembly includes a closing cap 88 ′, held in position by two threaded bolts 89 ′ configured to pass through the cover 20 ′ and mate with two threaded holes 91 ′ in the mounting member 70 ′. FIG. 10 . Finally, as in the previous embodiment, the floor 93 ′ of the recess is flat, to permit the cover 20 ′ to form a stable and wobble free connection to the mounting member 70 ′ when the covering nuts 86 ′ are tightened.
[0044] Thus, when the wheel covering system of the present embodiment is to be installed, the installer removes the corresponding bolts 58 ′ from the hub 44 ′, places the mounting member 70 ′ over the axle cap 54 ′, and reinserts the bolts 58 ′ in the same threaded holes from which they have been removed, thereby capturing the mounting member 70 ′ on top of the axle cap 54 ′. (If required, longer bolts may replace the original bolts.) The mounting member 70 ′ presents a suitable connection so that the covering system is mounted over the wheel on a part of the vehicle hub that is independent of the wheel attachment system. The mounting member 70 ′ has adequate stiffness and strength to resist the magnitude of loads that will be applied to the wheel cover during its lifetime, and overcomes shortcomings in the prior art. The mounting member and related cover assembly may be easily removed from the hub without having to jack up the wheel, and it is configured to resist unbalanced forces that may be caused by sudden stopping and impact loads.
[0045] Thus, it is seen that the covering system of the present invention provides novel and useful features for covering certain kinds of wheel hubs, and overcoming shortcomings in the prior art. The present invention may, of course, be carried out in other specific ways than those herein set forth without departing from the essential characteristics of the invention. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, and all changes coming within the meaning and equivalency range of the appended claims are intended to be embraced therein.
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A wheel covering system is disclosed having a first external cover element and a second internal cover element screwed to the first element. The wheel covering system is connected to an hub of a large vehicle such as a truck without relying on lugs provided on the hub for connecting the wheel to the hub. The connection is achieved by relying on bolts used to attach a hub cap (or axle cover) to the axle, without eliminating the hub cap (or axle cover), and at the same time providing a sturdy and robust connection capable of withstanding forces expected to be applied to a wheel cover during its lifetime.
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RELATED APPLICATION
[0001] This application is a divisional of application Ser. No. 11/960,145 filed Dec. 19, 2007, which is a continuation of application Ser. No. 10/642,638 (now U.S. Pat. No. 7,311,689), filed Aug. 19, 2003 (U.S. Pat. No. 7,311,689) which is a divisional of application Ser. No. 09/618,759, filed Jul. 18, 2000 (now U.S. Pat. No. 6,890,315) and claims priority to the Provisional Application Ser. No. 60/206,232, filed May 23, 2000, the entirety of all of these applications are incorporated by reference.
FIELD OF THE INVENTION
[0002] This invention relates to methods and apparatus for treatment of congestive heart failure (CHF). In particular, the invention relates to the removal of excessive fluids, such as water, in patients suffering from CHF.
BACKGROUND OF THE INVENTION
[0003] Congestive Heart Failure (CHF) is the only form of heart disease still increasing in frequency. According to the American Heart Association, CHF is the “Disease of the Next Millennium”. The number of patients with CHF is expected to grow even more significantly as an increasing number of the “Baby Boomers” reach 50 years of age.
[0004] CHF is a condition that occurs when the heart becomes damaged and reduces blood flow to the organs of the body. If blood flow decreases sufficiently, kidney function becomes impaired and results in fluid retention, abnormal hormone secretions and increased constriction of blood vessels. These results increase the workload of the heart and further decrease the heart's pumping ability and, that in turn, causes further reductions in blood flow to the kidney. It is believed that the progressively-decreasing perfusion of the kidney is the principal non-cardiac cause perpetuating the downward spiral of the “Vicious Cycle of CHF”. Moreover, the fluid overload and associated clinical symptoms resulting from these physiologic changes are the predominant cause for excessive hospital admissions, terrible quality of life and overwhelming costs to the health care system due to CHF.
[0005] While many different diseases may initially damage the heart, once present, CHF is split into two types: Chronic CHF and Acute (or Decompensated-Chronic) CHF. Chronic Congestive Heart Failure is a longer term, slowly progressive, degenerative disease. Over years, chronic congestive heart failure leads to cardiac insufficiency. Chronic CHF is clinically categorized by the patient's ability to exercise or perform normal activities of daily living (such as defined by the New York Heart Association Functional Class). Chronic CHF patients are usually managed on an outpatient basis, typically with drugs.
[0006] Chronic CHF patients may experience an abrupt, severe deterioration in heart function, termed Acute Congestive Heart Failure, resulting in the inability of the heart to maintain sufficient blood flow and pressure to keep vital organs of the body alive. These acute CHF deteriorations can occur when extra stress (such as an infection or excessive fluid overload) significantly increases the workload on the heart in a stable chronic CHF patient. In contrast to the stepwise downward progression of chronic CHF, a patient suffering acute CHF may deteriorate from even the earliest stages of CHF to severe hemodynamic collapse. In addition, Acute CHF can occur within hours or days following an Acute Myocardial Infarction (AMI), which is a sudden, irreversible injury to the heart muscle, commonly referred to as a heart attack.
[0007] A. Treatment Strategies for CHF
[0008] 1. The Treatment of Chronic CHF
[0009] There are currently two broad categories for the treatment of Chronic CHF: (1) drug therapy and (2) surgical therapy. All treatments share the common goal of the alleviation of CHF symptoms, the improvement of heart function, and the disruption of the neurohormonal secretions of a kidney to decrease stress and prevent possible failure.
[0010] A cornerstone of the drug therapy of Chronic CHF includes the use of angiotensin converting enzyme (ACE) inhibitors, positive inotropic agents, diuretics, digitalis, and, more recently, beta-blockers with the amount of each drug used dependent on the stage of heart failure.
[0011] Positive Inotropic Agents
[0012] Directly combating the inability of the heart to propel blood forward might seem to be the single most intuitive means for treating heart failure. A class of drugs known as inotropes increases the strength of contraction of the remaining viable heart muscle, allowing the heart to expel more blood with each beat. While all types of inotropes (e.g., dobutamine, dopamine, milrinone) are effective in the short-term, they lack long-term value in the treatment of heart failure because they, like the vasodilators, tend to cause additional neurohormonal activation (as evidenced by hormonal kidney secretions) and perpetuation of the downward spiral.
[0013] Diuretics
[0014] Diuretics decrease the sodium and water retention in a patient by preventing reabsorption of these substances at specific sites in the renal tubules of the kidney. Diuretics, such as Lasix and Bumex, are effective at reducing symptoms of heart failure due to fluid overload, especially in the lungs and extremities. In the long-term, diuretic therapy fails because it further activates the renin-angiotensin system (e.g., the hormones secreted by the kidney) and eventually overwhelms the ability of diuretics to control salt and water retention.
[0015] Vasodilators
[0016] The next logical step in the treatment of heart failure is to limit vasoconstriction and reduce its adverse effect on the heart. Unfortunately, vasodilatory agents, like diuretics, fail after a period of time, as they decrease kidney perfusion pressure and activate the renin-angiotensin system.
[0017] ACE Inhibitors and β-Blocking Drugs
[0018] In the past two decades, the development of angiotensin converting enzyme (ACE) inhibitors and β-blockers has signaled perhaps the most significant development of this century in the pharmacological treatment of heart failure. Both are aimed at the neurohormonal axis of this disease and both act by disruption of the feedback loops that characterize heart failure. β-blockers and ACE inhibitors are the first classes of drugs to be associated with a survival benefit for patients in heart failure. However, despite these significant advances in medical therapy, their effectiveness is limited, especially in the later stages of CHF. Patients become resistive to the increased dose and potency of drugs until further increase becomes too dangerous.
[0019] Surgical Therapies
[0020] There are three potential surgical treatments for patients in heart failure: (1) revascularization, (2) implantation of a heart assist device, and (3) heart transplantation. Revascularization is the restoration of blood flow to the heart itself, either angiographically (PTCA) or surgically (CABG). Revascularization is performed in patients in whom it is believed that a poor blood supply to the heart itself is the major cause of the observed heart dysfunction. A second surgical modality is the placement of an implantable pump that replaces the failed ventricle. This type of device is known as the Left Ventricular Assist Device (LVAD). The third and ultimate surgical modality for patients suffering from heart failure is transplantation. While this can be an effective means to cure heart failure, transplantation is replete with significant medical issues. In addition, for a majority of patients suffering from CHF, transplantation is not available because they fail to meet current criteria for heart transplant recipients, socioeconomic issues and, most commonly, lack of donor organs. Despite their benefit, surgical therapies are used in less than 1% of all heart failure patients due to their cost, invasiveness and a lack of donors' hearts.
[0021] 2. Treatment of Acute CHF
[0022] Pharmacologic Therapies
[0023] In contrast to the treatment of Chronic CHF, the abruptness and severity of the decrease in blood flow and pressure put the vital organs, e.g., the kidneys, at immediate risk of severe damage. Interestingly, the physiologic effects of some therapies used to treat Acute CHF closely parallel those of the “Vicious Cycle” of CHF in that they may transiently or permanently damage some organs to preserve the heart and the brain.
[0024] The first line of therapy for Acute CHF is the use of intravenous (IV) inotropic (“squeeze” enhancing) agents in concert with intensive diuretic therapy. The purpose of this therapy is to substantially increase the output of the heart, increasing kidney blood flow, and thereby increasing urine output. It may take hours to days for this therapy to restore hemodynamic stability and fluid removal. In addition, therapy with IV inotropic agents has side effects. Most inotropic drugs can cause vasodilation and hypotension (low blood pressure) that may lead to Acute Renal Failure. Cardiac arrest from inotropic-induced arrhythmias (irregular heartbeats) also can occur.
[0025] The second-line therapy is the use of vasopressor (vasoconstricting) agents. While they increase blood pressure, in the higher doses used in Acute CHF, these agents cause severe vasocontriction, and can lead to kidney and liver failure. In concert with a large mandatory fluid intake from multiple IV medications, progressively increasing diuretic unresponsiveness and concurrent hemodynamic instability, reduced renal perfusion leads to the refractory (drug resistive) fluid overload state seen in Acute CHF. This excess fluid decreases ventricular function, oxygenation and other organ function, and impairs the ability to give such additional therapies as increased IV pharmacologic therapy (such as vasopressors) or parenteral nutrition.
[0026] 3. Mechanical Fluid Removal Therapies
[0027] Once pharmacological therapy is exhausted, Continuous Renal Replacement Therapy (CRRT) has been used to treat patients suffering from excess fluid overload. CRRT has been performed previously using standard methods of hemodialysis and continuous arterio-venous hemofiltration (CAVH). More recently, continuous veno-venous hemofiltration (CVVH) has been used to reduce the complications associated with such issues as hemodynamic instability and need for arterial access.
[0028] In cases where drug therapy is no longer sufficient to support the patient, effective, intra-aortic balloon pumps (IABPs) are commonly used. IABPs provide limited support of blood flow and pressure in CHF. Other devices, including ventricular assist devices are invasive and costly, but effective at increasing blood flow. Implantation of these devices generally requires the patient to undergo heart transplantation.
[0029] 4. Failure of the Current Treatments for CHF
[0030] Current treatments for CHF share the common goal of the alleviation of symptoms, and the improvement of heart and kidney function. The cornerstone of the medical therapy of chronic CHF includes the use of angiotensin converting enzyme (ACE) inhibitors, positive inotropic agents, diuretics, digitalis, and more recently, beta-blockers with the amount of each drug used dependent on the stage of heart failure. While drug therapy is effective in the early stages of CHF, there is no truly effective drug treatment for the later stages of CHF. Acute CHF is generally treated with intravenous inotropic (“squeeze” enhancing) and vasopressor (blood pressure raising) agents in concert with intensive diuretic therapy. If this therapy fails, the patient can quickly develop severe fluid overload and suffer rapidly-worsening heart and kidney function. Intra-aortic balloon pumps (IABPs) are commonly used but of minimal benefit in CHF. Hemodialysis and hemofiltration have been shown to be effective in removing extra fluid, reducing symptoms and improving heart function, but its use is limited to the Intensive Care Units (ICU) patient population.
[0031] Surgical solutions exist, but are only used for the treatment of very end-stage heart failure. These therapies (such as LVADs) are very effective at increasing blood flow. However, they are invasive, costly and require the patient to undergo heart transplantation. Even with the wide variety of existing therapies, over 2,300,000 CHF patients become hospitalized each year at a cost of over $10 billion dollars to the health care system. New CHF therapies are needed.
[0032] B. A Large Unmet Clinical Need in Patients with CHF for Enhanced Fluid Removal
[0033] If excessive fluid is not promptly removed with medication, CHF patients are often intubated and placed on a ventilator. If the initial diuretic therapy has little affect, more aggressive treatment with increasingly potent diuretics is needed. In addition, inotropic agents such as dobutamine are administered to increase the pumping function of the heart and rise the blood pressure. Higher blood pressure is expected to assist in the perfusion of the kidneys and make diuretics work. In more recent years vasodilator therapy became a part of the standard therapy for a severely volume-overloaded, decompensated CHF patient. All the above-mentioned therapies as a rule require admission to the ICU. Potentially dangerous side affects of drugs, needed for advanced monitoring and intubation, are the main reasons for a typical ICU admission.
[0034] While there are many potential factors that cause a patient to be hospitalized, the primary causes of admission in CHF patients are symptoms of severe shortness of breath from fluid overload. Standard drug therapy is unable to remove excess fluid rapidly enough to prevent hospitalization before any increased standard medical therapy has time to work. There is a clear and unmet clinical need for a CHF treatment that allows physicians to rapidly, controllably and safely remove a clinically significant amount of fluid from a CHF patient. Such a treatment would reduce the need for excessive hospital admissions.
[0035] Symptoms of fluid overload are excessive fluid retained in the abdomen, legs and lungs. Of these, fluid in the lungs is the most important. Patients have difficulty breathing. Edema in the lungs leads to poor blood oxygenation. Poor oxygenation leads to acidosis and deleterious neurological and hormonal phenomena that increases vasoconstriction and load on the heart. In addition, vasoconstriction leads to reduced blood flow to the kidneys and diminishes the effectiveness of the main pharmacological means of fluid removal—diuretic treatment. This phenomenon is known as the “vicious cycle” of CHF heart failure.
[0036] As previously mentioned, hemodialysis and hemofiltration can be used to remove excess fluid from a patient, especially in patients whose kidneys are not working. The term “Renal Replacement Therapy” generally refers to any forms of dialysis, solute and fluid balancing therapy. These treatments circumvent the kidney and replace kidney functions. These treatments are not generally applicable to CHF patients having functional kidneys, but which lack sufficient blood flow to properly perform their kidney functions, especially the removal of excess fluids, e.g., water, from the body.
[0037] 1. Principles and Concept of Existing Methods of Renal Replacement Therapy
[0038] Renal replacement therapy performs two primary functions: ultrafiltration (removal of water from blood plasma), and solute clearance (removal of different molecular weight substances from blood plasma). The filter called “dialyzer” can be set up to perform either or both of these functions simultaneously, with or without fluid replacement, accounting for the various modes of renal replacement therapy. “Clearance” is the term used to describe the removal of substances, both normal and waste product, from the blood.
[0039] Ultrafiltration is the convective transfer of fluid out of the plasma compartment through pores in the membrane. The pores filter electrolytes and small and middle sized molecules (up to 20,000 to 30,000 daltons) from the blood plasma. The ultrafiltrate output from the filtration pores is similar to plasma, but without the plasma proteins or cellular components. Importantly, since the concentration of small solutes is the same in the ultrafiltrate as in the plasma, no clearance is obtained, but fluid volume is removed.
[0040] Dialysis is the diffusive transfer of small solutes out of a blood plasma compartment by diffusion across the membrane itself. It occurs as a result of a concentration gradient, with diffusion occurring from the compartment with higher concentration (typically the blood compartment) to the compartment with lower concentration (typically the dialysate compartment). Since the concentration of solutes in the plasma decreases, clearance is obtained, but fluid may not be removed. However, ultrafiltration can be combined with dialysis.
[0041] Hemofiltration is the combination of ultrafiltration, and fluid replacement typically in much larger volumes than needed for fluid control. The replacement fluid contains electrolytes, but not other small molecules. Since the net effect of replacing fluid without small solutes and ultrafiltration of fluid with small solutes results in net removal of small solutes, clearance is obtained.
[0042] While effective at removing excess fluid, substantial clinical data exists showing that ultrafiltration provides significant other benefits to patients with CHF. These benefits include the promotion a variety of compensatory neurohumoral mechanisms, such as activation of the renin-angiotensin-aldosterone system and stimulation of the sympathetic nervous system, resulting in both sodium accumulation and increased peripheral vascular resistance. Commonly, fluid removal with diuretics further enhances the neurohumoral stimulation and may even aggravate heart failure in some patients. Ultrafiltration interrupts this vicious cycle and represents an alternative approach to the treatment of refractory heart failure. Further beneficial effects of ultrafiltration include a subsequent increase in urine output, and an increased responsiveness to standard oral diuretic therapy.
[0043] For example, one study randomized congestive heart failure (NYHA Class II to III) to treatment with ultrafiltration (1.3 to 2.6 L over 3 to 5 hours) or with furosemide (potent diuretic). Both treatments produced similar hemodynamic and fluid losses. However, three months after intravenous furosemide treatment, hemodynamics and fluid volume had worsened back to baseline values, yet they were still significantly improved in the ultrafiltration group. The data suggest that fluid removal by ultrafiltration shifts the abnormal set point for fluid balance to a more physiologic level, an effect not accomplished by furosemide, despite comparable amounts of volume removal. Several other clinical studies showed similar beneficial results. Thus, ultrafiltration appears to be a beneficial in patients with CHF, even those still responsive to standard medical therapy.
[0044] 2. Limitations of Existing Methods of Ultrafiltration to Treat CHF
[0045] Ultrafiltration has not been used widely in the treatment of patients with CHF, despite its apparent clinical benefits. There are several issues limiting the use of currently available ultrafiltration devices:
[0046] i. Prior ultrafiltration devices require central venous access (e.g., via surgery) with its attendant risk of infection, bleeding, collapsed lung and death.
[0047] ii. Prior ultrafiltration treatments require interaction and use by a nephrologist who is not the patient's primary physician, and who may be reluctant to expend their device and personnel resources on these patients.
[0048] iii. Prior ultrafiltration devices draw large blood volumes of blood out of the body and, thus, require central venous access. Moreover, the temporary large blood loss may lead to hypotension (low blood pressure) and the potential for large losses of blood.
[0049] iv. Prior ultrafiltration devices are generally designed to be only used in the ICU or dialysis unit environment.
[0050] v. Prior ultrafiltration devices require high blood volume flows to prevent clotting in the blood circuit and filter apparatus.
[0051] vi. Most patients are required to be anticoagulated leading to an increased risk of bleeding.
[0052] Continuous Veno Venous Hemofiltration (CVVH) allows removal of blood fluid and modification of the volume and composition of extracellular fluid to occur evenly over time. A filter that is highly permeable to water and small solutes but impermeable to plasma proteins and erythrocytes, is placed in the extracorporeal circuit. As the blood perfuses the hemofilter an ultrafiltrate is removed in a manner similar to glomerular filtration in the kidney.
[0053] Modern CVVH machines over time can provide almost complete renal replacement therapy (act as an artificial kidney) in an anuric patient. The technique is typically used in the ICU setting on a patient that has permanently or temporarily lost natural renal function as an alternative to intermittent dialysis. Secondary to the artificial kidney function, CVVH offers precision and stability that allows electrolytes or any appropriately sized element of circulation to be removed or added independently of changes in the volume of body water. In turn, if desired, the volume of water can be adjusted in a controlled fashion. Although valuable and powerful clinical tool, the versatility of CVVH limits its use in clinical practice and acceptance. The limitations of CVVH include:
[0054] i. Electrolyte removal and replacement is a high risk therapy. It is particularly risky in cardiac patients, since excess or depletion of electrolytes can cause arrhythmias. For this reason primarily, CVVH is prescribed and administered by a nephrologist.
[0055] ii. Large amounts of blood, in the range of 100-400 mL/min or as much as 10% of the total cardiac output for an adult patient, are passed through the filter. This necessitates the so-called “central” vascular access. Relatively-large and long catheters are threaded from a peripheral vein in an arm or a leg of the patient until they reach a large vascular volume in the center of the body where the sufficient blood flow is present. These cavities containing large volumes of blood can be the vena cava or the right atrium of the heart. To establish the central access a vascular surgeon or another similar specialist is required. Patients with central access catheters require additional monitoring. The central access is associated with serious complications.
[0056] iii. Tens of liters of fluid are continuously removed and replaced in a patient over the course of one day. If the desired balance is disrupted, patient can rapidly gain or lose fluid. The part of the machine responsible for fluid balance is called an ultrafiltration controller (UC). The UC of a modern CVVH machine has evolved into an extremely sophisticated apparatus capable of measuring the rate at which fluid is added or removed with the accuracy of less than 0.5%. This accuracy comes at a price of technical complexity and cost.
[0057] As a result, CVVH has in the past only been used in the ICU of a hospital where resources, training and adequate nursing monitoring are available. In addition, controls of CVVH machines are difficult to understand and require extensive training. Although the latest and most sophisticated apparatus “Prisma” from Gambro takes advantage of interactive computer screens to simplify the task of setting up the device and controlling its use, it still requires many parameters to be configured before the device can be used.
[0058] Mechanical fluid removal such as SCUF (Slow Continuous Ultrafiltration) or CVVH is not used in these patients until it becomes obvious that the natural kidney function is insufficient. This typically is a result of an Acute Renal Failure (ARF) secondary to hypotension and hypoperfusion of the kidneys. The CVVH is prescribed by a nephrologist.
[0059] Abundant scientific and clinical evidence exists that aggressive early fluid removal with a machine would benefit CHF patients. It can reduce symptoms of fluid overload, prevent intubation, reduce load on the heart and reduce neuro-hormonal stimuli that drive vasoconstriction. To be truly affective the treatment shall precede the onset of ARF and shall be placed in the hands of a cardiologist who is the primary physician responsible for a CHF patient.
[0060] Current clinical use of CVVH in heart failure can be described as “too little too late”. As a result, CVVH is used for many days not as much for fluid removal but as an acute renal replacement therapy (similar to dialysis) in patients with lost renal function.
[0061] With the increasing prevalence of decompensated CHF and the increased cost of hospital admission and even more so of ICU treatment, a strong need has emerged for a new technology that will allow fluid removal in the non critical care setting. This need is for a device and technique that is simple and safe so that it could be used in the outpatient setting, doctors offices, Emergency Rooms (ER) and general hospital floors.
SUMMARY OF THE INVENTION
[0062] To better address this important therapeutic modality and eliminate these significant limitations, the inventors have developed a novel method and device that safely performs ultrafiltration using only the blood drawn from a peripheral vein.
[0063] One advantage of an embodiment of the invention is that it does not require surgery or ICU, and can be administered to patients in emergency rooms, clinics and other such facilities. The majority of the total of the 2.5 million CHF patients admitted per year in the United States do not require an ICU. The admission of many of these cases to the hospital could be adverted altogether if there existed a safe, simple means to remove excess fluid from these patient to relieve the CHF symptoms of fluid overload.
[0064] An embodiment of the invention includes a device that is suited to extract excess fluid from a CHF patient at a clinically relevant rate that will overcome the deficiencies of existing machines for renal replacement therapy and particularly could be used outside of an ICU. The embodiment of the invention provides a simple excess fluid extraction (SAFE) system for use with CHF patients.
[0065] The embodiment of the invention avoids the need for a central access to venous blood. Central access catheters such as 10 or 14FR catheters from Medcomp PA can are primarily used in the ICU or special dialysis setting. Thus, a device requiring central access to venous blood was generally not used to treat CHF patients, other than the most sick CHF patients.
[0066] An embodiment of the invention provides an acceptable level of invasiveness for a fluid removal treatment in the desired environment and patient population via a peripheral vein preferably in an arm of a patient. Such access is commonly established by a nurse to draw blood or to infuse drugs. An embodiment of the invention does not require an ICU or a special dialysis setting to be administered to a patient. If an apparatus for slow continuous ultrafiltration was available that would draw and re-infuse blood into the body using the access site similar to a common IV therapy, such device would have a widespread clinical use.
[0067] Extracorporeal blood treatment are known in the prior art where blood is continuously withdrawn from, processed and returned into the same or different vein in the patient's arm. For example, such methodology is commonly used in blood apheresis treatment. Examples of apparatus for plasma apheresis are Spectra or Trima from Gambro. The major limitation of peripheral access is the relatively modest amount of blood that can be withdrawn per unit of time. It is accepted that in almost all patients the blood flow of 40-60 mL/min can be established. In some cases blood flow of up to 100 mL/min can be achieved. Blood flow available from a peripheral vein is therefore a great deal lower than the blood flow of 100-400 mL/min that is required to operate renal replacement therapy machines such as Prisma or BP11 in an adult patient.
[0068] This apparently insufficient blood flow from a peripheral vein was perceived by the engineering and medical community as a prohibiting factor. In spite of an apparent clinical need, the peripheral vein ultrafiltration was never developed or even investigated. Rather than take the blood flow requirement on the “face value”, applicants analyzed the medical and engineering considerations behind the requirement for blood flow. They developed a clinically-useful method and apparatus for fluid removal that can operate at blood flows of less than 100 mL/min and preferably of 40 to 60 mL/min.
[0069] Existing renal replacement therapy machines and specifically ones used in acute setting to perform SCUF and CVVH therapy were all designed to primarily perform hemofiltration and hemodialysis, not fluid removal. Blood is composed of cellular components suspended in the fluid component called plasma. Water is the primary constituent of plasma in which physiological solutes such as sodium and potassium are dissolved. In plasma the larger molecules, proteins and blood cells, are suspended. Ultrafiltration and hemofiltration operate by convection. In ultrafiltration, a solute molecule is swept through a membrane by a moving stream of ultrafiltrate. Proteins and blood cells are retained by the membrane. In patients with renal failure, renal replacement therapy, such as hemofiltration or dialysis, removes undesired solute. In renal replacement therapy, vital elements such as electrolytes are removed from the blood and need to be replaced.
[0070] During hemofiltration solute removal is entirely dependent on convective transport. Hemofiltration is relatively inefficient for solute removal, as compared to dialysis. Hemodialysis allows the removal of water and solutes by diffusion across a membrane in the direction of the concentration gradient. Diffusion transfers solute molecules across the membrane in the direction of the lower solute concentration at the rate inversely proportional to the molecular weight.
[0071] Hemodialysis requires a large membrane surface to enable effective solute clearance by diffusion. Hemofiltration requires large amount of ultrafiltrate to be transferred across the membrane to remove a relatively small amount of solute. This is a consequence of convection being an inefficient method of solute transport. Large amounts of fluid such as 1 to 4 liters per hour (L/hour) are continuously being removed during CVVH. The resulting loss of water and electrolytes are immediately dangerous to the patient. To maintain fluid and electrolyte balance, equally large or slightly lower amount of replacement fluid is infused into the patient. Replacement fluid is thus added into the extracorporeal blood circuit before or after the filter.
[0072] There is a straightforward dependency between the maximum amount of ultrafiltrate removed from the blood and the flow (volume per unit time) of blood that must pass through the filter. Blood condenses in the filter as the water is removed. The water is removed as it is sieved from the blood in the filter. In practice only approximately 20% to 30% of the ultrafiltrate volume can be removed from blood safely as water. If more is removed, the blood becomes too dense with red blood cells and protein and will flow sluggishly.
[0073] Also, filter membranes are designed to pass water and small solutes as ultrafiltrate, but to retain red blood cells and proteins. This inherently limits the amount of fluid that the filter can remove per unit of surface area of the membrane. The permeability of a filter to ultrafiltrate per unit of driving Trans Membrane Pressure (TMP) is a constant called the ultrafiltration coefficient (KUF) of a filter. The KUF of blood filters has increased dramatically in recent years. In modern CVVH machines filters with KUF as high as 50 mL/hour/mmHg are used. For example, the popular Fresenius F-series of filters have KUF of 20, 30 and 40. The higher KUF of filters was achieved by using more permeable membranes. Permeability of fibers is measured in mL/hour/m2/mmHg. The permeability of fiber used in Fresenius filters is 33 mL/hour/m2/mmHg Higher permeability membranes allow efficient ultrafiltration with smaller membrane surface areas. This method of increasing efficiency of ultrafiltration has inherent limitations. KUF of a membrane substantially higher than 50 mL/hour/m2/mmHg cannot be achieved since the filter will eventually become permeable to proteins.
[0074] In general, an increase in the flow of ultrafiltrate requires a larger filter membrane surface. The rate of ultrafiltration can be somewhat improved by increasing the TMP, but the effectiveness of this method is also limited. When TMP increases over a value of 200-300 mmHg, the ultrafiltration rate stops increasing and will actually start dropping if TMP is increased much further. This is explained by the fouling of the membrane. Proteins are pushed into the pores of the membrane by higher TMP and the actual KUF of the membrane becomes lower than the theoretical KUF. Eventually the membrane is clogged and the ultrafiltration stops. Also high TMP leads to hemolysis and distruction of red blood cells.
[0075] These limitations are well known and accepted in the industry. As a result, filters used for CVVH in adults have the membrane surface area of 0.7-2 m2. The required minimal surface area drives several design constraints of the filter. A substantial number of hollow membrane fibers (typically >3,000) are used in parallel to create the desired surface area in a bundle of practical length. This determines the area of the contact of blood with an artificial material and the time of the exposure of blood to that material for a given blood flow. Prolonged exposure to plastics is known to trigger the process of coagulation of blood. Unless undesirable high doses of anticoagulants such as heparin are used, blood flowing slowly through a filter with a substantial membrane surface area will inevitably clot. In fact, filter clotting is the number one problem of both intermittent dialysis and continuous hemofiltration. To prevent blood from clotting in the filter substantial blood flows in access of 100 mL/min are maintained through the extracorporeal circuit. As a result, although CVVH machines such as Gambro Prisma can, according to the specification, pump blood at flows as low as 10 mL/min, these flows are not practical and are never used in adults.
[0076] The above-mentioned facts frame an unsolvable problem for a designer of a CVVH machine that would function reliably for many hours and draw blood from a peripheral vein access. The blood flow available is not sufficient to provide the clinically useful rate of solute removal using any existing filter material or design. In addition, the high extracorporeal flow of blood is likely to require close monitoring of the patient even in the presence of a sophisticated ultrafiltration controller. The existing ultrafiltration controllers are based on either integration of flow or measuring weight of removed and added fluid. Both measurement methodologies are dependent on calibration and are sensitive to drift, noise and artifacts.
[0077] To overcome some of the problems with CVVH, applicants determined that the invention need not provide total renal replacement therapy. Patients with fluid overload resulting from decompensated heart failure do not suffer from acute or chronic renal failure. Their needs are different from the ICU patients that the CVVH is used on. The intrinsic kidney function of these patients would be sufficient to remove fluid and solute if the vasoconstriction of the renal artery was not limiting the blood flow to the kidney. In those patients that respond well to diuretics, kidneys usually start functioning quite adequately after the initial 2-5 liters of excessive fluid is removed.
[0078] The total renal function can in general be divided into water and solute removal. An embodiment of the present invention provides a water removal function, but does not provide solute removal. An apparatus of an embodiment of the present invention may not be capable of removing clinically significant amount of solute. The lack of solute removal in an embodiment of the present invention is beneficial in that it does not significantly remove electrolytes from the blood. In heart failure patients, loss of electrolytes can lead to dangerous arrhythmias. Moreover, even with very low daily urine output the kidney is capable of the solute clearance that is sufficient to sustain metabolic equilibrium. Kidney can concentrate solute in as little as 0.6 liters per day of urine. However, this amount of urine output is not sufficient to maintain the fluid balance. Accordingly, the kidneys of a CHF patient may be sufficient for solute removal needs, and require the assistance of the present invention for water (fluid) removal.
SUMMARY OF THE DRAWINGS
[0079] A preferred embodiment and best mode of the invention is illustrated in the attached drawings that are described as follows:
[0080] FIG. 1 illustrates the treatment of a fluid overloaded patient with an embodiment of the present invention.
[0081] FIG. 2 illustrates the operation and fluid path of the preferred embodiment of the present invention.
[0082] FIG. 3 is a graphical illustration tracing how the desired average ultrafiltration rate of 250 mL/hour is achieved with a 50% duty cycle control.
[0083] FIG. 4 illustrates another embodiment of the invention when more precise removal of fluid is desired.
[0084] FIG. 5 is a graph comparing the effect of the reduction of the filter membrane area on the residence time of blood by comparing transit time of blood in contact with plastic tubing, a standard F40 filter, and the filter described herein.
[0085] FIG. 6 is a graphical representation illustrating that the desired amount of ultrafiltrate can be removed with the filter described in the preferred embodiment.
[0086] FIG. 7 is an illustration of another embodiment of the invention with an apparatus designed for removing blood in a batch type process using a single needle and blood storage bag.
DETAILED DESCRIPTION OF THE INVENTION
[0087] For the proposed clinical use, the capability of the disclosed embodiment of the invention is to remove water drove the design. This is fortunate since the convection technique proposed here for removal of water is inefficient (in terms of the solute material removed per unit of the surface area of the membrane) in removing solute from the blood plasma. The functional kidneys of the patient are relied on to remove solutes from the plasma. The kidneys are, thus, relived of having to perform substantially all fluid removal from the blood.
[0088] FIG. 1 illustrates the treatment of a fluid overloaded patient with the embodiment of the invention 100 . Patient 101 can undergo treatment while in bed or sitting in a chair. Patient can be conscious or asleep. To initiate treatment two relatively standard 18 G needles 102 and 103 are introduced into suitable peripheral veins (on the same or different arms) for the withdrawal and return of the blood. This procedure is no different from blood draw or IV therapy. Needles and attached to tubing 104 and 105 and secured to skin with attachments 106 and 107 . The blood circuit that consists of the blood filter 108 , tubes, pressure sensors 109 , 110 and 111 and the ultrafiltrate collection bag 112 . The circuit is supplied in one sterile package and is never reused. It is easy to mount on the pump 113 and can be primed and prepared ready for operation within minutes by one person.
[0089] During operation, the disclosed embodiment of the invention requires minimal intervention from user. User sets the maximum rate at which fluid is to be removed from the patient using the control panel 114 . Ultrafiltrate is collected into a graduated one-liter collection bag 112 . When the bag is full, ultrafiltration stops until the bag is emptied. Information to assist the user in priming, setup and operation is displayed on the LCD display 115 .
[0090] FIG. 2 illustrates the operation and fluid path of the preferred embodiment of the present invention. The embodiment of the present invention consists of a microprocessor controlled console and a disposable kit. Disposable kit is bonded (with the exception of needles) and is supplied sterile.
[0091] Blood is withdrawn from the patient through the 18 Gage or similar withdrawal needle 201 . The needle 201 is inserted into a suitable peripheral vein in the patient's arm. Blood flow is controlled by the roller pump 204 . Before entering the pump blood passes through approximately two meters of plastic tubing 202 . Tubing is made out of medical PVC of the kind used for IV lines and has internal diameter (ID) of 3 mm. Pump is rotated by a DC motor under microprocessor control. The pump segment (compressed by the rollers) of the tubing has the same ID as the rest of the blood circuit. The system is designed so that approximately 1 mL of blood is pumped per each full rotation of the pump, e.g. pump speed of 60 RPM corresponds to 60 mL/min.
[0092] The disposable withdrawal pressure sensor 203 is a part of the blood circuit. Pressure sensor 203 is a flow-through type commonly used for blood pressure measurement. There are no bubble trap or separation diaphragms in the sensor design, which reduce the accuracy. Pressure sensor is designed to measure negative (suction) pressure down to −400 mmHg. All pressure measurements in the fluid extraction system are referenced to atmospheric. The withdrawal pressure signal is used by the microprocessor control system to maintain the blood flow from the vein. Typically, a peripheral vein can continuously supply 60-100 mL/min of blood. This assumption is supported by the clinical experience with plasma apheresis machines.
[0093] In some cases, blood flow can be temporarily impeded by the collapse of the vein caused by the patient motion. In other cases the vein of the patient may not be sufficient to supply the maximum desired flow of 60 mL/min. The software in the present invention microprocessor is designed to control the withdrawal of blood to prevent or recover from the collapse of the vein and reestablish the blood flow based on the signal from the withdrawal pressure sensor.
[0094] The same pressure signal from the sensor 203 is used to detect the disconnect of the withdrawal bloodline 202 from the needle 201 . This condition is detected by the abrupt decrease of the withdrawal pressure generated by the pump. The resistance of the 18 Gage needle, which is 4 cm long with an approximately 0.8 mm ID at a flow rate corresponding to a 60 mmHg, pressure drop is on the order of the 100 mmHg. The resistance of 2 meters of blood tubing with a 3.5 mm ID at the same flow rate is on the order of 20 mmHg. This enables automatic reliable detection of the line disconnection. The occlusion of the withdrawal bloodline is detected in the similar fashion. The occlusion can be caused by the collapse of the vein or by the kinked blood tube. Occlusion results in a rapid decrease (more negative) of the pump suction pressure that is detected by the microprocessor. In response to this condition, the microprocessor stops the pump and alarms the user.
[0095] The present invention uses a double roller pump 204 to pump blood. As the pump 204 rotates, rollers compress the segment of PVC tubing and generate flow. Pump 204 is adjusted to be fully occlusive until the pressure limit is reached. The rollers are spring loaded to limit the maximum positive and negative pressure generated by pump head. This feature is not normally used to limit pressure in the circuit and is only included as a secondary safety precaution.
[0096] A direct drive stepper motor rotates the rollers, and the speed of the motor is determined by the controller microprocessor. The RPM of the pump 204 is used as a feedback signal by the controller to determine the blood flow. Normal operational blood flow in the present invention is between 40 and 60 mL/min. This minimum rate of blood flow is needed to generate Trans Membrane Pressure (TMP) needed for ultrafiltration and to prevent stagnation and clotting of blood in filter 207 .
[0097] Pump pressure sensor 205 is incorporated into the post-pump segment of the blood tubing connecting pump 204 to the blood inlet port 214 of the filter 207 . Like other pressure sensors in the present invention it is a flow through device that does not create a blood-air interface and does not disturb the blood flow. The pump pressure signal is used by the microprocessor to determine TMP used to calculate the ultrafiltration rate. It is also used to detect abnormal conditions in the circuit such as occlusion or unacceptable clotting of the filter and disconnection of the blood line between the pump 204 and the filter 207 .
[0098] On its way from the pump 204 to the filter 207 , blood passes through the air detector 206 . The air detector 206 is of ultrasonic type and can detect air in amounts exceeding approximately 50 microliters. The detector 206 uses technology based on the difference of the speed of sound in liquid and in gaseous media. If an air bubble is detected, the pump 204 is stopped almost instantaneously (within few milliseconds). The bubble detector output signal is hard wired into the motor control logic and the pump 204 is stopped independently of the microprocessor control if a bubble is detected.
[0099] Air can only enter the present invention circuit from the pre-pump (negative pressure) segment of the blood circuit 202 . All the rest of the circuit downstream of the pump 204 is always pressurized. For this reason, the bubble detector is placed before the filter.
[0100] Blood pressure in the post pump, pre-filter segment of the circuit is determined by the patient's venous pressure, the resistance to flow generated by the return needle 210 , resistance of hollow fibers in the filter assembly 207 and the resistance of interconnecting tubing 208 . At blood flows of 40 to 60 mL/min the pump pressure is in the 300 to 500 mmHg range depending on the blood flow, condition of the filter, blood viscosity and the conditions in the patient's vein.
[0101] The filter 207 is a main component of the present invention. Inside the filter 207 the ultrafiltration occurs. Whole blood enters the bundle of hollow fibers from the connector on the top of the cap of the filter canister. There are approximately 700 hollow fibers in the bundle, and each fiber is a filter. Blood flows through a channel approximately 0.2 mm in diameter in each fiber. The walls of the channel are made of a porous material. The pores are permeable to water and small solutes but impermeable to red blood cells, proteins and other blood components that are larger than 50,000-60,000 Daltons. Blood flow in fibers is tangential to the surface of the filter membrane. The shear rate resulting from the blood velocity is high enough such that the pores in the membrane are protected from fouling by particles, allowing the filtrate to permeate the fiber wall. Filtrate (ultrafiltrate) leaves the fiber bundle and is collected in space between the inner wall of the canister and outer walls of the fibers.
[0102] The geometry of the present invention filter is optimized to prevent clotting and fouling of the membrane. The active area of the filter membrane is approximately 0.1 m2. The permeability KUF of the membrane is 30 to 33 mL/hour/m2/mmHg. These parameters allow the desired ultrafiltration rate of approximately 500 mL/min at the TMP of 150 to 250 mmHg that is generated by the resistance to flow. The effective filter length is 22.5 cm and the diameter of the filter fiber bundle is 1.2 cm. This results in the shear rate of 1,200 to 1,800 sec-1 at the blood flow rate of 40 to 60 mL/min.
[0103] The TMP in the present invention is defined predominantly by the resistance of the return needle 210 and the resistance of the filter bundle inside the filter 207 . The properties of the filter 207 and the needle 210 are selected to assure the desired TMP of 150 to 250 mmHg at blood flow of 40-60 mL/min where blood has hematocrit of 35 to 50% at 37° C.
[0104] The quantitative clinical goal was formulated for the apparatus being developed in terms of fluid removal. Applicants' research established that for the fluid removal device to be clinically useful it should remove water at the rate of 100 to 500 mL/hour. Lower rates of fluid removal are only required in hemodynamically unstable patients that are treated in the ICU and are not the targeted patient population. Fluid removal rates higher than 500 mL/hour (theoretically as high as 1,000 mL/hour) may be practical in some patients but are expected to be too high risk in the majority. It is only advisable to remove water from blood at the rate at which fluid can be recruited from tissue. Higher rates may lead to hypotension.
[0105] Blood hematocrit (volume fraction of red blood cells) in CHF patients is expected to be in the range of 30 to 40% of the total blood volume. It is possible to condense the filtered blood to the hematocrit range of 50% to 60% and still be able to return blood through a standard needle. Therefore, extraction of approximately 20% to 30% of volume from blood as water is possible. Assuming this extraction rate, the amount of blood removed from a peripheral vein is less than 2% of the total cardiac output. In addition, at this extraction rate, the potential ultrafiltrate flow may be as much as 1 L/hour. Alternatively, a lower extraction rate, e.g., 0.1 liter/hour, may be selected. At the blood flow rate of 60 mL/min applicants successfully extracted up to 12 mL/min (or 720 mL/hour) of ultrafiltrate in the laboratory using the filter described here. Therefore, it is possible to consistently extract the required 500 mL/hour of water from the blood flow withdrawn and returned into a peripheral vein.
[0106] Applicants established that the much higher blood flows that are used in adults by all existing renal replacement therapy machines and particularly by machines for acute CVVH treatment of CHF patients are necessitated by the filter designed to remove solute and more specifically by the relatively high surface area of the filter. This large surface area is needed for solute removal. If the goal of treatment was to remove water only, high blood flow will still be needed to reduce the time of exposure of blood to the synthetic membrane and to prevent clotting.
[0107] Another important consideration that forces the designers of CVVH machines to use high blood flow and consequentially the central venous access is the need to maintain substantially high wall shear rate of blood flowing inside the filter capillaries (hollow fibers). Flow of blood inside a fiber is laminar Shear rate at the wall can be calculated using the simple Equation 1:
[0000] y= 32 ×Q /( d 3 ×pi ) (Equation 1)
[0108] Q is blood volumetric mass flow rate and “d” is the internal diameter of the capillary.
[0109] The ultrafiltration rate is influenced by membrane fouling which is an equilibrium of wall shear rate and ultrafiltration rate per unit surface area. With the increasing surface area the wall shear rate will decrease unless the blood flow is increased to compensate. It becomes apparent from literature that the wall shear rate should be 1,000 sec-1 or higher to achieve sufficient filtrate flux at high hematocrit. It is also known from literature that the high shear rate in excess of 2,500 sec-1 is undesirable since it can cause hemolysis and damage to red blood cells. At the same time, it is apparent that the surface area and size of the filter should be minimized. Biocompatibility is inversely proportional to the surface area exposed to blood. The likelihood of clotting increases with residence time proportional to the filling volume. Also, cost of a smaller filter is lower.
[0110] To minimize the cost of the filter, the use of commercially-available fibers with optimized biocompatibility and consistent filtration properties is desired. Suitable filter fiber is available, for example, from Minntech Inc. in Minnesota. Each fiber has internal diameter of 0.2 mm. Pores in the fiber walls are optimized to retain solutes of greater than 50,000 Daltons. The permeability of this fiber is 33 mL/hour/m2/mmHg. If a membrane with total surface area of only 0.1 m2 is constructed from this fiber, the resulting theoretical ultrafiltration rate will be 330 mL/hour at TMP of 100 mmHg and 660 mL/hour at TMP of 200 mmHg. These numbers are consistent with the objective of the design.
[0111] To calculate the KUF of the filter, the permeability of fiber is multiplied by the surface area of the membrane. Therefore KUF filter=33×0.1=3.3 mL/hour/mmHg.
[0112] It is known from literature that the blood flow is not equal between the fibers in the filter bundle. Blood flow and consequentially the wall shear rate tends to be lower in the fibers closer to the periphery and higher in the central ones. Accordingly, blood residence time is longer in peripheral fibers. It is known from the practice of dialysis that the peripheral fibers tend to clot first.
[0113] To reduce the extracorporeal blood volume and the time that blood resides outside of the body it is desired to use blood lines that have internal diameter as small as practical without creating excessive resistance to flow. For our application, an internal diameter of around 3.0 mm is well suited. When blood exits the tubing and flows into the fiber bundle the diameter of the channel through which blood flows increases substantially. This creates turbulence and stagnant zones at the entrance into the bundle. These factors increase the probability of clotting.
[0114] It is therefore beneficial to design a filter that has a minimal but still practical diameter of the fiber bundle. This is achieved by reducing the number of fibers and increasing the length of the bundle. This approach is limited by two constraints. Resistance of the bundle to flow increases in proportion to the bundle length. Also, long filters substantially in access of 20-25 cm are difficult to manufacture and cumbersome to use.
[0115] Applicants chose to use a maximum length of the filter that is practical from the manufacturing standpoint. The resulting working length of the bundle is 22 cm (centimeters). To ensure the required surface area of the membrane, approximately 620 to 720 fibers of this length are need to be bundled in parallel. Assuming the fiber density of approximately 630 capillaries per cm2 the diameter of the bundle is 1.2 cm. Such filter can be easily manufactured using existing methods and equipment. At the blood flow of 40 to 60 mL/min and blood hematocrit of approximately 40%, the resistance of this filter to blood flow is on the order of 100 to 200 mmHg. This pressure level is acceptable for the design of a circuit with a standard peristaltic pump and an 18 to 20 Gage (internal diameter of 0.8-1.0 mm) return needle.
[0116] Applicants overcame the perceived impossibility of clinical peripheral vein ultrafiltration that limited the use of mechanical fluid removal in CHF patients outside of the ICU environment. Applicants did this by drastically reducing the filter membrane surface area compared to common dialysis or CVVH filters to maintain high shear rate and low blood residence time. Specifically, a filter with the membrane surface of less than 0.2 m2 and preferably 0.05 to 0.15 m2 can remove the desired 100 to 700 mL/hour of water from the extracorporeal blood flow of less than 100 mL/min or more specifically of 40 to 60 mL/min with an average blood cell residence time outside the body of less than 2 minutes, and may be less than 1 minute. Although the filter is made of high permeability fiber due to the small surface area the KUF of the filter is less than 5 mL/hour/mmHg or preferably 2 to 4 mL/hour/mmHg. Typical filters used in adult patients have KUF of 30 to 50 mL/hour/mmHg. The much lower KUF gives the present invention device design an advantage of inherently safer operation. Food and Drug Administration (FDA) classifies all filters with KUF greater than 8 mL/hour/mmHg as “high permeability dialyzers”. According to current FDA safety standards these devices have to be labeled for use only with ultrafiltration controllers that are independent of TMP based ultrafiltrate rate calculation. A small error of TMP measurement or a deviation of membrane permeability from the specification can result in substantial over or under filtration. The use of a low KUF filter enables, if desired, the present invention to avoid using a cumbersome and expensive ultrafiltration controller that typically involves a scale balance and an ultrafiltration pump.
[0117] A filter that is relatively long and narrow may optimize the blood flow inside the filter, maintain the desired wall shear rate and minimize membrane fouling and filter clotting. A filter with a fiber bundle that is approximately 20 cm long and 1.5 cm in diameter is particularly well suited for the application and is practical for manufacturing.
[0118] Filters for ultrafiltration of blood with small surface area of less than 0.2 m2 are known. Example of such filter is Miniflow™ 10 from Hospal. Miniflow has surface area of 0.042 m2 and KUF of 0.87 mL/hour/mmHg. All such filters without exception are used for hemofiltration therapy in neonatal patients and infants. The clinically used amount of blood flow through these filters is within the range that we targeted or 10 to 60 mL/min. Nevertheless, this amount of flow—if expressed as a fraction of the cardiac output for infants—is the same as the blood flow used in adult hemofiltration. Consequently, these infant filters are used with the central and not peripheral venous access.
[0119] To minimize clotting and fouling of the membrane it is desired to maintain substantially high blood flow through the filter even if the desired ultrafiltration rate is low. In traditional machines for renal replacement therapy it is typically achieved by reducing the TMP. Flow of ultrafiltrate is actively controlled by the roller pump in the ultrafiltrate removal line between the filter and the ultrafiltrate collection bag. When the pump is slowed down ultrafiltrate flow is retarded, pressure gradient across the membrane is reduced and ultrafiltration is slowed to the desired level. Alternatively, if the pump RPM is increased, the flow of ultrafiltrate is accelerated. Negative pressure can be developed by the pump to actively suck the ultrafiltrate across the membrane. For reasons of safety and simplicity, it was desired to have a machine that can reduce the ultrafiltration rate at the user command without an ultrafiltrate pump. For our preferred embodiment we used the duty cycle controlled ultrafiltration. A simple pinch valve is placed in the ultrafiltrate line. When the valve is closed, pressure across the membrane quickly equilibrates, and no ultrafiltration occurs. When the valve is opened, ultrafiltration occurs at the rate determined by the TMP and the KUF of the membrane. This rate can be calculated by the controller. Valve is cycled approximately every minute. The fraction of the cycle during which the valve remains opened determines the average rate at which fluid is removed.
[0120] Since the system embodying the present invention does not employ an ultrafiltrate pump that can create sub-atmospheric pressure on the ultrafiltrate side of the membrane, a simple and reliable method of controlling the total amount of fluid removed in one treatment iteration is possible. The ultrafiltrate is collected into a sealed bag that is connected by a tube to the ultrafiltrate collection chamber of the filter casing. During the treatment the bag is gradually filled up with fluid. It is desired to have a bag that has a relatively small volume and specifically volume of 0.5 to 1.5 liters. When the bag is full and its walls are fully distended, the pressure in the bag will start to rise until it is equal to the average pressure of blood inside the filter capillaries. Although some circulation of fluid is still possible in and out of fibers the net loss of fluid is zero. Until a nurse empties the bag, no removal of fluid is possible.
[0121] Pressure sensors are used in the blood circuit to alarm the disconnection and occlusion of blood lines. The pre- and post-filter pressure signals are also used to calculate TMP and ultrafiltration rate. Two types of pressure measurement devices are typically used in machines for renal replacement therapy.
[0122] Machines such as BP11 from Baxter use disposable air filled separation or drip chambers that are connected to permanently installed pressure sensors that are the part of the machine. This design introduces potentially hazardous air into the circuit. Air can cause embolism and accelerated clotting. Also, this type of measurement is affected by gravity.
[0123] Machines such as Prisma from Gambro use flexible silicone diaphragms to transmit blood pressure to sensors once again mounted on the apparatus itself. This method overcomes the deficiencies of drip chambers. Separation diaphragms are subject to error when the travel of a diaphragm is restricted. This necessitated a complicated diaphragm positioning system if the system is used for a substantial duration of time. Also, a substantial area of a diaphragm (typically 2-3 cm in diameter) is required to ensure reliable transmission of pressure. At a low blood flow it is likely that a stagnant zone will form inside the diaphragm chamber that will eventually lead to clotting.
[0124] The present invention utilizes flow through disposable pressure sensors. This sensors are a part of the disposable blood circuit. They do not disturb the laminar blood flow inside the blood line since the internal diameter of the sensor element is the same as of the blood tubing (3 mm) The sensing element is less than 2 mm in diameter and is embedded flush in the wall of the sensor housing. The housing is bonded flush with the internal wall of the blood line tube to form a continuous channel. Although similar disposable blood pressure sensors (such as ones made by Merit Medical of Utah) are used widely for invasive blood pressure measurement this design has never been previously used in an apparatus for fluid removal.
[0125] The present invention is intended to provide safe, controlled fluid removal in patients with fluid overload for up to 8 to 24 hours. These patients all suffer from decompensated chronic CHF and are admitted or on the verge of admission to a hospital. Regardless of the exact nature of their disease theses patients present at the hospital with a number of symptoms that manifest fluid overload and result in difficulty of breathing and pulmonary edema require immediate treatment. These patients are typically 5 to 20 kg over their dry weight and, if treated with diuretics, can tolerate fluid removal rates of up to 0.5 L/hour for until symptoms are relieved.
[0126] The intended use of the present invention is to assist in the initial removal of 2 to 4 liters of fluid that should result in the relief of symptoms and much improved responsiveness to medication. The present invention can be performed by a physician or nurse trained in the use of the device. Treatment can be performed in the setting of a monitored hospital floor, outpatient clinic or Emergency Room. The present invention is prescribed by a cardiologist. The main idea behind the present invention is to remove excess water from the patient's blood using a well-accepted ultrafiltration technique at the same rate at which the surplus fluid can be recruited from the tissue.
[0127] The intended use of the present invention is slow continuous removal of fluid by ultrafiltration of blood. Excessive removal of fluid can lead to hypotension and serious risks to health. If the fluid is removed from vascular space too fast, it is equally dangerous and can lead to hypotension. The principle method of treatment with the present invention is to remove fluid at a rate that allows vascular blood volume to be replenished with water that has accumulated in the interstitial space as a result of the patient's condition. Patients that should be treated by the present invention are typically 10 to 20 kg over their dry weight due to this excess water.
[0128] Potential excessive water loss or gain is a recognized hazard associated with RRT. Modern CRRT machines used in SCUF or CVVH mode can potentially remove and replace tens of liters of fluid from patient in a space of several hours. As a result, even a small error in fluid balance can result in severe risks to a patient. To prevent this from happening accurate ultrafiltration controllers are used that are based on continuous measurement of the weight of extracted and infused fluids. Ultrafiltration rate is adjusted accordingly by controlling the speed of an ultrafiltration pump that can apply negative or positive pressure to the ultrafiltrate side of the filter membrane.
[0129] In the case of the present invention, fluid gain is not a risk. The present invention is designed for fluid removal only. To prevent excessive removal of fluid from the patient, the present invention relies on a number of inherently safe features and materials properties rather than the ultrafiltrate pump controller.
[0130] Ultrafiltrate rate (UF) is a function of TMP, Permeability of the membrane and the membrane surface. Membrane surface is a constant and in the case of the present invention is 0.1 m2. Permeability of a filter membrane is expressed as ml of ultrafiltrate per hour per unit of the membrane surface area, and may be 30 to 33 mL/hour/m2/mmHg The resulting KUF of the filter may be 3 mL/hr/mmHg. KUF of a filter can decrease during the operation owing to the fouling of the membrane but can not increase unless the membrane is broken. Equation 2 takes into account the affects of oncotic pressure on the ultrafiltration rate. The KUF of the membrane is determined using animal blood at standard conditions such as hematocrit of 27%, temperature of 37° C. and appropriate concentration of protein and electrolytes. Although these conditions do not perfectly reflect clinical conditions in all patients it is a useful engineering approximation.
[0000] UF=TMP ×( KUF ×Area) (Equation 2)
[0131] In the present invention, TMP is a function of blood flow and the resistance of circuit elements downstream, including the filter. TPM can be calculated in real time by the microprocessor using equation 3 from the readings of pressure transducers.
[0000] TMP =( Pp−Pr )/2 +Pr−Pg (Equation 3)
[0132] Where Pp is the pump (pre filter) pressure, Pr is the return (post filter) pressure and Pg is a pressure generated by the weight of the column of ultrafiltrate. Given the unadjustable design of the ultrafiltrate circuit, Pg is a constant. For the 20 cm level difference between the filter and the level of fluid in the bag Pg is 17 mmHg
[0133] Substitution of the calculated TMP into Equation 2 gives a reasonable estimate of the ultrafiltration rate.
[0134] During the use of the present invention the operator sets the maximum allowed rate of ultrafiltration in mL/hour. Values between 100 and 500 mL/hour are allowed. The present invention microprocessor establishes the rate of withdrawal of blood in the range of 40 to 60 mL/min. This flow rate is determined by the quality of access. It is advantageous to establish and maintain blood flow constant.
[0135] Based on the pressure sensor readings the TMP is calculated. This allows the calculation of ultrafiltrate rate for known KUF of the filter.
[0136] If the ultrafiltration rate is higher than desired it is reduced using the solenoid ultrafiltrate pinch valve 213 in FIG. 2 . When the valve 213 is closed the pressure inside the ultrafiltrate compartment of the filter 6 rises rapidly until it is equal to the pressure in the blood compartment (fibers). When the system is in equilibrium, no ultrafiltration occurs. The pinch valve 213 is cycled approximately once per minute. The duty cycle (ratio of open to closed state) is calculated ratiometrically from the actual and desired ultrafiltration rate.
[0137] Traces on FIG. 3 illustrate how the desired average ultrafiltration rate of 250 mL/hour is achieved with a 50% duty cycle control. In FIG. 3 , graph 300 shows time 301 versus ultrafiltrate flow rate 302 . Times t 1 306 , t 2 307 , t 3 308 , t 4 309 , t 5 310 and t 6 311 are evenly spaced with equal periods between them. The valve position 303 shows during which periods the valve 213 is open 304 and closed 305 . For example, between time t 1 306 and time t 2 307 , valve 213 is open, but between time t 2 307 and time t 3 308 , valve 213 is closed. For example, when the valve is opened ultrafiltrate flow is 500 mL/min, shown by lines 312 . When the valve is closed it is zero, shown by lines 313 . Thus, using equal periods of opened valve 213 and closed valve 213 will effectively achieve an average flow rate equal to half of the open valve flow rate.
[0138] Other factors limiting the ultrafiltration rate are the amount of blood available for filtration and the hematocrit of the blood entering the filter. Equation 4 can be used to calculate the return blood hemotocrit HR from the blood flow BF, ultrafiltrate flow UF and withdrawal blood hemotocrit HW.
[0000] UF=BF ×( HR−HW )/ HW (Equation 4)
[0139] The safe pump 204 can deliver up to 60 mL/min of blood. The maximum amount of water that can be extracted from the blood is determined by the hematocrit of the return blood. As the water is extracted, hematocrit increases. This in turn increases the viscosity of blood. Blood entering the filter typically has hemotocrit of 35 to 45%. The corresponding viscosity is approximately 3 to 4 mPa-s. Viscosity of blood with the hematocrit of 60% is 6 mPa-s. At 70% hematocrit blood becomes too viscous to pass through the filter or the return needle.
[0140] The volume of the ultrafiltrate collection bag 215 determines total amount of fluid removed from the patient. The bag 215 is connected to the fluid removal port 211 of the filter 207 by the bonded PVC tube 212 . The ultrafiltrate collection system is sealed. When the bag is full, the pressure in the bag 215 rises until it is equal to the average pressure of blood in the filter fibers. Ultrafiltration is stopped until the bag is emptied by the operator by opening the ultrafiltrate valve 216 . The volume of the ultrafiltrate bag 215 is one liter. This automatically limits the maximum amount of water that can be removed from the patient without an operator's interaction. Bag 215 is transparent and has volume marks that allow user to read the actual amount of fluid removed in preferably 100 mL increments.
[0141] Blood exiting the filter 207 through the connector on the bottom of the filter casing is continuously returned to the patient through the return needle 210 . Blood flow leaving the filter is the same as the blood flow entering the filter if the ultrafiltrate clamp 213 is closed. If the clamp 213 is open ultrafiltration occurs and the blood is continuously fractured into the ultrafiltrate and more concentrated blood. The hematocrit and the volume of returned blood are determined by the ultrafiltration fraction, which is the volumetric fraction of the ultrafiltrate relative to the volume of whole blood entering the filter.
[0142] Blood return circuit pressure sensor 209 serves several functions. The return pressure is used in the TMP calculation that is in turn used to calculate input data for the control of the ultrafiltration rate. It is also used to detect a disconnected or occluded circuit. Excessive pressure signals the occlusion that can be caused by a kinked tube or a clotted needle. Since the resistance of the needle 210 is much higher than the resistance of the blood line 208 , disconnection of the needle from the tubing is easy to detect from an abrupt drop of the return pressure.
[0143] FIG. 4 shows another embodiment of the invention. This embodiment is preferred when more precise removal of fluid is desired. An ultrafiltrate pump 17 is used to pump and meter ultrafiltrate into the collection bag 13 . Weight scale 18 allows additional control and monitoring of the amount of the removed fluid. Ultrafiltrate pressure sensor 15 is used to monitor the TMP and to detect clotting or fouling of the filter. Blood leak sensor 16 is used to detect the leakage of red blood cells across the filter membrane if the membrane is damaged. The blood sensor is of photometric type and responded to the change of color of the ultrafiltrate.
[0144] FIG. 5 illustrates the effect of the reduction of the filter membrane area on the transient time of blood in contact with plastic. Experiments were performed using the thermodilution method. At the time mark 0 iced water flowing through the system at 60 mL/min replaced the room temperature water. Three curves show the time delay before the cold water reached the exit of the circuit (simulated return of blood to the patient). Curve 510 corresponds to a continuous 2 meter long tube with internal diameter of 3 mm with no filter at all. Curve 520 is the filter described in this invention. Curve 530 is the standard F40 filter by Frescenious. Traces show that the time of contact of blood with plastic during the treatment with proposed invention will be significantly shorter than that with a conventional dialysis machine.
[0145] FIG. 6 proves that the desired amount of ultrafiltrate can be removed with the filter described in the preferred embodiment. Curves 560 , 550 and 540 correspond to blood flows of 40, 50 and 60 mL/min accordingly. Animal blood with hematocrit of 27% at the temperature of 37° C. was used in the experiment. TMP was between 100 and 250 mm Hg and shear rate of blood inside the filter was maintained in the 1000 to 2000 sec-1 range. The desired amount of 5-10 mL/min of ultrafiltrate was filtered out of blood before it was returned into a vessel using a 18 Gage needle. Filter had surface are of 0.1 m2 with membrane permeability of 33 mL/hr/m2/mmHg supplied by Minntech. Filter bundle was made out of 700 fibers 22 cm long as described previously in this invention.
[0146] FIG. 7 shows yet another potential embodiment of the invention. This apparatus is of a batch type and uses one needle 60 . Blood is withdrawn from the vein and stored in the bag 51 . During the withdrawal phase roller pump 52 rotates counter clockwise. Approximately 50 mL of blood can be stored in the bag 51 . Valve 59 is open and valve 58 is closed so that the filter 54 is bypassed. Blood is then ejected from the bag 51 through the filter 54 back into the patient's vein through the needle 60 . Valve 58 is opened and valve 59 is closed and the pump 52 rotates clock wise. During this phase filtration occurs and the ultrafiltrate is collected in the bag 55 . Pressure sensors 53 and 56 are used to control the process so that vein does not collapse or over-extend and TMP is not too high. Air detector 57 is used to protect the patient from embolism. An anti-coagulant may be needed in view of the temporary storage of blood in the bag 51 .
[0147] The invention has been described in connection with the best mode now known to the applicant inventors. The invention is not to be limited to the disclosed embodiment. Rather, the invention covers all of various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
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An ultrafiltration filter for an extracorporeal blood circuit having an input for blood withdrawn from a human patient and a blood output for filtered blood to be infused into the patient including: a filter body having a length of at least 20 centimeters (cm) and an interior diameter of no greater than 1.5 cm; an input at a first end of the body to receive the withdrawn blood; an output at a second end of the body to discharge the filtered blood; a filter membrane in the body defining a blood passage through the body, wherein the membrane has an active filter membrane surface area of no greater than 0.2 meters squared (m 2 ) and the filter membrane blocks passage of blood molecules having a molecular weight cut of greater than 60,000 Daltons and a volume of the blood passage in the filter being less than two percent of a cardiac output of the patient, and an ultrafiltrate output to the body and open to a side of the filter surface area opposite to the blood passage.
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TECHNICAL FIELD
The present invention generally relates to coke oven construction and more specifically to an offtake piping of a coke oven with integrated flow control valve to adjust the raw gas flow from each individual oven chamber to the collecting main.
BRIEF DESCRIPTION OF RELATED ART
Conventionally in coke plants comprising a battery of coke ovens the raw gases (distillation gases and vapors) from each single oven are lead through an offtake piping to a collecting main extending typically over the entire length of the battery of coke ovens. The offtake piping itself typically comprises a standpipe (also known as riser or ascension pipe) extending upwardly from the oven roof and a gooseneck, i.e. a short curved pipe communicating with the top of the standpipe and leading to the collecting main. One or more spraying nozzles are arranged in the gooseneck to cool (quench) the raw gases from about 700-800° C. down to a temperature of about 80-100° C.
In order to individually control the gas pressure in each coke oven chamber, it is known to provide a control valve in the offtake piping or at its discharge opening in the collecting main, that allows to close and/or throttle the gas flow through the offtake piping. Such devices offer the possibility of continuously controlling the oven pressure during distillation time so as to avoid overpressure during the first phase of the distillation process, by maintaining a negative pressure in the collecting main, whereby emissions from doors, charging holes etc. can be fully reduced. Moreover, a continuous oven pressure control allows avoiding negative relative pressures at the oven bottom during the last phase of distillation when the coke gas flow rate is low.
A known type of pressure control valve is e.g. described in U.S. Pat. No. 7,709,743. This valve is arranged inside the collecting main at the discharge extremity of a vertical discharge section of the gooseneck. The valve permits controlling the backpressure in the oven chamber and is based on the adjustment of water level inside the valve, providing a variation of the valve port area through which the raw gas flows.
EP 1 746 142, which relates to a method of reducing the polluting emissions from coke ovens, uses a pot valve pivotable about a lateral axis. Each distillation chamber is connected by a gooseneck to a collecting main via such interposed pot valve. The oven pressure in the individual distillation chambers is detected by means of pressure sensors and the pot valve position is adjusted in order to control the flow rate to the collecting main depending on the pressure in the oven. In one embodiment, the valve member is provided with a curved tubular metal structure to limit the flow cross section during the beginning of the opening stroke. Despite the reliable design of this valve, it does not allow much progressivity in the flow rate control.
BRIEF SUMMARY
The disclosure provides an alternative coke oven offtake piping system with improved integrated flow control capability.
The present invention relates to a coke oven offtake piping system comprising a pipe assembly with a discharge section including a discharge pipe having a discharge orifice, a gate member cooperating with the discharge orifice for controlling the flow rate to the collecting main. At least one spraying nozzle is preferably provided for quenching the raw gas flow from the oven.
According to an important aspect of the present invention, the gate member is designed so as to be movable along the discharge orifice in order to present a closing surface to the extremity of the discharge pipe. This allows varying the opening area of the discharge orifice to control the flow rate to the collecting main.
Contrary to valves having a closure member, which is lifted off the valve seat in opening positions (as e.g. with the pot valve of EP 1 746 142), the gate member used in the present invention has an operating movement that is configured for moving along the discharge orifice. The gate member, seen with respect to the discharge orifice, is thus moved somewhat transversally in front of the discharge orifice rather than away from (resp. closer to) the discharge orifice. In practice, for high flow rates, the gate member is advantageously in a position where it does not at all cover/obstruct the discharge orifice (typically is laterally parked). Partial obturation is obtained by progressively moving the gate member below the discharge orifice to cover a desired proportion of the discharge orifice. This is, in practice, not possible with a valve design where the closure member is lifted off from the valve seat in the opening position, since it is quite difficult to precisely control the spacing between the valve member and the valve seat. Since there is no lifting movement, the part of the closing member that obstructs the discharge orifice can be maintained at a constant distance from the pipe extremity: this allows a precise control of the opening area while limiting leaks due to the operating gap between the closure member and discharge pipe.
The closing surface of the gate member may be flat or curved. In the case of a flat gate member, its operating movement can be a simple translation from the side of the discharge pipe (fully open) to a desired position under the discharge pipe to partially or fully obstruct the discharge orifice.
Alternatively, the closing surface of the gate member may be curved, in which case the closure member may describe a pivoting operating movement around a pivoting axis allowing its pivoting along the discharge orifice to obstruct a desired proportion of the discharge orifice (preferably between 0 and 100%). The gate member may thus present a generally convex or concave surface profile to the extremity of the discharge pipe, preferably with a constant curvature radius. In practice, the gate member may be a spherical or cylindrical cap.
For improved flow regulation capability towards the end of the distillation phase, at least one cut-out is advantageously arranged in the gate member or in the discharge pipe about the discharge orifice so as to form a variable section opening during a portion of the pivoting stroke of the gate member. The cut-out is preferably positioned so that, as the gate member has been progressively closed to reduce the opening area of the discharge orifice, the latter is completely obstructed by the gate member except for the opening defined by the cut-out, which itself can be reduced by further moving the gate member in the closing direction.
Such valve design with fine flow control capability provides a simple and efficient solution for precisely controlling the flow rate to the collecting main at low pressures inside the coke oven chamber (typically towards the end of the distillation phase).
The shape and number of cut-outs can be adapted at will, in order to provide the desired flow characteristics trough the valve. Preferably the cut-out(s) is(are) arranged to extend inwardly from an edge of the member in which they are provided. In case the cut-out is to be borne by the discharge pipe, it may e.g. be arranged in an inwardly extending lip at the bottom of the discharge pipe that follows the curvature of the closing member. In another embodiment cut-outs are formed by a series of holes in the gate member, arranged about an edge thereof.
For ease of implementation, the cut-out (or a plurality thereof) is arranged in the gate member so that the discharge pipe may be a simple cylindrical or frustoconical pipe. Preferably, the cut-out extends inwardly from an edge of the gate member. The cut-out is arranged in the closing member at a position where it will form a reduced, variable section opening towards the end of the closing stroke of the gate member. For example the cut-out can be provided on the leading edge of the gate member, so that as from a given position of the gate member, the gate member will completely obstruct the discharge orifice except for the opening area defined by the cut-out and the rim of the discharge opening.
Advantageously, the gate member is designed in such a way that in the closed position, its peripheral borders extend upwardly beyond the extremity of the discharge orifice, so that a hydraulic seal forms and closes the operating gap between the orifice and the gate member as process fluid collects in the gate member cavity.
Preferably, the concave (or convex) surface profile of the gate member has a centre of curvature that is substantially coaxial with the pivoting axis. This allows pivoting the gate member about the discharge orifice with a constant operating gap between the two parts. Alternatively, a slight shift between pivoting axis and curvature centre may exist, to provide a metallic contact between parts in the closed position.
In one embodiment, the discharge pipe extends in a discharge cage connecting the collecting main; and spray means are provided to spray the outer wall of the discharge pipe. Spray means are advantageously arranged in the discharge cage so that in certain partially open positions of the gate member, sprayed fluid flows between the outer wall of the discharge pipe and the gate member cavity and forms a hydraulic seal.
To avoid water accumulation in the discharge pipe up above a certain level, overflow means may be integrated in the discharge pipe, excess water being evacuated into the discharge cage.
A conventional-type pot valve may be provided downstream of the gate member to permit sealed closure of the offtake piping. However, as mentioned above, when the gate member forms a cavity with borders extending beyond the discharge orifice, such pot-valve is not needed since a hydraulic seal forms in the gate member cavity.
As illustrated in FIG. 23 , any appropriate drive means may be used for pivoting the gate member about its axis at an end of the discharge pipe 20 . Typically the gate member 24 may be supported by one or two arms 231 , whose opposite extremities can be housed in bearings 232 coinciding with the pivoting axis A. The actuation mechanism 223 may be designed to permit manual and/or automated actuation.
In one embodiment, the closing member is a spherical cap with a truncated edge that forms a flat leading edge of the gate member. This is an interesting alternative to a full spherical cap because the leading edge can provide a narrower flow area when associated with a circular discharge orifice.
As illustrated in FIG. 24 ,the coke oven offtake piping system 242 according to the present invention can be associated to one or more actuator(s) 223 for its actuation. The actutaror(s) 233 is/are controlled by an electric/electronic control unit 244 also connected to pressure sensor(s) 243 in the coke oven 241 chamber. The control unit 244 is advantageously configured to—based on the detected pressure—progressively adjust the position of the gate member 246 relative to the discharge orifice to provide a progressive constriction of the discharge opening as the pressure varies in the oven 241 chamber.
As illustrated in FIG. 25 , the present invention also concerns a coke plant 250 comprising a battery of coke ovens 251 and a collecting main 253 , wherein the gases from each single oven 251 are lead to said collecting main 253 via a coke oven offtake piping system as defined hereinabove. In a coke plant 250 equipped with such offtake piping system, the oven pressure can be continuously controlled during distillation time so as to avoid overpressure during the first phase of the distillation process, by maintaining a negative pressure in the collecting main 253 , whereby emissions from doors, charging holes etc. can be fully reduced. Such continuous oven pressure control further allows avoiding negative relative pressures at the oven bottom during the last phase of distillation when the coke gas flow rate is low.
According to another aspect of the present invention, there is proposed a method of controlling the gas flow rate from coke ovens, wherein a battery of coke oven chambers are each connected by a coke oven offtake piping system as described above to a collecting main. The method comprises the steps of detecting the oven pressure in the individual coke oven chambers by means of pressure sensors, and based on the detected pressure, progressively adjusting the position of the gate member relative to the discharge orifice to provide a progressive constriction of the discharge opening as the pressure varies in the oven. This method can be implemented using appropriate actuators, e.g. solenoid-type, for the gate member that are controlled by a control circuit responsive to the pressure signals generated by the pressure sensors. The actuators may be coupled to positional transducers generating position signals received by the control unit.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be more apparent from the following description of several not limiting embodiments with reference to the attached drawings, wherein:
FIG. 1 : is a vertical section view through a first embodiment of an coke oven offtake piping system in accordance with the present invention, the gate member being in the closed position;
FIG. 2 : is a section of the piping system of FIG. 1 with the gate member in a partially open position;
FIG. 3 : is a section of the piping system of FIG. 1 with the gate member in the fully open position;
FIG. 4 : is a vertical section view through the gate member and discharge pipe of FIG. 1 ;
FIG. 5 : is a vertical section view through the gate member and discharge pipe of FIG. 1 , the cutting plane containing the pivoting axis of the gate member;
FIG. 6 : is a perspective view of the gate member of FIG. 1 ;
FIG. 7 : is a top view of the configuration shown in FIG. 4 ;
FIG. 8 : is a top view of an alternative embodiment with a cylindrical gate member and square discharge pipe;
FIG. 9 : is a perspective view of the gate member of FIG. 8 ;
FIG. 10 : is a top view of another embodiment with a cylindrical gate member and square discharge pipe; and
FIG. 11 : is a perspective view of the gate member of FIG. 10 ;
FIG. 12 : is vertical section view through an alternative embodiment of cooperating gate member and discharge pipe;
FIG. 13 : is a front view of FIG. 12 ;
FIG. 14 : is vertical section view through another alternative embodiment of cooperating gate member and discharge pipe.
FIG. 15 : is a front view of FIG. 12 ;
FIG. 16 : is a top view of FIG. 14 ;
FIG. 17 : is a perspective view of the gate member of FIG. 14 ;
FIG. 18 : is vertical section view through a further alternative embodiment of cooperating gate member and discharge pipe.
FIG. 19 : is a front view of FIG. 18 ;
FIG. 20 : is a perspective view, from below, of the discharge pipe of FIG. 18 ;
FIG. 21 : is a vertical section view through another embodiment of a coke oven offtake piping system, where the bottom of the discharge pipe has a plurality of cut-outs and the gate member is shown in the closed position;
FIG. 22 : is a view of the piping system of FIG. 21 with the gate member in a Partially open position;
FIG. 23 illustrated a portion of a coke oven offtake piping system;
FIG. 24 illustrated a block diagram of a control system for controlling a gate member of an offtake piping system; and
FIG. 25 illustrated a block diagram of a coke plant according to an embodiment of the invention.
DETAILED DESCRIPTION
FIG. 1 shows a preferred embodiment of a coke oven offtake piping system in accordance with the present invention. It comprises a piping assembly for conveying the raw distillation gas from an individual coke oven chamber to the collecting main. In the present embodiment, the piping assembly comprises a standpipe (not shown) connected at its bottom to the roof of a coke oven (not shown), e.g. a slot-type chamber of a coke oven battery. Reference sign 12 indicates a gooseneck (curved pipe) for conveying the raw coke oven gases (arrow 16 ) from the upper part of the standpipe to the collecting main 14 of the coke plant, which typically extends over the entire length of the battery of coke ovens. These piping elements may be conventionally provided with a refractory lining. Gases exiting the oven chamber at a temperature of about 700 to 800° C. are quenched in the gooseneck 12 by means of one (or more) spraying nozzle 18 (spraying process fluid such as ammonia water or the like) down to a temperature of 80-100° C.
Intermediate the gooseneck 12 and the collecting main 14 is a discharge section, generally indicated 19 , with a cylindrical (may also be e.g. a conical segment) discharge pipe 20 having a discharge orifice 22 . The quenched gas exiting the gooseneck portion 12 thus flows to the collecting main 14 via the discharge section 19 . A gate member 24 cooperating with the discharge orifice 22 allows controlling/throttling the gas flow rate to the collecting main 14 .
It shall be appreciated that the gate member 24 is designed so as to be movable along the discharge orifice 22 , which allows varying the opening area of the discharge orifice 22 . In the present embodiment the gate member is pivotable about a pivoting axis 26 (perpendicular to the cutting plane of FIG. 1 ) and presents a generally concave surface profile to the bottom extremity of the discharge pipe 20 . The concave surface profile preferably has a centre of curvature located essentially coaxially with the pivoting axis 26 , whereby the gate member 24 can be pivoted along the discharge orifice 22 . Main operating phases of the present gate member 24 are illustrated in FIGS. 1 to 3 . At the beginning of the distillation process, where large amounts of gas are to be drawn off, the gate member 24 is in a fully open position (laterally parked) so that it does not obstruct the discharge orifice 22 (see FIG. 3 ; also note the compactness of this position). As the distillation goes on, the opening area of the discharge orifice 22 is reduced by pivoting the gate member 24 in the clockwise direction in order to obtain the desired flow conditions through the offtake piping (one partially open position is shown in FIG. 2 ). In FIG. 1 the gate member 24 is in the closed position and completely obstructs the discharge orifice 22 .
In addition, to provide a fine flow control capability, a cut-out 30 is advantageously arranged in the gate member 24 so as to form a variable section opening during a portion of the pivoting stroke of the gate member 24 . This can be better understood from FIGS. 4-7 , which simply illustrates the gate member 24 and the discharge pipe 20 of the discharge section 19 .
As can be seen in FIG. 6 , in the present embodiment the gate member is designed as a spherical cap. A single cut-out 30 extends inwardly from an edge of the gate member 24 (here the cut-out is arranged in the front or “leading” edge portion seen in the closing direction). The cut-out 30 is dimensioned so that in the closed position of the gate member 24 ( FIG. 1 ), its innermost extremity is located outwardly beyond the discharge orifice 22 . Logically, the cut-out 30 preferably extends substantially perpendicularly to the pivoting axis 26 . In the position of FIG. 1 the discharge orifice is thus completely closed, because the cut-out 30 is beyond the rim of orifice 22 .
As mentioned, the aim of the cut-out is to permit a fine flow control capability towards the end of the distillation phase. In the position of FIG. 2 where the gate member 24 partially obstructs the discharge orifice, the opening area corresponds to the area defined between the rim of the discharge orifice 22 and the peripheral, leading edge of gate member 24 . As the gate member is further closed (further pivoting in the clockwise direction) the gate member 24 moves to the left along the discharge orifice 22 and covers and increasingly greater proportion of the discharge orifice 22 . Once the foremost point of the leading edge arrives below the rim of the discharge orifice (position indicated F with phantom lines in FIG. 2 ), the discharge orifice 22 is fully obstructed by the gate member 24 , except at the location of the cut-out 30 . Pivoting the gate member 24 further in the clockwise direction will progressively reduce the opening area (see e.g. FIG. 7 ) defined by the cut-out 30 and the rim of the discharge orifice until the cut-out passes beyond the rim ( FIG. 1 ).
The discharge pipe 20 and gate member 24 thus act as a throttling valve in the present offtake piping system, which has a fine flow control capability that is useful for controlling the pressure and flow towards the end of distillation phase.
Any appropriate drive means (not shown) may be used for pivoting the gate member about its axis 26 . Typically the gate member may be supported by one or two arms, whose opposite extremities can be housed in bearings coinciding with the pivoting axis. The actuation mechanism may be designed to permit manual and/or automated actuation.
Another advantageous design aspect of the present throttling valve is that due to the spherical inner shape of the gate member 24 and to the location of its pivoting axis 26 , it can be pivoted about the discharge orifice 22 with a constant operating gap between the bottom extremity of tube 20 and the inner cavity of the gate member 24 . Minimizing this operating gap permits limiting gas leakages. Indeed, when desiring to finely control the gas flow rate through the variable section opening formed with the cut-out 30 as in FIG. 5 , it is preferable to avoid significant gas leakages between the gate member 24 and discharge pipe 20 . The present design thus permits to avoid such leakages. The operating gap may e.g. be of about 1 mm, but is preferably less than one mm.
As mentioned above, in the position of FIG. 1 the gate member 24 completely obstructs the discharge orifice 22 . In addition, the peripheral edge of the gate member 24 extends above the discharge orifice 22 . Hence, in the closed position, process liquid will accumulate in the cavity formed by the gate member and rise to a level above the discharge orifice 22 , thereby forming a hydraulic seal. In such case, the present throttling valve can also sealingly close the communication between the oven chamber and the collecting main 14 , so that no other closing valve is required.
In the present embodiment, the discharge section 19 comprises a discharge cage 32 in which the discharge pipe 20 extends. Spray means 34 are arranged so as to spray process fluid on the outer surface of the discharge pipe 20 . It may be noticed that in the configuration of FIG. 2 where the gate member 24 is in a partially open position, the process fluid will collect in the upper, outer region of the gate member and form a hydraulic seal about the operating gap between the discharge pipe 20 and gate member 24 (as indicated by arrow 23 ). Use of ammonia water e.g., as for spraying nozzle 18 , also permits cleaning of the piping elements.
In order to prevent excessive process fluid accumulation in the closed position of the gate member 24 up to the gooseneck 12 , overflow means 35 are advantageously arranged in the upper part of the discharge pipe 20 . As can be understood from FIG. 1 , liquid rising up to the level of the overflow means 35 will be evacuated through the overflow means 35 and fall in the discharge cage 19 . Under normal operating conditions a certain level of water remains in the overflow means 35 , which avoids gas leakage.
The discharge section 19 is connected to the collecting main 14 via an expansion joint realized between the bottom of the cage 32 and a cylindrical connecting portion 36 bearing a U-shaped peripheral rim 38 . The U-shaped rim 38 is filled with tar or like material and thus provides a sealed joint with some expansion capability, as known in the art. Connecting portion 36 has a flanged bottom by means of which it is screwed to the collecting main 14 .
Although not required since the present configuration of gate member 24 allows to sealingly close the discharge opening 22 , a conventional pot-valve 40 can be arranged downstream of the gate member 24 . Here the pot-valve 40 cooperates with a frustoconical sleeve 42 . In FIG. 1 the pot valve 40 is in the closed position: it bears against the bottom of sleeve 42 . In such position, the pot-valve fills up with process falling from above and forms a hydraulic seal, as is well known. In FIGS. 2 and 3 , pot valve 40 has been pivoted about axis 44 in its open position.
FIGS. 8-11 illustrate alternative configurations with a cylindrical gate member 124 a or 124 b and square discharge pipe 120 . To provide a liquid collecting cavity, the ends of the cylinder are closed by walls 150 ; this is however not mandatory should a hydraulically sealed gate not be required. Gate member 124 b ( FIG. 11 ) is provided with a single cut-out 30 of similar shape than gate member 24 , whereas gate member 124 a bears a set of five cut-outs 130 . As it is clear from the drawings, the opening and flow control principle is the same as for the embodiment of FIGS. 1 to 7 .
It may be noted that in the case of a cylindrical gate member, the pivoting axis of the gate member may be slightly shifted (from one to several mm) from the centre of curvature of the cylinder, so as to obtain a metal to metal contact between gate member 124 a or 124 b and the discharge pipe 120 on the side bearing the cut-out(s). These axes may however also be coaxial.
The above embodiments provide an offtake piping with improve flow control capapility, permitting a precise control of oven backpressure. The gate member 22 may act as a shutoff and throttling member that offers the possibility of continuously controlling the oven pressure during distillation time, with a fine control function. This flow control capability permits to avoid overpressure during the first phase of the distillation process, by maintaining a negative pressure in the collecting main, whereby emissions from doors, charging holes etc. can be fully reduced. Moreover, a continuous oven pressure control allows avoiding negative relative pressures at the oven bottom during the last phase of distillation when the coke gas flow rate is low. Coke oven pressure control thus permits to achieve both emission reduction (during first phase of distillation) and prevention of air infiltration (during last distillation phase).
Turning now to FIGS. 12 and 13 , they concern an alternative embodiment where the gate member 224 is a full spherical cap (i.e. without cut-out) associated to a circular discharge pipe 20 .
FIGS. 14-17 show another embodiment using a truncated spherical cap 324 as gate member: as can be understood from the Figs., the leading edge of the gate member 324 is flat. It corresponds to a cut in a vertical plane when the cap 324 lies on its vertex (see FIG. 4 e.g.). Compared to the full spherical cap 224 , this design makes it easier to control fine flows (compare FIGS. 12 and 14 , resp. 13 and 15 ).
Finally, a further embodiment of the valve design is illustrated in FIGS. 18-20 . Here the gate member is a full spherical cap (i.e. without cut-out) and the cut-out 230 for fine flow control is arranged in the discharge pipe 220 . As can be seen, on the closing side of the discharge pipe 220 , the latter has a lip 232 portion extending inwardly and having the same curvature as the gate member 424 . The cut-out 230 is arranged in this lip 232 . Towards the end of the closing stroke of the gate member 424 this cut-out 230 provides a fine flow control capability, until the discharge orifice 222 is fully obstructed.
As it will be understood, the person skilled in the art may design the gate member so that its leading edge has a profiled shape (with one or more cut-out or truncated segment), which is formed so as to provide a desired flow characteristic (flow vs stroke position) towards the end of the closing stroke/movement.
Still a further embodiment of the present invention is illustrated in FIGS. 21 and 22 , which essentially varies from the embodiment of FIG. 1 in that the bottom end of discharge pipe 20 is provided with a plurality of cut-outs 25 . The cut-outs 25 extend inwardly (here axially and upwardly) from the discharge orifice 22 . The gate member 24 , preferably taking the form of a spherical cup, and the cut-outs 25 are configured so that in the closed position of FIG. 21 , the peripheral borders of the gate member 24 extend upwardly above the upper, closed end of the cut-outs 25 . Hence, when the gate member 24 is completely filled with process liquid having accumulated in its cavity, the liquid level is at a level above the openings formed by the cut-outs 25 , thereby forming a hydraulic seal.
It may be noted that this embodiment allows a fine throttling of the gases towards the end of the closing stroke based on the liquid level. Indeed, the liquid level in the gate member 24 and the angular position of the latter to define a throttling area through the cut-outs 25 . For example in FIG. 22 the level of liquid is indicated 27 ; the top region of the cut-outs 25 is thereby not obstructed by the process liquid and the gas flow is made possible therethrough. The flow area through the cut-outs 25 is thus dependent on the angular position of the gate member 24 and level of liquid therein. In other words, the gas flow rate is set by adjusting the angular position of the gate member so as to control the leak flow of process liquid.
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A coke oven offtake piping system includes a pipe assembly for conveying coke oven gases from a coke oven to a collecting main, at least one spraying nozzle in the pipe assembly, and a discharge section with a discharge pipe having a discharge orifice. A gate member cooperates with the discharge orifice and is movable along the discharge orifice in order to present a closing surface to the extremity thereof, whereby the opening area of said discharge orifice can be varied for controlling the flow rate to the collecting main. The gate member is a spherical cap with a concave closing surface. The gate member is configured to pivot around a pivoting axis to expose the discharge orifice and to cover the discharge orifice, respectively.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims priority from U.S. Provisional Application Ser. No. 62/051,153, filed Sep. 16, 2014, herein incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] The present invention pertains generally to medical catheters and methods of percutaneous delivery of a catheter to a site within the body for diagnostic or therapeutic purposes. More particularly, the present invention relates to a rapid exchange catheter having a tethered or fixedly attached vena cava filter and a method for percutaneous delivery of the rapid exchange vena cava filter for use in indicated medical situations in which prophylactic or therapeutic protection against pulmonary embolism are indicated.
[0003] The accepted standard of care for patients with venous thromboembolism (VTE) is anticoagulant therapy. Inferior vena cava (IVC) filters are reserved for those patients who fail anticoagulant therapy, or have a complication or contraindication to anticoagulant therapy. Until the early 1970's, the only method of IVC interruption was surgical, either by clipping, ligation or plication. The first clinical experience of an endoluminally-placed device to interrupt IVC flow was reported by Mobin-Uddin et al. in 1969. However, it was not until the introduction of a stainless steel umbrella-type filter by Greenfield et al. in 1973 that an effective method of endoluminally trapping emboli while simultaneously preserving IVC flow became possible. Indeed, for many years, the Greenfield filter set a benchmark by which newer filters were measured. Early generations of filters were inserted by surgical cut-down and venotomy. Eventually filters were able to be inserted percutaneously: initially through large 24 Fr sheaths, though newer generations of filters are able to be delivered through 6 Fr systems. Percutaneous delivery through a 6 Fr introducer minimizes the likelihood that surgical intervention to close the access site will be required when the system is withdrawn from the patient.
[0004] Despite the safety and efficacy of modern day filters, systemic anticoagulation remains the primary treatment for VTE. Either unfractionated or low molecular weight heparin followed by three months of oral anticoagulation in patients with proximal deep venous thrombosis (DVT) is approximately 94% effective in preventing pulmonary embolism (PE) or recurrent DVT. The routine placement of IVC filters in addition to anticoagulation in patients with documented DVT was investigated by Decousus et al. in a randomized trial. Decousus H, Leizorovicz A, Parent F, et al. A clinical trial of vena caval filters in the prevention of pulmonary embolism in patients with proximal deep-vein thrombosis. N Engl J Med 1998; 338:409-415. This study revealed that the use of a permanent filter in addition to heparin therapy significantly decreased the occurrence of PE within the first 12 days compared to those without a filter. However, no effect was observed on either immediate or long-term mortality, and by 2 years, the initial benefit seen in the group of patients with filters was offset by a significant increase in the rate of recurrent DVT.
[0005] Despite the efficacy of anticoagulant therapy in the management of VTE, there are certain situations and conditions in which the benefits of anticoagulation are outweighed by the risks of instituting such a therapy. These include contraindications and complications of anticoagulant therapy. In such circumstances, there may be absolute or relative indications for filter insertion.
[0006] Currently, there are several different types of U.S. Food and Drug Administration (“FDA”) approved vena cava filters. These include the Bird's Nest filter (Cook Incorporated, Bloomington, Ind.), Vena Tech LGM filter (B. Braun, Bethlehem Pa.), Vena Tech LP (B. Braun), Simon Nitinol filter (Bard, Covington, Ga.), Titanium Greenfield filter (Boston Scientific, Natick Mass.), Over-the-Wire Greenfield filter (Boston Scientific), TrapEase filter (Cordis Corp.) and the Günther Tulip filter (Cook Inc.).
[0007] Well-founded concerns over the long-term complications of permanent IVC filters, particularly in younger patients in need of PE prophylaxis with a temporary contraindication to anticoagulation, has led to the development of temporary and retrievable filters. Temporary filters remain attached to an accessible transcutaneous catheter or wire. These have been used primarily in Europe for PE prophylaxis during thrombolytic therapy for DVT. Currently these devices are not approved for use in the United States. Retrievable filters are very similar in appearance to permanent filters, but with modifications to the caval attachment sites and/or hooks at one end that can facilitate their removal. Retrievable filters that are currently available in the United States include the Günther Tulip (Cook Inc.), Opt Ease (Cordis Corp.), and Recovery nitinol filters (Bard Peripheral Vascular, Tempe, Ariz.) Lin P H, et al., Vena caval filters in the treatment of acute DVT. Endovascular Today 2005; January: 40-50. The time limit of retrievability is in part dependent on the rate of endothelialization of the device, which typically occurs within 2 weeks, but may occur within five days or as much as 30 days. However, differences in design may extend the time period in which the filter may be safely retrieved.
[0008] Currently no consensus exists as to which patients have an indication for a retrievable filter. However, it is generally accepted that patients at high risk for pulmonary embolism or with documented PE and with a temporary contraindication to anticoagulation are candidates.
[0009] Certain circumstances preclude the placement of a filter in the infrarenal IVC. This includes thrombus extending into the infrarenal IVC, renal vein thrombosis or pregnancy. The safety of suprarenal placement of IVC filters is well documented, with no reported instances of renal dysfunction and no differences in the rates of filter migration, recurrent PE or caval thrombosis.
[0010] Pulmonary embolism may complicate upper extremity DVT in 12-16% of cases. In patients who have such a complication or contraindication to anticoagulation, a filter can be safely placed immediately below the confluence of the brachiocephalic veins. However, misplacement of an SVC filter is theoretically more likely than with an IVC filter because of the relatively short target area for deployment.
[0011] The most common imaging modality used for filter insertion is fluoroscopy, performed either in an interventional suite or an operating room. Bedside placement of filters has inherent advantages, particularly for critically ill patients in intensive care settings where transport can be avoided. Portable fluoroscopy, surface duplex ultrasound and intravascular ultrasound (IVUS) have all been used to assist with bedside filter placement.
[0012] Vena cava filter placement frequently occurs concomitantly with central access line placement.
SUMMARY OF THE INVENTION
[0013] The present invention relates to a central access catheter having a vena cava filter at a distal end, a port proximal the filter and a port distal the filter and plural infusion ports. Accordingly, it is an objective of the present invention to provide a rapid exchange catheter coupled to a vena cava filter that is useful both as a central venous access catheter for administration of intravenous fluids, bioactive agents, contrast agents, flushing agents, pressurized fluids for mechanical thrombolysis and/or withdrawal of blood samples and for capture of thrombus or emboli.
[0014] Another aspect of the present invention is to provide a filter geometry in which the proximal portion of the filter, relative to the axis of blood flow, has larger interstitial openings to permit thrombus or embolic material to flow into the filter, while the distal portion of the filter, again relative to the axis of blood flow, has relatively smaller interstitial openings that capture the thrombus or embolic material within the filter. Another way to view this aspect is that the structure of the filter includes a greater open surface area exposed to the flow of embolic material into the filter at its proximal end, while the distal end has smaller open surface area exposed to the flow of embolic material to capture the embolic material in the distal end of the filter member.
[0015] Yet another aspect of the present invention is to provide an asymmetrical vena cava filter in which the vena cava filter has a distal end that is asymmetrical relative to a proximal end of the filter. In accordance with this aspect of the invention, the vena cava filter includes a first conical section and a second conical section, with each of the first and second conical sections forming one of the proximal end or distal end of the filter. Each of the first and second conical sections taper long the longitudinal axis of the catheter member such that an apex of each conical section is generally co-axial with the longitudinal axis of the catheter member and the catheter member passes through a central longitudinal axis, and both apices of the first and second conical sections, respectively.
[0016] It is yet another aspect of the invention to provide a rapid exchange vena cava filter catheter in which a proximal aspect of the catheter has a first diameter and a distal aspect of the catheter has a second larger diameter than the proximal aspect of the catheter.
[0017] It is still yet another aspect of the invention to provide a rapid exchange vena cava filter catheter having a rapid exchange guide wire port passing through the distal aspect of the catheter. The rapid exchange guide wire port further includes a seal that permits a guide wire to be passed into and through a central lumen of the catheter, and exit through the rapid exchange guide wire port, while the seal substantially seals the rapid exchange guide wire port such that medically significant fluid flow does not pass through the rapid exchange guide wire port during use within the body.
[0018] Still another objective of the present invention is to provide a contrast port medial along a length of the rapid exchange vena cava filter catheter. The contrast port is positioned in a medial position along the length of the rapid exchange vena cava filter catheter in order to allow for sufficient distance between the contrast port and the vena cava filter member for dispersion of a contrast medium within the blood flow to optimize visualization of the vena cava filter member, any region proximal to the filter member, and any thrombus captured by the vena cava filter member.
[0019] A further object of the present invention is to configure the medial contrast port such that a flow of contrast agent out of the contrast port occurs only when the contrast agent is introduced at or above a predetermine pressure, while allowing other fluids introduced below such threshold predetermined pressure to pass through the central lumen of the catheter system and bypass the contrast port.
[0020] These and other objects, features and advantages of the present invention will be more apparent to those skilled in the art from the following more detailed description of the invention with reference to the accompanying Figures. In the accompanying Figures, like reference numerals refer to similar features across multiple embodiments of the invention. It will be understood by those skilled in the art that while the Figures describe the present invention with reference to exemplary embodiments, the present invention is intended to be limited only by the claims appended hereto. Moreover, it will be understood by those skilled in the art that various features of the invention may be described with reference to one or more embodiments and are intended to be applicable to each embodiment described in the specification and within the scope of the appended claims.
DESCRIPTION OF THE FIGURES
[0021] FIG. 1 is a perspective view of a rapid exchange vena cava filter catheter in accordance with the present invention.
[0022] FIG. 2A is a fragmentary cross-sectional view of a section of the inventive rapid exchange vena cava filter catheter illustrating a rapid exchange guide wire port and a medial contrast port.
[0023] FIG. 2B is a fragmentary top view taken from direction of arrow 2 B in FIG. 2A and is a section of the inventive rapid exchange vena cava filter catheter illustrating a rapid exchange guide wire port and a medial contrast port.
[0024] FIG. 2C is a fragmentary top view taken from direction of arrow 2 C in FIG. 2A and is a section of the inventive rapid exchange vena cava filter catheter illustrating a rapid exchange guide wire port and a medial contrast port.
[0025] FIG. 3A is a side elevational view of a medial contrast port in accordance with the present invention.
[0026] FIG. 3B is a transverse cross-sectional view taken along line 3 B- 3 B of FIG. 3A .
[0027] FIG. 4 is a side view of a section of the inventive rapid exchange vena cava filter catheter with the sheath shown in phantom illustrating the rapid exchange guide wire port, the medial contrast port and an in-line flow restrictor insert within a lumen of the inventive catheter.
[0028] FIG. 5 is a perspective view of another embodiment of a rapid exchange guide wire port of the inventive rapid exchange vena cava filter catheter.
[0029] FIG. 6 is a cross-sectional view taken along line 6 - 6 of FIG. 5 .
[0030] FIGS. 7A-7C are sequential perspective views depicting a method of assembling the rapid exchange guidewire port depicted in FIG. 5 .
[0031] FIG. 8A is a top elevational fragmentary view of a proximal hub of the inventive rapid exchange vena cava filter in accordance with the present invention.
[0032] FIG. 8B is an exploded perspective view of the proximal hub of the rapid exchange vena cava filter in accordance with the present invention.
[0033] FIG. 9A is a side elevational view of the proximal hub of the inventive rapid exchange vena cava filter catheter in accordance with the present invention.
[0034] FIG. 9B is a top plan view of the proximal hub of the inventive rapid exchange vena cava filter catheter in accordance with the present invention.
[0035] FIG. 10 is a side elevational view of a vena cava filter member of the inventive rapid exchange vena cava filter catheter in accordance with the present invention.
[0036] FIG. 10A is a cross-sectional view taken along line 10 A- 10 A of FIG. 10 .
[0037] FIG. 10B is a cross-sectional view taken along line 10 B- 10 B of FIG. 10 .
[0038] FIG. 11 is a side elevational view of another embodiment of the vena cava filter member of the inventive rapid exchange vena cava filter catheter in accordance with the present invention.
[0039] FIG. 12 is a cross-sectional view taken along line 12 - 12 of FIG. 11 .
[0040] FIG. 13 is a cross-sectional view taken along line 13 - 13 of FIG. 11 .
DETAILED DESCRIPTION OF THE INVENTION
[0041] In accordance with the present invention, there is provided a rapid exchange vena cava filter catheter 100 . Rapid exchange vena cava filter catheter 100 includes generally a vena cava filter member 110 that is coupled to an elongate member 120 , such as an elongate wire 120 . The vena cava filter member 110 is more fully described with reference to commonly owned U.S. Pat. Nos. 8,613,753, 8,668,712, 8,771,226, 8,777,977, 8,777,981 and/or 8,808,323, each of which is hereby incorporated by reference. Briefly, the vena cava filter member 110 is formed of a plurality of strut members forming first and second conical sections of the filter member 110 . The first and second conical sections define proximal and distal ends of the filter member 110 . Each of the first and second conical sections have a base and an apex, with the apices of each of the first and second conical sections forming one of the proximal and distal ends of the filter member 110 , with the base of each conical section being positioned intermediate the proximal and distal ends of the filter member 110 .
[0042] The rapid exchange vena cava filter catheter 100 also includes a catheter sheath member formed from a proximal catheter sheath 114 and a distal catheter sheath 112 . At a proximal end of the proximal catheter sheath 114 is provided a proximal hub 116 . The catheter sheath member has a central longitudinal lumen that extends from and is in fluid flow communication with the proximal hub. The central longitudinal lumen of the catheter sheath extends to a distal end 119 of the catheter sheath member and terminates at a distal opening in the distal catheter sheath 112 . An elongate wire 120 passes through the catheter sheath member and extends at its proximal end from the proximal hub and is coupled near its distal end to the filter member 110 . In another embodiment, the elongate wire 120 may be a tube, including, for example a single lumen or a multi-lumen tube to provide an additional lumen the rapid exchange or dual lumen design configurations. As used herein, the term elongate wire 120 is intended to encompass a wire or a tube. The elongate wire 120 is capable of being longitudinally translated within and through the catheter sheath member in order to push the filter member 110 out of the distal end 119 of the catheter sheath member and also retract the filter member 110 back into the distal end 119 of the catheter sheath member. An atraumatic tip 122 is provided at a very distal end of the elongate wire 120 to facilitate navigation of the rapid exchange vena cava filter catheter 100 through the vasculature or other anatomic passageway.
[0043] A rapid exchange guide wire port 118 is provided in the catheter sheath member and is positioned generally at the transition between the proximal catheter sheath 114 and the distal catheter sheath 112 . The rapid exchange guide wire port 118 permits a guide wire 102 to exit from the rapid exchange guide wire port 118 .
[0044] Each of the first and second conical sections of the filter member 110 are asymmetrical relative to each other. For example, a length of the first conical section will be either greater than or less than a length of the second conical section. Additionally, the number and configuration of struts forming the first conical section will be different than the number and configuration of struts forming the second conical section of the filter member 110 . It has been found advantageous to configure the filter member 110 such that whichever of the first and second conical sections are oriented toward the direction of fluid flow within the body structure, i.e., retrograde relative to the fluid flow, that section have a lower number of struts and interstitial openings between struts in that section be of a relatively larger open surface area relative to the other section that is oriented away from the direction of fluid flow within the body structure, i.e., antegrade relative to the fluid flow. For example, when delivered infra-renal within the inferior vena cava by a femoral approach, blood flow is in a cephalic direction, i.e., toward the patient's head, thus, the conical section of the filter member 110 that tapers toward an apex that is retrograde to the blood flow within the inferior vena cava, i.e., pointed caudal relative to the patient, will be configured to have interstitial spaces relatively larger than the conical section of the filter member 110 that tapers toward and apex that is antegrade to the blood flow with in the inferior vena cava, i.e., pointed cephalic relative to the patient, which will be configured to have interstitial spaces that are relatively smaller in order to capture thrombus. FIGS. 10 and 11 , described in greater detail hereinafter, illustrate this described configuration and orientation of the filter member 110 .
[0045] The rapid exchange guide wire port 118 is depicted in FIGS. 2A-2B in greater detail. As discussed above, the rapid exchange guide wire port 118 consists of a large opening in the side wall of the rapid exchange catheter member. It will be understood that port 118 may be positioned at any longitudinal position along the length of the rapid exchange catheter member. However, for purposes of illustration and in accordance with one aspect of the present invention, rapid exchange guide wire port 118 is positioned at the transition between the proximal catheter sheath member 114 and the distal catheter sheath member 112 . Proximal catheter sheath member 114 has a transverse diameter D 2 that is smaller than a transverse diameter D 1 of the distal catheter sheath member 112 . Alternatively, the catheter could be configured to have a substantially uniform diametric profile along the entire longitudinal length of the device depending on geometry required. The port 118 is positioned at the diametric transition between the proximal catheter sheath member 114 and the distal catheter sheath member 112 .
[0046] Because of its relatively large open surface area necessitated by its function, the guide wire port 118 must be sealed to prevent undesired fluid flow out of or into the port 118 . In order to seal port 118 , a resilient seal 130 is provided within the lumen 113 of the distal catheter sheath member 114 that seats against a luminal wall surface surrounding the rapid exchange guide wire port 118 . Resilient seal 130 is deformable in order to accommodate passage of a guide wire past the seal and through the port 118 opening, while still providing a substantially fluid tight seal to reduce or prevent fluids from passing through the port 118 opening. Resilient seal 130 preferably has a tapered section 134 that projects distally toward the vena cava filter member 110 , yet permits fluid to flow from lumen 113 in the distal catheter sheath member 112 past or through the resilient seal 130 and into a second lumen 135 in communication therewith within the proximal catheter sheath member 114 . In accordance with one aspect of the invention, resilient seal 130 consists of a generally tubular member that has a proximal end 132 which is generally cylindrical and capable of being joined to the proximal catheter sheath member 114 , and a distal end 134 that has a generally tapered frustroconical shape, tapering distally and ending in a distal seal opening 138 . Alternatively, the resilient seal 130 may have a generally tubular shape with one wall surface of the seal 130 forming a diametrically enlarged bulge 131 toward an intermediate aspect of the seal 130 which then tapers toward the distal end 134 and opens at distal seal opening 138 . The diametrically enlarged bulge 131 seats against the luminal wall surface perimeter rapid exchange guide wire port 118 to seal port 118 .
[0047] The resilient seal 130 has a seal lumen 135 that is in fluid communication at it proximal end 132 with the lumen 115 of the proximal catheter sheath member 114 and at its distal end 134 , distal seal opening 138 is in fluid communication with lumen 113 of the distal catheter sheath member 112 . In this manner, fluid introduced into proximal lumen 115 will pass through the resilient seal lumen 135 and into the distal lumen 113 of the distal catheter sheath member 112 , without exiting the rapid exchange guide wire port 118 .
[0048] FIGS. 5-6 illustrate an alternative embodiment of a resilient seal 200 and FIGS. 7A-7C represent a manner in which resilient seal 200 is disposed within the rapid exchange vena cava filter catheter 100 . In accordance with the alternative embodiment of resilient seal 200 , there is provided a resilient seal member 210 having a generally tubular cylindrical shape having a seal lumen 235 that passes through the resilient seal member 210 and opens at each end thereof. A proximal end 214 of the resilient seal member 210 is configured with an outer diameter sized to be inserted within and be coupled to an inner diameter of the proximal catheter sheath member 114 . Thus, as depicted in FIGS. 7A and 7B , a proximal end 214 of the resilient seal member 210 is engaged within the distal end of lumen 115 of the proximal catheter sheath member 114 . The proximal end 214 of the resilient seal member 210 may be joined to the proximal catheter sheath member 114 by any suitable method of creating just coupling, including, without limitation, reflow, thermal welding, ultrasonic welding, adhesive, interference or such other means for joining two components of a catheter device as are known in the art. Once the resilient seal 210 is joined to the proximal catheter sheath member 114 , the distal catheter sheath member 112 may be engaged over the resilient seal 210 , such that the guide wire port 118 is positioned over a portion of the resilient seal 210 , and the distal catheter sheath member 112 and the proximal catheter sheath member 114 are joined by any suitable method of creating just coupling, including, without limitation, reflow, thermal welding, ultrasonic welding, adhesive, interference or such other means for joining two components of a catheter device as are known in the art.
[0049] A distal end 216 of the resilient seal member 210 has a beveled wall surface 212 that tapers distally toward the vena cava filter member 110 forming a guide wire ramp. In this manner, as the vena cava filter catheter 100 is passed over a guide wire 102 , the guide wire 102 passes through distal lumen 113 of the distal catheter sheath member 112 , and will be deflected by the beveled wall surface 212 that forms a ramp, the resilient seal 210 will deform to guide the guide wire 102 toward and out the rapid exchange guide wire port 118 . In another embodiment, the guide wire ramp may be configured to facilitate guidance of the wire through the rapid exchange pathway, such as, for example, by forming a bevel or concave profile of the guide wire ramp.
[0050] The elongate wire 120 traverses the distal lumen 113 of the distal catheter sheath member 112 , the seal lumen 235 and the proximal lumen 115 of the proximal catheter sheath member 114 . While not shown in FIG. 5 or 6 , the resilient seal member 210 may also optionally be employed in conjunction with the contrast port opening 142 , sleeve 144 and contrast fluid outlet opening 146 as depicted in and described above with reference to FIGS. 2-3B . Moreover, while not shown in FIG. 5 or 6 , the resilient seal member 210 may also optionally be employed in conjunction with the flow restrictor member 160 as depicted in and described above with reference to FIG. 2 . Similarly, while not shown in FIG. 5 or 6 , the resilient seal member 210 may also optionally be employed in conjunction with all of the contrast port opening 142 , sleeve 210 , contrast fluid outlet opening 146 , and flow restrictor 160 , as depicted in and described above with reference to FIGS. 2-3B .
[0051] Optionally, a contrast port 142 is provided in the rapid exchange vena cava filter catheter 100 . Contrast port 142 may be disposed in a wall of the proximal catheter sheath member 114 and communicate with the lumen 115 of the proximal catheter member 114 . It has been found desirable to position the contrast port 142 sufficiently proximal the filter member 110 so that adequate dispersion of a contrast medium will occur at the position of the filter member 110 for visualization of the filter 110 and its placement, or for visualization of the region proximal to the filter member. In accordance with the exemplary embodiment of the invention depicted in FIG. 2 , the contrast port 142 is positioned proximal the rapid exchange guide wire port 118 and near a distal end 140 of the proximal catheter sheath member 114 .
[0052] A flow restrictor member 160 having a restrictor lumen 162 may optionally be provided and interposed intermediate the contrast port 142 and the rapid exchange guide wire port 118 . The restrictor lumen 162 is of a smaller diameter relative to the proximal lumen 115 of the proximal catheter sheath member 114 and is also smaller in diameter relative to the distal lumen 113 of the distal catheter sheath member 112 . In this manner, flow restrictor member 160 permits regulation of pressures at which contrast medium is either emitted from contrast port 142 or pressures at which fluids, including contrast medium, flow through the restrictor lumen 162 , through the resilient port seal 130 and through the distal lumen 113 of the distal catheter sheath member 112 , exiting the rapid exchange vena cava filter catheter 100 at its distal end 119 . It will be appreciated that at higher injection pressures, fluids, such as contrast medium, will encounter a back pressure exerted by the flow restrictor member 160 and will flow primarily out of the contrast port 142 , with a secondary flow passing through restrictor lumen 162 and into the distal section of the catheter 100 . At lower injection pressures, fluid will primarily flow distally through the restrictor lumen 160 and into the distal section of the catheter 100 . It will be understood by those skilled in the art that the relative diameter and length of the restrictor lumen 160 relative to the diameter of the proximal lumen 115 and distal lumen 113 will determine the pressure above which the primary fluid flow will exit the contrast port 142 .
[0053] Contrast port 142 may have an opening size dimensioned to regulate the outflow of contrast medium there through. However, in order to facilitate dispersion of the contrast medium in the blood flow, it has been found desirable to sheath the contrast port 118 with a sleeve 144 that circumferentially covers the proximal catheter sheath member 114 and covers the contrast port, while allowing a fluid flow channel 150 between an inner surface of the sleeve 144 and the outer surface of the proximal catheter sheath member 114 . A contrast fluid outlet opening 146 is provided in the sleeve 144 and is spaced apart from the contrast port 142 . One example is to position the contrast fluid outlet opening 146 180 degrees opposite from the contrast port 142 about the circumferential axis of the catheter sheath member 114 . This position allows for the contrast medium to flow bidirectionally about the entire circumference of the catheter sheath member 114 . Where the contrast fluid outlet opening 146 is formed as a slot oriented parallel to the longitudinal axis of the catheter sheath member 114 , the contrast medium will flow out of the contrast fluid outlet opening 146 in a substantially laminar flow. The contrast fluid outlet opening 146 may be a single or plural circumferentially oriented slots, helical slots, longitudinally oriented slots, circular openings, polygonal openings, or other shaped openings as are appropriate to provide for dispersion of a contrast medium as it is released from the contrast port 142 .
[0054] The sleeve 144 is preferably joined to the vena cava filter catheter 100 at proximal and distal aspects of the sleeve 144 , leaving the fluid flow channel 150 in an unjoined intermediate aspect of the sleeve 144 that overlays the contrast port 142 and is in fluid communication with the contrast fluid outlet opening 146 .
[0055] As illustrated in FIGS. 4 and 6 , the elongate wire 120 traverses the proximal lumen 115 of the proximal catheter sheath member 114 , passes through the flow restrictor lumen 162 , if the flow restrictor member 160 is present, through the lumen 135 of the resilient seal 130 and then into the distal lumen 113 of the distal catheter sheath member 115 . As noted above, the proximal end of vena cava filter member 110 is coupled to the distal end of the elongate wire 120 .
[0056] Turning now to FIGS. 8A to 9C , a proximal hub 300 in accordance with the present invention is illustrated. The proximal hub 300 forms the proximal end of the rapid exchange vena cava catheter 100 and is the proximal terminus of the proximal catheter sheath member 114 and the elongate wire 120 . The proximal hub 300 also provides fluid access for fluid injection into the proximal lumen 115 of the proximal catheter sheath member 114 .
[0057] The proximal hub 300 includes first section 310 and a second section 320 that cooperate with each other. The first section 310 , which is preferably a distal section of the proximal hub 300 , is formed of a housing 311 having a first channel 312 and a second channel 314 . First channel 312 has a receiving section 315 in a distal portion of the first channel 312 and a proximal section 317 . A proximal end of the proximal catheter sheath member 114 engages and seats within the receiving section 315 of the first channel 312 and is in fluid flow communication with the proximal section 317 . The proximal lumen 115 of the proximal catheter sheath member 114 is in fluid flow communication with the proximal section 317 of the first channel 312 . The second channel 314 has a proximal receiving section 319 and a distal section 321 . An extension line 316 engages and seats within the proximal receiving section 319 and is in fluid flow communication with the distal section 321 of the second channel 314 . Distal section 321 of the second channel 314 joins in fluid flow communication with the distal section 317 of the first channel 312 .
[0058] It has been found desirable that the first channel 312 be co-axial with a central longitudinal axis L of the proximal hub 300 and that the second channel 314 be angularly displaced from the central longitudinal axis L by an angle α. Angle α is preferably greater than 0 and less than or equal to 90 degrees, preferably between 15 and 45 degrees from the central longitudinal axis L.
[0059] The first housing 310 further includes a seating recess 350 that accommodates a hemostatic seal seating member 352 therein. Seating recess 350 is co-axial with the central longitudinal axis L and has a bore 354 in fluid communication with the proximal section 317 of the first channel 312 . Seating recess 350 has a generally annular shape and has a proximal receiving recess 356 in a proximal aspect of the seating recess 350 . Bore 354 tapers proximally and opens to the proximal receiving recess 356 .
[0060] There is also provided a hemostatic sealing member 340 that has a distal projection 342 and a sealing member 345 interfacing between the distal projection 342 and the proximal receiving recess 356 of the seating recess 350 in the first housing 310 . The hemostatic sealing member 340 further has a bore 344 passing through the hemostatic sealing member 340 and through the distal projection 242 that communicates with bore 354 in the seating recess. Finally, hemostatic sealing member 340 further includes an engagement section 348 having enlarged receiving bore 346 in a proximal aspect of the hemostatic sealing member 340 that communicates with the bore 344 .
[0061] Finally, the first section 310 includes at least one, preferably two, apertures 311 for securing the proximal hub 300 to the patient. In the illustrated embodiment in FIGS. 8A-9C , apertures 311 are present in suture wings that project outwardly from the first section 310 .
[0062] The second section 320 removably engages with the first section 310 , such as by a threaded connection or a luer-type connection. Second section 320 is rotatably connected with a distal end of the elongate wire 120 (not shown in FIG. 8A ), such as by a swage fitting. Second section 320 includes a rotatable cap housing 322 that removably couples to the first section 310 , such as by engagement and disengagement with the engagement section 348 of the hemostatic sealing member 340 . The distal end of the elongate wire 120 is connected within a wire bore 332 in a connecting fitting 330 . Connecting fitting 330 is rotatably coupled to the rotatable cap housing 322 , such that rotational movement of the rotatable cap housing 322 does not translate rotational forces to the connecting fitting 330 or to the elongate wire 120 , but rather permits rotational coupling and decoupling of the rotatable cap housing 322 from the first section 310 of the proximal hub 300 and then allows for longitudinal translation of the elongate wire 120 , the rotatable cap housing 322 and the connecting fitting 330 relative to the first section 310 . It will be understood that this longitudinal translation of the elongate wire 120 serves to push the vena cava filter member 110 coupled to the distal end of the elongate wire 120 out of the distal end 119 of the distal catheter sheath member 112 and also to retrieve the vena cava filter member 110 within the distal end 119 of the distal catheter sheath member 112 .
[0063] In accordance with one embodiment of the proximal hub 300 , the first section 310 and the seating recess 350 may optionally be fabricated of pliant or resilient materials. In this embodiment, proximal hub 300 may have resilient or pliant opposing first and second surfaces 315 , 317 , respectively. By fabricating the seating recess 350 of a pliant or resilient material, bore 354 may be dimensioned to bear against the elongate wire 120 and exert a pressure that creates drag when the elongate wire 120 is translated through the bore 354 . Deformation of the seating recess 350 will deform the bore 354 and release some of the pressure bearing against the elongate wire 120 . In use, the medical practitioner may depress first and second surfaces 315 , 317 to deform the first section 310 and the seating recess 350 therein, thereby deforming the bore 354 surrounding the elongate wire 120 passing there through and releasing pressure by the bore 354 bearing against the elongate wire 120 to allow for smoother longitudinal translation of the elongate wire 120 through the proximal hub 300 .
[0064] One embodiment of the filter member 110 is illustrated in its diametrically expanded configuration in FIG. 10 . In this embodiment, filter member 110 consists of a plurality of strut members 12 arranged to form a first generally conical end 18 and a second generally conical end 20 of the filter member 110 . The plurality of strut members 12 define wall surfaces of the filter member 110 and delineate a first space 22 and a second space 24 within the filter member 110 for capturing thrombus sequestered from the circulating blood flow by at least some of the plurality of strut members 12 .
[0065] In addition to forming a first generally conical end 18 and a second generally conical end 20 , optionally, some of the plurality of strut members 12 may be arranged to form an intermediate section 16 of the second generally conical end 20 of the filter member 110 . The intermediate section 16 is characterized by having interstitial openings 19 that are smaller relative to the interstitial openings 15 of the first generally conical end 18 or the interstitial openings 13 of the second generally conical end 20 .
[0066] The first generally conical end 18 may form either the proximal or the distal end of the filter member 110 depending upon the orientation of the filter on the catheter and the anatomical approach for which the rapid exchange vena cava filter catheter 100 is intended, e.g., femoral or jugular. In forming the first generally conical end 18 , a plurality of first strut members 62 , for example three, are coupled at their proximal end to the proximal end 18 of filter member 110 and each extends distally relative to the longitudinal axis of the rapid exchange vena cava catheter 100 . Each of the first strut members 62 is an elongate member that projects away from the central longitudinal axis of the catheter 100 and terminates in a distal end section 63 that defines a base of the first generally conical end 18 . A plurality of second strut members 64 extend from a distal end of the second generally conical end and extend proximally form a distal end ofare coupled at their distal end to the distal end 20 of filter member 110 and each extends proximally relative to the longitudinal axis of the catheter 100 . A plurality of third strut members 66 form the intermediate section 26 , if present, and at least some of the plurality of third strut members 66 are joined at their distal ends to a proximal end of at least some of the plurality of second strut members 64 , and at least some of the plurality of third strut members 66 are joined at their proximal ends a distal end of at least some of the plurality of first strut members 62 . A hoop member 70 , which may be formed from some of the plurality of third strut members 66 , extends circumferentially to define a circumferential axis of the filter member 110 and has a series of continuous undulations defining a series of peaks 75 and valleys 77 about the circumference of filter member 110 . Each of the plurality of first strut members 62 , the plurality of second strut members 64 and the plurality of third strut members 66 are coupled to the hoop member 70 at different points about its circumferential axis and intermediate the proximal end 18 and the distal end 20 of the filter member 110 .
[0067] The plurality of first strut members 62 are preferably evenly offset from each other. For example, where three first strut members 62 are employed, each will be offset by approximately 120 degrees about the circumference of the filter member 110 . The plurality of second strut members 64 are also preferably evenly offset from each other. Thus, for example, if twelve second strut members are employed, each will be offset by approximately thirty degrees about the circumference of the filter member 110 .
[0068] It will be understood that each of the plurality of first strut members 62 , plurality of second strut members 64 , plurality of third strut members 66 and the hoop member 70 are preferably fabricated of biocompatible materials, such as shape memory alloys, superelastic materials or elastic materials, including, without limitation, titanium, vanadium, aluminum, nickel, tantalum, zirconium, chromium, silver, gold, silicon, magnesium, niobium, scandium, platinum, cobalt, palladium, manganese, molybdenum and alloys thereof, such as zirconium-titanium-tantalum alloys, cobalt-chromium-molybdenum alloys, nitinol, and stainless steel.
[0069] FIGS. 10-10B and 11-13 illustrate two alternate attachments of the filter member 410 , 510 to the elongate wire 120 . In each embodiment, the filter member 410 , 510 is attached to a distal end of the elongate wire 210 by means of an attachment tube 40 . A filter attachment member 30 , such as that described in U.S. Pat. No. 8,808,323, which is hereby incorporated by reference, is employed to couple the filter member 410 , 510 to the attachment tube 40 .
[0070] As illustrated in FIGS. 10-10C , attachment tube 40 has a guide wire lumen 27 that extends from a distal end of the attachment tube 40 and passes through the atraumatic tip 122 . Guide wire lumen 27 terminates proximal to the filter attachment member 30 in the guide wire port 118 . A second lumen 29 is provided in the attachment tube 40 that extends and opens to a proximal end of the attachment tube 40 . The distal end of the elongate wire 120 is received within the second lumen 29 and the elongate wire 120 is secured therein. The guide wire port 118 aligns with a port 118 a disposed on the distal catheter sheath 114 when the filter member 110 is in contracted state.
[0071] Like with filter 410 , and as illustrated in FIGS. 11-13 , filter 510 is also coupled to a filter attachment tube 40 . In this embodiment, however, filter attachment tube 40 has a guide wire lumen that passes along an entire longitudinal length of the filter attachment tube 40 and opens distally at the atraumatic tip 122 and proximally at the proximal end of the filter attachment tube 40 . Like with filter 410 , a second lumen 29 is provided in the attachment tube 40 that extends and opens to a proximal end of the attachment tube 40 . The distal end of the elongate wire 120 is received within the second lumen 29 and the elongate wire 120 is secured therein.
[0072] It is contemplated that the elongate wire 120 may be made of any suitably biocompatible metal, such as nickel-titanium alloy, chromium-molybdenum alloy, stainless steel or the like. The elongate wire 120 may optionally be reinforced with a winding of another metal wire or may be coated with a polymer and/or a bioactive agent, such as an antithrombotic agent. It is further contemplated that the proximal and distal catheter sheaths 114 , 112 , may be made of any suitably biocompatible polymer, such as polyurethane, polytetrafluoroethylene, polyether block amide (PEBAX®, Arkema, Paris, France), and may also optionally be coated or covered with another polymer and/or a bioactive agent, such as an antithrombotic agent. It is also contemplated that the vena cava filter member 110 , 410 , 510 may be made of any suitably biocompatible metal or polymer, as are known in the art. Finally, the attachment tube 40 may be made of any suitably biocompatible metal, such as nickel-titanium alloy or polyether block amide (PEBAX®, Arkema, Paris, France).
[0073] It will be understood by those skilled in the art that the foregoing description of the inventive rapid exchange vena cava filter catheter is made with reference to exemplary embodiments only. Such exemplary embodiments are not intended to be, nor should be construed to be limiting of the scope of the invention, which is defined solely by the claims appended hereto.
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A rapid exchange catheter having a vena cava filter and a method for percutaneous delivery of the rapid exchange vena cava filter for use in indicated medical situations in which prophylactic or therapeutic protection against pulmonary embolism are indicated.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a process and apparatus for the preparation of a single crystal of a biopolymer. More particularly, the present invention relates to a process and apparatus for preparing a single crystal of a biopolymer by growth from a solution.
2. Description of the Related Art
The preparation of a single crystal of a biopolymer such as a protein by growth from a solution is an important technique applied in protein engineering or drug design.
To induce crystallization, an aqueous solution of ammonium sulfate, methylpentanediol or polyethylene glycol is added to an aqueous solution of a biopolymer, to be crystallized, the precipitated high polymer is allowed to stand, and the formation of a crystal nucleus and growth of a crystal are effected by the solution growth method. In this connection, various methods for the precipitation of a biopolymer are known [Lecture on Biochemical Experiments, Volume 1-III, pages 6-17 published by Tokyo Kagaku Dojin in 1976].
Nevertheless, since setting of crystallization conditions must be precise, crystallization is conducted under a variety of conditions to determine the optimum conditions, and since a manual operation for finding out optimum conditions is carried out, it is difficult to maintain a good reproducibility. Accordingly, the present inventors previously proposed a method of automatically performing this operation (see Japanese Unexamined patent Publication No. 62-106000). But in this system, where a solution path is changed according to which of many crystallization conditions is used, by a valve, the dead volume of the pipe system is increased and much valuable protein sample is wasted. Accordingly, the above-mentioned system must be improved.
SUMMARY OF THE INVENTION
A primary object of the present invention is to provide a process and apparatus for preparing a single crystal of a biopolymer by growth from a solution, in which the optimum conditions for crystallization of a biopolymer can be easily and efficiently determined by using a small amount of a sample.
More specifically, in accordance with the present invention, there is provided a process for the preparation of a single crystal of a biopolymer by growth from a solution, which comprises continuously changing one factor having an influence on the conditions for crystallization of a solution of a biopolymer, fractionating the solution, and independently crystallizing the resultant fractions.
The present invention further provides an apparatus for the preparation of a single crystal of a biopolymer by growth from a solution, which comprises:
a means for feeding a crystallizing agent solution;
a means for feeding a biopolymer solution;
a means for producing a series of changes of predetermined crystallization conditions, said means continuously changing at least one factor having an influence on the conditions for crystallization of the biopolymer solution; and,
a means for fractionating the solution and independently crystallizing the resultant fractions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram illustrating a first embodiment of the apparatus for carrying out the process of the present invention;
FIGS. 2 and 3 are graphs illustrating the ammonium sulfate concentration gradient and the number of crystals formed in examples of the present invention;
FIG. 4 is a diagram illustrating a second embodiment of the apparatus for carrying out the process of the present invention;
FIG. 5 is a schematic perspective view illustrating a compression tool used in the process of the present invention;
FIG. 6 is a diagram illustrating a tube when compressed by the compression tool;
FIG. 7 is an enlarged view of a part of FIG. 6;
FIG. 8 is a diagram illustrating a crystal-growing apparatus according to another embodiment of the present invention;
FIG. 9 is a diagram illustrating an example of the fabrication of a crystallizing vessel;
FIG. 10 is a diagram illustrating another embodiment of the process for preparing a crystal according to the present invention;
FIG. 11 is a graph illustrating the results obtained by the embodiment shown in FIG. 10;
FIGS. 12A and 12B are diagrams each illustrating an example of the apparatus structure in which the process of the present invention is advantageously carried out; and,
FIG. 13 is a block diagram showing the operations in the apparatus shown in FIGS. 12A and 12B.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is different from the conventional method, in which a solution is independently formed and transferred for each crystallization condition, since according to the process of the present invention, a series of changes of predetermined crystallization condition are continuously produced and the solution is fractionated to form fractions corresponding to independent conditions.
More specifically, for example, the concentration of ammonium sulfate precipitating a protein is gradually changed to form a concentration gradient, drops of the solution are collected one by one, and crystallization is carried out for the respective drops by the vapor diffusion process.
As the factor of the crystallization condition for formation of the concentration gradient, there can be utilized the concentration of a precipitating agent or crystallizing agent such as ammonium sulfate mentioned above, magnesium sulfate, sodium sulfate, sodium phosphate, sodium chloride, cesium chloride, methylpentanediol, methanol or acetone, the protein concentration, the pH value (hydrogen ion concentration), the concentration of a substance, the presence of which increases the regularity of the crystal, for example, an inorganic salt such as sodium sulfate, cesium chloride or aluminum chloride, and the concentration of a substance specifically bonding with a protein, for example, an enzyme reaction inhibitor.
As the fractionating and crystallizing means, there can be mentioned a method in which the solution is charged and sealed in, for example, screw-mouth bottles having a small capacity, and crystallization is carried out batchwise in each respective bottles by standing (FIG. 1), and a method in which drops are received on small glass sheets and crystallization is effected by the vapor diffusion method.
An example of the structure of the apparatus for carrying out the process of the present invention is shown in FIG. 1. In this example, an ammonium sulfate solution 1 (ammonium sulfate concentration=80% of the saturation concentration, 10 mM sodium phosphate buffer, pH=7.0) and an ammonium sulfate solution 2 (ammonium sulfate solution=95% of the saturation concentration, 10 mM sodium sulfate buffer, pH=7.0) are supplied to a concentration gradient-producing system 3 for a usual high-speed liquid chromatography, and a concentration gradient of from 83% saturation concentration to 95% saturation concentration is formed with a total solution amount of 3.34 ml. A separately prepared protein solution 4 (3% sperm whale myoglobin, 50% ammonium sulfate, 10 mM sodium phosphate buffer, pH=7.0) is mixed with the above solution having the concentration gradient at a volume ratio of 1/2. To attain this mixing ratio, the feed rates of two pumps 5 and 6 are adjusted to 0.5 ml/min and 1.0 ml/min, respectively. The formed solution contains 1% of myoglobin in 10 mM sodium phosphate and has a pH value of 7, and a concentration gradient in which the ammonium sulfate concentration linearly changes from 70% to 80% is formed (FIG. 2). The solution is supplied to a fraction collector 7 for the liquid chromatography, and the solution is divided into fractions, each having a volume of 0.5 ml, and charged in microvial bottles having a capacity of 1 ml. The microvial bottles are immediately sealed and stored in a thermostat tank maintained at 20° C., and thus, myoglobin solutions containing ammonium sulfate at concentrations corresponding to 70.5, 71.5, 72.5, 73.5, 74.5, 75.5, 76.5, 77.5, 78.5 and 79.5% of the saturation concentration are obtained. After 1 day, the formation of crystals is initiated and the crystals grow gradually over about 7 days. The number of crystals formed is largest at the concentration corresponding to 75.5% of the saturation concentration (FIG. 3). Namely, this concentration is an optimum concentration condition for the crystallization in the present example.
Another example of the structure of the apparatus for carrying out the process of the present invention is shown in FIG. 4. In this example, a protein solution 8 (3% sperm whale myoglobin, 60% saturation ammonium sulfate, 10 mM sodium phosphate buffer, pH=7.0) and a protein solution 9 (0.75% sperm whale myoglobin, 60% saturation ammonium sulfate, 10 mM sodium phosphate buffer, pH=7.0) are supplied to a gradient-forming device 10 of an acrylic resin (supplied by Sanko Plastics Co.) and a concentration gradient is formed to a total liquid amount of 2 ml. The feed rates of two peristaltic pumps 12 and 13 are adjusted to 0.3 ml/min and 0.6 ml/min, respectively, so that a separately prepared ammonium sulfate solution 11 (80% ammonium sulfate, 1.0 mM sodium phosphate buffer, pH=7.0) is mixed with the above solution having a concentration gradient at a volume ratio of 1/2. The final solution contains 70% of ammonium sulfate in 10 mM sodium phosphate buffer and has a pH value of 7.0, and the myoglobin concentration changes from 0.5% to 2%. The solution is divided into fractions, each having a volume of 0.1 ml, and received on glass sheets 14, and crystallization is effected at 20° C. by the vapor diffusion method. After 3 days, the formation of crystals is initiated, and the crystals grow slowly over about 2 weeks. The number of formed crystals is largest at a myoglobin concentration of 1.5%. Namely, this concentration is an optimum myoglobin concentration for the crystallization in this example.
According to another embodiment of the present invention, as the means for fractionating and crystallizing a solution having a concentration gradient, a method is adopted in which the solution having a concentration gradient prepared in the above-mentioned manner, is guided to a soft hollow tube, the soft hollow tube is compressed at a plurality of predetermined parts to divide the tube into a plurality of small chambers, and each chamber is used as a crystal-growing vessel filled with the solution to be crystallized.
According to still another embodiment of the present invention, a plurality of blocks having a through hole are arranged close to one another to form a hollow pipe cavity defined by the through holes of the blocks, whereby a crystal-growing apparatus is constructed. The solution to be crystallized and having a concentration gradient is filled in the hollow pipe cavity, and the connection of the through holes is sealed so that the through holes are used as independent small chambers. Namely, each small chamber acts as a crystal-growing vessel filled with the solution to be crystallized.
For compression of the soft hollow tube, for example, a compression tool 21 comprising members having the same rectangular sectional shape, as shown in FIGS. 5 and 6, can be used. For example, a soft tube 22 is supported on the compression tool 21 and the tube 22 is divided into a plurality of crystal-growing small chambers by this tool 21. This apparatus is operated in the following manner. One end of the compression tool is fixed, and four ball screws are attached to the other end so that a cantilever structure is not formed. Timing pulleys attached to one ends of the screws are driven by one motor through a timing belt to compress one side of the compression tool against the other side thereof. The terminal point is automatically detected by using a photointerrupter or the like, to stop the supply of power to the motor. A reverse revolution after the supply of power is stopped can be prevented by driving the motor through a gear.
A transparent soft hollow tube is used in the present invention, but if observation of the crystal-forming process over a period of time is not necessary, a semi-transparent or opaque tube can be used. A material having a low water permeability is preferably used as the material of the hollow tube. For example, there are advantageously used a vinyl chloride polymer marketed under the tradename of "Tygon", and fluorine-containing polymers such as a tetra-fluoroethylene/ perfluoroalkyl vinyl ether copolymer (PFA), a tetrafluoroethylene/hexafluoropropylene copolymer (FEP), a tetrafluoroethylene/ethylene copolymer (ETFE), polytrifluorochloroethylene (PCTFE), a trifluorochloroethylene/ethylene copolymer (ECTFE), polyvinyl fluoride (PVF), polyvinylidene fluoride (PVDF), and polytetrafluoroethylene (PTFE).
The sample is introduced into the soft hollow tube of the above-mentioned apparatus from the concentration gradient-preparing apparatus, the soft hollow tube is divided into small chambers, and crystals are grown therein. The crystals are recovered by cutting off one end of the small chambers of the soft tube.
More specifically, a transparent tube having a good elasticity and a low water permeability (composed of Tygon in the present embodiment), as shown in FIG. 5, is arranged downstream of the concentration gradient-preparing apparatus as shown in FIG. 1 or 4. A predetermined amount of the solution is fed from the concentration gradient-preparing apparatus to prepare a predetermined concentration gradient in the tube, the tube is compressed at predetermined intervals to divide the tube into small chambers, and crystals are grown and in each chamber.
A concentration gradient solution comprising 1% of myoglobin and 10 mM sodium phosphate buffer and having an ammonium sulfate concentration gradually changed from 70% to 80% is prepared in the same manner as described above with reference to FIG. 1, and the solution is guided into a Tygon tube having an inner diameter of 3 mm and a length of 8 cm. The tube is gripped by metal sheets having convexities and concavities to divide the tube into 10 small chambers at intervals of 0.8 cm. Solutions having concentrations corresponding to 70.5, 71.5, . . . 79.5% of the saturation concentration are charged in the small chambers, and the growth of the crystals is carried out in a thermostat tank maintained at 20° C. while the tube is gripped thereby.
After one day, the growth of crystals is initiated, and the crystals grow gradually over 7 days. The number of the crystals formed is largest at a concentration corresponding to 75.5% of the saturation concentration. In the present embodiment, this concentration is an optimum concentration for crystallization.
Where the soft hollow tube is formed of a fluorine-containing polymer, a hollow tube having a structure described below is very advantageously used. Namely, PFA, FEP, PVDF, PVF, and PTFE hollow tubes having a wall thickness of 0.2 to 2.0 mm and ETFE, PCTFE, and ECTFE tubes having a wall thickness of 0.2 to 1.0 mm are preferably used.
Where small chambers are formed by using a plurality of blocks, a crystal-growing apparatus shown in FIG. 8 can be used, in which a plurality of blocks 24 having a hole 23 formed at an appropriate position and a plurality of thin sheets 26 having a hole 25 corresponding to the hole 23 are arranged alternately. This crystal-growing apparatus is used, for example, in the following manner. A hole is formed at the central portion of the top end of the thin sheet gripped between the blocks, and a rod for sliding the thin sheet upward is inserted through this hole. Ball screws are arranged on both the ends of the rod. As in the above-mentioned apparatus, timing pulleys are driven by a motor through a timing belt to simultaneously slide the thin sheets 26 upward, whereby the tube hole is divided into small chambers as crystallizing vessels (see FIG. 9).
The material of the blocks may be either an inorganic material such as glass or an organic polymer such as an acrylic polymer, polymethylpentene or polycarbonate.
The thin sheets are preferably composed of a metal such as stainless steel or titanium.
For example, blocks having a thickness of at least 2 mm and this sheets having a thickness of not larger than 200 μm can be used.
When constructing the crystal-growing apparatus of the present embodiment, a through hole is formed in each member comprising a block and a thin sheet and the members are assembled by using bolts and nuts. After crystals have been grown by the predetermined operation, the crystals are recovered, for example, in the following manner. Namely, the apparatus is vertically erected, and the bolts and nuts are removed by using a disjointing tool while all of the blocks are clamped (to prevent leakage of the solution by using such as an O-ring 32 as shown in FIGS. 9 and 10), and then the blocks are removed one by one and the crystals in the respective chambers are recovered in sequence.
For example, a tool comprising methylmethacrylate polymer (Plexiglas) blocks (having a length of 0.8 cm) having a hole having a diameter of 3 mm and stainless steel sheets (having a thickness of 50 μm) having a hole having a diameter of 3 mm, which are gripped between adjacent blocks, is used (see FIG. 8). Where the thin sheets are gripped between the acrylic resin blocks so that the holes of the blocks are in agreement with the holes of the thin sheets, the same concentration gradient solution as described above with reference to FIG. 1 is filled in the tube path, and the stainless steel sheets are slid by 10 cm to divide the tube path into 10 small chambers. In the same manner as described in the foregoing embodiments, crystals are grown for 7 days, and the formed crystals are recovered by disjointing the blocks by using the above-mentioned disjointing tool.
In accordance with still another embodiment of the present invention, small chambers are formed by the means illustrated in FIG. 10. FIG. 10, (A) shows the state of the tool at the step of charging the concentration gradient solution, and (B) shows the state after the division of the concentration gradient solution.
Another example of the concentration gradient solution is now given. Referring to FIG. 1, an aqueous solution of ammonium sulfate having a concentration corresponding to 95% of the saturation concentration as a concentrated solution 1, an aqueous solution of ammonium sulfate having a concentration corresponding to 72.5% of the saturation concentration as a dilute solution 2, and a protein solution 4 formed by dissolving 3% of sperm whale myoglobin in an aqueous solution of ammonium sulfate having a concentration corresponding to 50% of the saturation concentration are charged. Note, 1/15 mole/1 sodium phosphate buffer (pH=7.4) is added in each solution for buffering the pH value.
The mixing device 3 is operated to form a concentration gradient solution having a concentration changed from a 72.5% saturation concentration to a 95% saturation concentration with a total liquid amount of 2 ml. The concentration gradient solution is caused to flow to the right in the drawings by the pump 5, and the protein solution 4 is caused to flow in a volume corresponding to 1/2 of the volume of the concentration gradient solution by the pump 6, both solutions are then mixed and the solution having a concentration gradient is fed out.
The tool 30 shown in FIG. 10 comprises a plurality of transparent block plates 31 formed of a transparent acrylic resin and having a thickness of several mm and a through hole 31a having a diameter of 2 to 3 mm, and in contact with one another. The block plates 31 are moved alternatively, for example, in the direction b (vertical to the surface of the drawing sheet) rectangular to the thickness direction by an operating member (not shown) disposed outside. Packings 32 are provided in circular grooves 31b provided around the through holes 31a at the both sides of the block plates 31, so that a seal is maintained between the opposing surfaces of the adjacent block plates.
A solution-charging port 33 is fixed to one end of the tool 30, and a hole 33a of the port 33 is formed substantially coaxially with the through hole 31a of the block plate 31.
In the state (A) where the through holes 31a of the block plates 31 are communicated with one another, the predetermined concentration gradient solution is charged into the tool 30 from the port 33, and the block plates 31 are alternately moved upward on the drawing sheet by an external mechanism not shown in the drawings to disconnect the communication of the through holes and produce the state (B).
In this divided state, the through holes 31a of the respective block plates 31 are filled with solutions having different compositions, respectively, and the solution are allowed to stand in this state in a thermostat tank maintained at about 20° C. The formation of crystal nuclei and growth of the crystals is observed from the outside.
Even if the block plates 31 are formed of a transparent glass, polymethylpentene resin or polycarbonate resin instead of the acrylic resin used in the present embodiment, similar effects can be attained, as has been experimentally confirmed.
FIG. 11 illustrates the relationship between the concentration of the concentration gradient solution and the size of crystals in each small chamber, as observed in the above-mentioned embodiment. The ammonium sulfate concentration (%) is plotted on the left ordinate Y1 and the average value (mm) of the long sides of crystals is plotted on the right ordinate Y2, and the small chamber number is shown on the abscissa X.
In the present invention, the portion in which the crystals are largest, i.e., the average value of the long sides of crystals is about 0.8 mm, is present in the vicinity of the small chamber No. 11, and the point p indicating an aqueous solution of ammonium sulfate having a concentration corresponding to 74% of the saturation concentration corresponds substantially to this portion.
FIGS. 12A and 12B each illustrates still another embodiment of the structure of the apparatus for advantageously carrying out the process of the present invention. Referring to FIGS. 12A and 12B, a crystallizing agent solution 42 is contained in a liquid feed portion 41, and a crystallizing agent solution 44 having different factor of the crystallizing agent solution 42 is contained in a concentration gradient-forming portion 43. The crystallizing agent solution may be fed in the concentration gradient-forming portion 43 previously by a means similar to the liquid feed portion 41 mechanism. The solution 42 is fed at a constant rate from the liquid feed portion 41, whereby a predetermined concentration gradient is formed by stirring the crystallizing agent solution fed into the concentration gradient-forming portion 43 and the crystallizing agent solution 44, and simultaneously, the concentration gradient solution is fed out in sequence. A sample solution 46 is fed from a liquid feed portion 45 at a constant rate. These solutions are mixed by the stirring portion 61 to form a crystallizing agent-containing sample solution having a certain concentration gradient. The concentration gradient solution is then introduced to a crystallizing portion 47, and a compression tool 48 is driven by a tube-pressing driving portion 49 to form a plurality of sample solution-containing small chambers. Note, reference numeral 50 represents a drain vessel and reference numeral 60 represents valves. FIG. 13 is a block diagram showing the operations in the apparatus shown in FIG. 12. In FIG. 13, 51 represents a control portion, 52 represents a temperature-controlling portion, 53 represents a solution reserve and feed portion, 54 represents a concentration gradient-forming portion, 55 represents a solution reserve and feed portion, 56 represents a crystallizing portion and 57 represents a tube-pressing driving portion. The arrow from the portion 51 indicates the stream of a command for causing a coordinated action of the respective portions. It is important that the portions 53, 54, 55, 56 and 57 act correlatively. The arrows from 52 indicate the streams of commands for appropriately controlling the temperatures of the respective portions. The arrows from the portion 53 to the portion 54 (or 55), 54 to 55, and 55 to 56 indicate the streams of the solution. The arrow from the portion 57 to the portion 56 indicates the driving force for compressing the tube.
The process and apparatus of the present invention can be applied not only for terrestrial experiments but also for cosmical experiments.
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A process for the preparation of a single crystal of a biopolymer by growth from a solution, which comprises continuously changing one factor having an influence on the conditions for crystallization of a solution of a biopolymer, fractionating the solution, and independently crystallizing the resultant fractions. The process may be carried out by an apparatus comprising a means for feeding a crystallizing agent solution, a means for feeding a bioploymer solution, a means for producing a series of changes of predetermined crystallization conditions, said means continuously changing at least one factor having an influence on the conditions for crystallization of the biopolymer solution, and a means for fractionating the solution and independently crystallizing the resultant fractions.
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This is a division, of application Ser. No. 451,776, filed Mar. 18, 1974 now U.S. Pat. No. 3,910,627.
BACKGROUND OF THE INVENTION
This invention relates to vehicle visor assemblies.
Sun visors of the type generally installed in motor vehicles above windshields commonly have an annoying trait: they often fail to hold the selected position of adjustment to which they are swung for effectively blocking sun rays or the head beams of oncoming vehicles. Moreover, they may, after some usage, fail to stay in their normal out-of-the-way inoperative position and hence tend to obstruct vision or otherwise become a nuisance.
Visors have commonly comprised a flat portion or blade contoured to provide a movable mask, and a hinge portion extending along a longitudinal edge of the flat portion. One end of the hinge portion has ordinarily been formed to receive a pivotal carrier rod, and the other end adapted to be secured in latching position in front of and/or to one side of a vehicle occupant. Frequent and often sudden shifting of the blade, both angularly about the pivot axis at one end of the rod and about the longitudinal axis of the rod itself to meet changing circumstances tends to render the frictional operative holding relation of the carrying rod and the blade inconstant and unreliable.
A further disadvantage in vehicle visors is that, although their blade portions, often of laminar wood or cardboard, may be covered as by a flocculent or fabric, they are apt to be harmful in the event of vehicle accident since they may well be impacted by the heads of passengers and are inadequately yieldable to cushion a blow.
SUMMARY OF THE INVENTION
In view of the foregoing it is an object of this invention to provide an improved visor assembly mountable on a carrier rod and capable of frictionally retaining any adjusted position of angularity.
Another object of the invention is to provide an adjustable vehicle visor assembly, the molded blade of which is shaped to facilitate at least partial yielding or collapse in the event of an impact therewith, but which otherwise exhibits adequate resistance to deformation during manual operation thereof to overcome restraint maintaining the blade in a selected position.
To these ends, and as herein illustrated, a visor assembly comprises an integral, molded plastic body, including a substantially rigid hinge portion extending along one side thereof, one end of the hinge portion being axially tubular, and a sheet metal clip extending in the tubular hinge portion and having laterally projecting means engageable with the wall of said hinge portion to prevent relative rotation of the clip, the clip including axially spaced arcuate bearing bands, and a mounting rod arranged to be received in frictional engagement with the inner walls of the bands. Preferably, as shown herein the visor includes a planar blade portion extending along one side of the hinge portion, the blade portion being generally of parallelogram configuration and having an open or skeletal web-like frame structure consisting of angularly interconnecting members and an outer margin, the cross sections of which are concavo-convex. These molded lightweight members thus are individually bendable lengthwise but transversely rigid, and hence provide a unitary visor blade capable of buckling upon accidental impact.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other features of the invention will now be more particularly described in connection with an illustrative embodiment and with reference to the accompanying drawings thereof, in which:
FIG. 1 is a view in side elevation of a sun visor assembly, its upper or hinge portion being horizontal and its blade portion being suspended therefrom and having its cover partly broken away to reveal its novel frame;
FIG. 2 is a perspective of the assembly shown in FIG. 1, without its cover, full lines now illustrating partial deformation resulting from an accidental impact;
FIG. 3 is an enlarged exploded perspective of a mounting end of the visor, configuration of a relaxed friction clip and FIG. 3a is a typical cross section of a blade member being shown;
FIG. 4 is an end view showing a mounting rod received in the installed friction clip, and
FIG. 5 is an enlarged axial section showing mounting of the clip and rod.
DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 shows a visor blade and clip assembly generally designated 10. It comprises a unitary frame 11 of plastic molded to provide a desired, for instance parallelogram, configuration. Along the longer, upper side of the assembly there extends a rigid hinge portion 12 (FIGS. 1-4) having at its tapering larger end an axial bore 14, preferably formed with opposed axial slots 16,16 (FIGS. 2,3) for a purpose later mentioned. The bore 14 is sized to receive and rotationally anchor a friction clip 18 (FIGS. 3-5) to be more fully described. The other end of the hinge portion 12 may be formed with a reduced socket 20 for releasably and pivotally securing the visor in a latch (not shown) mounted, for instance, above the windshield of a vehicle.
The clip 18 is preferably formed from a sheet metal blank of roughly about 0.020 inch gauge. Opposite margins 22,22 of the blank remain generally in a plane and are to be thrust axially into the slots 16,16 respectively. Tangs 24 (FIGS. 3-5) stuck from the margins 22 are provided to resist retraction of the clip from the bore 14. The margins 22 and end tabs 26,26 fitted in an end of the hinge portion thus prevent relative rotation of the clip in the visor when the latter is turned about its hinge axis, i.e. the axis of a cylindrical carrier or mounting rod 28 (FIGS. 3 and 5). This rod 28 has a leading end which may be beveled to be telescoped in the clip 18 as will be explained and an opposite end (not shown) is secured to a universal joint or other suitable means permitting the rod to be swung in such direction as it is desirable manually to orient the rod and the visor.
For enabling a planar blade portion 30 of the visor frame 11, which may be covered with fabric, plastic or other suitable soft material 32, to be swung about the axis of the carrier rod 28 and then held in any selected position, the clip 18 includes arcuate, substantially semi-elliptoidal bearing bands 34,36 (when relaxed as in FIG. 3) pressed from opposite sides of the original blank. These bands preferably are axially spaced uniformly and alternately project from opposite sides. Inner opposed minor radii of these relaxed bands 34,36 are slightly less than the radius of corresponding portions of the rod 28 and predetermined to provide tension when distended on the circumference of the rod 28. Their frictional gripping engagement therewith, in sum, consistently enables the visor portion to be angularly held as intended. Whereas prior designs have in time, through parts loosening or vibrations and the like, allowed a visor blade to fail to keep some angular settings and even to never retain other selected angular positions, the tensioning of the distended bands 34,36 engaging the rod 28 provides holding friction which is adequate and substantially uniform at all desired angular settings of the visor. Obviously fewer or more bands 34,36 may be employed as desired.
The planar blade portion 30 of the frame 11 desirably comprises, within the cover 32, a skeletal web-like structure of an outer margin 40 and interconnecting members 42. These are uniformly thin and lightweight, the member 42 intersecting near or substantially at the hinge portion 12 and at the opposite margin 40 of the parallelogram. As indicated at 44,46 (FIGS. 1,2) a "corner" portion may be cut away, in effect, to permit requisite clearance for a mirror or the like. Preferably for reinforcing purposes one of the members 42 terminates at a corner of the parallelogram. More particularly two or more of the members 42 are parallel and intersect at their junctions with the longer sides of the parallelogram at similar acute angles. To provide appropriate strength for rendering the visor repeatedly maneuverable and yet permit it to buckle on impact, each of the members 42 and the margin 40 has a shallow concavo-convex cross section as shown in FIG. 3; generally similar longitudinal shaped sections, though somewhat longer, are formed at the intersections of the members 40,42 and 12,42.
It will be appreciated from the foregoing that the invention provides a visor blade and clip assembly of simple structure which is relatively economical to manufacture. The clip 18 and unitary molded frame 11 when assembled are turned as one about the axis of the carrying rod 28 to position the visor blade portion 30 as desired. Frictional gripping of the distended bands 34,36 with the circumference of the rod 28 assures that all adjusted angular positions of the visor blade will be held. Moreover, yieldability in the concavo-convex shape of the visor blade web members 42 and of the margin 40 assures that accidental impact of the head for instance, of an occupant of the vehicle will collapse the visor at least partly and thereby assist in reducing and possibly avoiding serious injury.
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A visor blade of molded, collapsible truss formation is provided which features both safety and reliable position-holding capability. The latter is attained by a clip blanked from sheet metal and of a configuration to be anchored in a hinge portion of the visor, and tensionally grip a mounting rod to uniformly resist turning of the visor from any selected angular position about the rod.
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[0001] The instant application is a continuation-in-part of co-pending U.S. patent application Ser. No. 10/194,251, filed Jul. 15, 2002.
BACKGROUND OF THE INVENTION
[0002] The invention relates to compositions for rapid bowel cleansing which are particularly useful for preparing the bowel prior to surgery or diagnostic procedures such as colonoscopies.
[0003] 1. Field of the Invention
[0004] Gastrointestinal agents for regulating bowel movement can conveniently be placed into two categories: laxatives and bowel cleansers. Laxatives are formulated for long-term use, with the intention of eliminating constipation and obtaining a regular bowel function. Many laxatives work by stimulating bowel motility (peristalsis) in various ways, as by distending the gut with bulking or osmotic agents, or by directly stimulating the bowel nerves or muscles with stimulant laxatives. Other laxatives function as stool softeners or lubricants. The various types of laxatives are often combined in attempts to maximize efficacy or to reduce side effects of the agents.
[0005] Bowel cleansers, also called purgatives, cathartics, and lavages, are formulated for rapid emptying of the bowel and are intended for short-term use only. They are commonly used as “bowel preps” for emptying the bowel prior to surgery, childbirth, or diagnostic procedures, and usually comprise an osmotic or stimulant laxative administered by either oral or anal route. While purgatives formulated for patient use as enemas are often prescribed before examinations, they are awkward to handle and are frequently not properly administered, so orally-administered preparations are generally preferred. However, the orally-administered compositions for rapid bowel cleansing in common use also have disadvantages which discourage patient compliance.
[0006] 2. Description of Related Art
[0007] The most commonly prescribed oral bowel preps today for bowel examination comprise sodium phosphate compositions in varying proportions of mono- and dibasic species, and polyethylene glycol (PEG) in combination with electrolytes.
[0008] Sodium phosphate is a saline osmotic laxative, sold, for example, as Fleet Phospho-Soda® (C.B. Fleet Co., Lynchburg, Va.), which contains both monobasic and dibasic uncoated sodium phosphate powders. It is also sold as Visicol™, which comprises mono- and dibasic sodium phosphates in tablet form. This laxative, when formulated and used as a bowel cleanser, is associated with nausea, vomiting, and symptoms of electrolyte imbalance; the product also has an unpleasant taste. As a result, patient compliance is difficult to obtain, particularly when the cleanser is supplemented with, for example, another saline agent such as a magnesium salt, or a bowel stimulant such as bisacodyl.
[0009] While PEG is known for its successful use as a long-term osmotic laxative in combination with dietary fiber (as described in U.S. Pat. No. 5,710,183, issued Jan. 20, 1998 to Halow, and incorporated herein by reference), PEG purgatives such as Colyte® (Braintree Laboratories, Braintree, Mass.) have poor patient compliance. They have an unpleasant taste, and the amount and frequency of fluid the patent is required to drink, typically 8 fluid ounces every ten minutes over several hours, frequently cause severe bloating and attendant nausea. Further, although these purgatives normally include electrolytes to counterbalance electrolyte loss during treatment, symptoms of electrolyte imbalance are, notwithstanding, often experienced by the patient.
SUMMARY OF THE DISCLOSURE
[0010] The inventions accordingly provide dry bowel cleansing compositions for oral administration comprising polyethylene glycol; dibasic sodium phosphate; and, optionally, monobasic sodium phosphate; which are dissolved in an aqueous carrier prior to use. For added potency in certain clinical applications a bowel stimulant such as biscodyl, or other agent known for its laxative properties may be taken in conjunction with the administration of these compositions as appropriate.
[0011] The inventions further provide methods for the short-term use of the compositions as cathartics in emergency situations or in severe constipation, or as bowel preparations prior to surgery, bowel examinations, childbirth, or similar occasions.
[0012] The compositions demonstrate significantly improved patient compliance and very good efficacy.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] [0013]FIGS. 1-6 are video photographs taken during colonoscopy of six different patients, illustrating clean-out of various sections of their colons using a bowel prep according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0014] Polyethylene glycols useful in the composition of the invention broadly comprise any food-grade or pharmaceutical-grade PEG. Currently preferred for convenience of use in preparing and using the composition of the invention are polymers having molecular weights above about 900 which are solid at room temperature and soluble in or miscible with water. Polymers having average molecular weights between about 3000 and 8000 are exemplary; PEG 4000, which is nearly odorless and tasteless and widely available in USP grade, or PEG 3350, are very suitable. A proprietary laxative, MiraLax® (Braintree Laboratories, supra), is a useful source of PEG 3350 powder readily soluble in water. Other suitable PEG powders are commercially available, as from the Spectrum Chemical Mfg. Company, Gardena, Calif. Non-powdered PEG should be comminuted to a particle size that is readily soluble in water before use.
[0015] The sodium phosphate powder according to the invention comprises a pharmaceutical-grade (USP) free flowing powder of anhydrous dibasic sodium phosphate (Na 2 HPO 4 , disodium phosphate), optionally in combination with monobasic sodium phosphate monohydrate (NaH 2 PO 4 .H 2 O, monosodium phosphate), or anhydrous, such as conventionally used in saline laxatives, for example, the powders described in the Fleet Phospho-Soda® composition discussed supra. The phosphate powder provides the compositions of the invention with a saline osmotic effect which complements the effect of the PEG component and is used in amounts which provide the desired osmolarity for this purpose, as known in the art.
[0016] To administer, the phosphate and PEG powders are simply dissolved by mixing into any desired aqueous carrier, such as water or juice.
[0017] PEG and phosphate powder are combined in amounts which provide a composition that will preferably evacuate the bowel in the course of a few (3-4) hours. Compositions ranging from at least about 50% to about 90% by weight PEG and from at least about 10% to about 50% by weight phosphate, based on the combined weight of the phosphate and PEG in the composition, are provided. Typically, a dry prep composition according to the invention will contain about 60 to 80% by weight PEG and 20 to 40% by weight of phosphate; the term “phosphate” herein refers to either disodium phosphate alone, or disodium phosphate in combination with monosodium phosphate. In typical embodiments, the amount of PEG in a composition according to the invention will be about 70 to 80% by weight, and 20 to 30% by weight sodium phosphate, based on the total amount of PEG and phosphate; the combined PEG and phosphate should make up no less than about 80% by weight of a composition containing additives for optimum results. Compositions containing about 75 to 80% by weight PEG and 20 to 25% by weight phosphate are particularly contemplated for most applications. However, under some circumstances it may be desirable to use amounts of PEG at the high end of the range (e.g., from above about 80% to about 90% by weight) with a concomitant decrease of phosphate to below about 20% by weight to about 10% by weight, for example to obtain a more rapid bowel cleanout. Conversely, under some circumstances, amounts of phosphate at the high end of the range (e.g., from above about 40% to about 50% by weight) with a decrease in PEG to below about 60% to about 50% by weight may be desirable. Generally, at least a major amount (greater than about 50% by weight) of the phosphate present is disodium phosphate; if monosodium phosphate is included in the composition, it should usually make up less than one-half, and preferably less than one-quarter, of the phosphate content of the composition.
[0018] To formulate a convenient single dosage drink, a dry prep composition containing from about 45 to 130 g PEG and from about 5 to about 45 g phosphate powder, typically from about 45 to 70 grams powdered PEG and 10 to 30 grams phosphate powder, preferably about 55 to 65 grams PEG and 15 to 25 grams phosphate powder, is dissolved or suspended in an aqueous liquid of choice, such as water, tea, or juice. The phosphate powders should be readily soluble in the aqueous drink medium to promote optimum palatability and patient compliance. Reduced-solubility powders such as powders coated with insoluble materials are not recommended. Suitable powders for use in the practice of the present invention comprise the water-soluble free-flowing untreated powders described and exemplified supra as mono- and di-sodium phosphate powders commonly used in this art. In an exemplary drink formulation, a single dose dry prep composition containing from about 58 to 63 grams PEG and from about 15 to 20 grams phosphate powder, for example, 60 grams powdered PEG and 18 grams sodium phosphate powder, preferably disodium phosphate powder, is dissolved in about 1 to 1.5 quarts of water or other aqueous liquid, for oral ingestion. Alternately, the compositions can be dissolved in a smaller portion of water, such as eight fluid ounces, and the remainder of the liquid taken in conjunction with this solution. The amount of water or other aqueous medium in which the dry prep composition is dissolved or which is taken with the dry prep composition is not critical; however, for optimum bowel cleansing, at least about a pint should be used, and preferably at least a quart, depending upon the patient's total liquid intake during the treatment.
[0019] In another embodiment of the invention, lower molecular weight PEG polymers such as PEG 400 which are liquid at room temperature may be used in lieu of the above powdered PEG polymers in the same proportions by weight, and the phosphate powder dissolved therein; if desired, the solution may then be diluted to taste with an aqueous liquid. Also, a solution of the phosphate powder may be combined with the liquid PEG instead of the powder, per se.
[0020] The single dosage drinks so prepared are taken from twice per day to four times per day on the day preceding the colonoscopy or other procedure, depending upon the degree of clean-out required and the presence of complicating bowel conditions such as constipation. Typically, in an average patient, twice per day for one day will provide the desired result. If, for example, the patient has failed a standard prep, a two day prep is recommended. Preferably, the patient is restricted to a clear liquid diet while on the regimen, i.e., a diet of liquids containing no significant solid material. Suitable clear liquids include apple juice, tea, plain Jello®, 7-Up®, Sprite®, and chicken or beef broth. If the patient receives a sufficient amount of liquids containing sodium and potassium ions to satisfy hunger, no supplemental electrolytes need be used with the PEG/phosphate compositions.
[0021] For added potency in certain clinical applications, the compositions may be taken in conjunction with a bowel stimulant such as bisacodyl, generally available over-the-counter as Dulcolax®, BiscoLax®, or other proprietary product. For use with the present invention, bisacodyl should not be taken in powder form to avoid neutralization with stomach acids. Enterin-coated 10 milligram tablets once or twice a day are suitable.
[0022] The compositions may include, or be taken in conjunction with, conventional additives such as flavoring or coloring agents. While not presently recommended, an herbal bowel stimulant such as Cascara sagrada may also be included in or taken in conjunction with the inventive compositions. Additionally, psyllium or other fiber commonly used as a stool-bulking agent may be optionally added to or taken with the compositions, both for its laxative properties and its potential ability to counteract any adverse effects of the other components. Kits containing single dosage units with optional adjuvants such as flavor packets, dietary powders such as powdered bouillon, or herbal preparations are also provided.
EXAMPLES
[0023] Methods and Materials:
[0024] Patients were prepared for colonoscopy with a dry prep composition of 60 grams PEG powder and 18 grams disodium phosphate powder per dose.
[0025] Each patent was given two single-dose packets for self-administration on the day preceding the colonscopy, with instructions to dissolve each dose in water and drink the first dose at 10 a.m. and the second at 4 p.m. For each patient, a clear liquid diet was prescribed for that day. A flavor packet containing powdered Crystal Light® Ice Tea was provided for use as desired with the prep to encourage drinking.
[0026] Results:
[0027] The results reported here are representative of those obtained in the experimental group.
[0028] Patient #1:
[0029] This is a 61 year-old female with weight loss and decrease in appetite. She underwent a clear liquid diet the day before with bowel prep taken at 10 a.m. and at 4 p.m. Good prep and adequate view of the colon was verified by multiple photographs during colonoscopy. She had no complaints of cramping or complaints of nausea. Mild dislike of taste. View of transverse colon, FIG. 1.
[0030] Patient #2:
[0031] This is an 86 year-old female with a history of anemia who underwent bowel prep, taking it twice the day before examination with a clear liquid diet. There was adequate clean out and a good view of the entire colon with no abnormalities found in the colon.
[0032] View of sigmoid colon, FIG. 2.
[0033] Patient #3:
[0034] This is a 62 year-old male with hemorrhoidal bleed and diarrhea undergoing colonoscopy. Bowel prep at 10 a.m. and 4 p.m. and a clear liquid diet were prescribed. He had no complaints of nausea, vomiting, or discomfort. No complaints of taste abnormalities. He was given flavor packet to use as needed.
[0035] View of transverse colon, FIG. 3.
[0036] Patient #4:
[0037] This is a 74 year-old male with a history of colon polyps for surveillance colonoscopy, underwent bowel prep and clean out the day before using the dry prop at 10 a.m. and 4 p.m. with one Dulcolax 10 milligram tablet. Adequate clean out showing diverticulosis at the sigmoid colon. Mild rectal irritation and inflammation with a good view of the entire colon verified by video photographs taken during colonscopy. Tolerance of the prep and slight complaint about taste, but no crampy sensation. No nausea and vomiting that he has had with other preps.
[0038] View of descending colon, FIG. 4.
[0039] Patient #5:
[0040] This is a 50 year-old female with a first degree relative with colon cancer who underwent surveillance colonoscopy. Took the bowel prep at 10 a.m. and 4 p.m.; some stool found in the sigmoid colon. There was no liquid, able to suction out completely and got a good visualization of the entire colon verified by video photographs during he colonoscopy with the patient having no complaints of product tolerance. No nausea and no vomiting with diarrhea, and no crampy sensation.
[0041] View of transverse colon, FIG. 5.
[0042] Patient #6:
[0043] This is a 50 year-old female who presented with diarrhea for colonscopy. The bowel prep was taken at 10 a.m. and 4 p.m. on the day before the exam, with a clear liquid diet. The bowel prep was good, with adequate view of colon. No complaints.
[0044] View of transverse colon, FIG. 6.
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The invention provides compositions for rapid bowel cleansing comprising a water-soluble mixture of polyethylene glycol and sodium phosphate(s). The compositions are particularly useful for preparing the bowel prior to surgery or diagnostic procedures such as colonoscopies. The invention further comprises methods for cleansing the bowel using these compositions, and bowel cleansing kits comprising these compositions.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Cross-reference and incorporation by reference is made to U.S. application No. 09/973,351, filed Oct. 9, 2001 by Robert C. U. Yu and John A. Bergfjord, Sr., entitled STRESS RELEASE METHOD (Attorney Docket No. D/A1414).
FIELD OF THE INVENTION
[0002] The invention relates to treatment methods for web stock. In particular, the invention relates to stress relief treatment methods for laminate web stock.
BACKGROUND AND SUMMARY
[0003] Flexible electrostatographic imaging members are well known in the electrostatographic marking art. Typical flexible electrostatographic imaging members include, for example, (1) electrophotographic imaging members (photoreceptors) commonly utilized in electrophotographic (xerographic) processing systems and (2) clectroreceptors, such as ionographic imaging members for electrographic imaging systems. The flexible electrostatographic imaging members can be in the form of seamless or seamed belts. Typical electrophotographic imaging member belts comprise a charge transport layer and a charge generating layer on one side of a supporting substrate layer and an anticurl back coating applied to the opposite side of the supporting substrate layer to induce flatness. Electrographic imaging member belts, however, typically have a more simple material structure, including a dielectric imaging layer on one side of a supporting substrate and an anticurl back coating on the opposite side of the substrate. While the scope of embodiments covers an improved preparation process for flexible electrostatographic imaging members producing a crack resistance enhanced outer top imaging layer, the following discussion will focus only on processing of flexible electrophotographic imaging members for simplicity.
[0004] Electrophotographic flexible imaging members typically comprise a photoconductive layer, which can include a single layer or composite layers. Since typical electrophotographic imaging members can exhibit undesirable upward imaging member curling, the anticurl back coating brings each imaging member to at least a desired flatness.
[0005] One type of composite photoconductive layer used in electrophotography, illustrated in U.S. Pat. No. 4,265,990, for example, the disclosure of which is hereby incorporated by reference, has at least two electrically operative layers. One layer comprises a photoconductive layer that can photogenerate holes and inject the holes into a contiguous charge transport layer. Generally, where the two electrically operative layers are supported on a conductive layer with the photoconductive layer sandwiched between the contiguous charge transport layer and the conductive layer, the outer surface of the charge transport layer is normally charged with a uniform charge of a negative polarity and the supporting electrode is utilized as an anode. The supporting electrode can still function as an anode when the charge transport layer is sandwiched between the supporting electrode and the photoconductive layer. The charge transport layer in this case must be able to support the injection of photogenerated electrons from the photoconductive layer and to transport the electrons through the charge transport layer. Photosensitive members having at least two electrically operative layers can provide excellent electrostatic latent images when charged with a uniform negative electrostatic charge, exposed to a light image and thereafter developed with finely divided electroscopic marking particles. The resulting toner image is usually transferred to a suitable receiving member, such as paper.
[0006] As more advanced, higher speed electrophotographic copiers, duplicators and printers were developed, degradation of image quality was encountered during extended cycling. Moreover, complex, highly sophisticated duplicating and printing systems operating at very high speeds have created stringent requirements including narrow operating limits on photoreceptors. For flexible electrophotographic imaging members having a belt configuration, the numerous layers found in modern photoconductive imaging members must be highly flexible, adhere well to adjacent layers, and exhibit predictable electrical characteristics within narrow operating limits to provide excellent toner images over many thousands of cycles. One type of multilayered photoreceptor belt that has been employed as a belt in negatively charging electrophotographic imaging systems comprises a substrate, a conductive layer, a blocking layer, an adhesive layer, a charge generating layer, a charge transport layer, and a conductive ground strip layer adjacent to one edge of the imaging layers. This photoreceptor belt can also comprise additional layers, such as an anticurl back coating to balance curl and provide the desired belt flatness.
[0007] In a machine service environment, a flexible multilayered photoreceptor belt, mounted on a belt supporting module that includes a number of support rollers, is generally exposed to repetitive electrophotographic image cycling, which subjects the outer-most charge transport layer to mechanical fatigue as the imaging member belt bends and flexes over the belt drive roller and all other belt module support rollers. The outer-most layer also experiences bending strain as the backside of the belt makes sliding and/or bending contact above each backer bar's curving surface. This repetitive action of belt cycling leads to a gradual deterioration in the physical/mechanical integrity of the exposed outer charge transport layer, leading to premature onset of fatigue charge transport layer cracking. The cracks developed in the charge transport layer as a result of dynamic belt fatiguing are found to manifest themselves into copy print defects, which thereby adversely affect the image quality on the receiving paper. In essence, the appearance of charge transport cracking cuts short the imaging member belt's intended functional life.
[0008] When a production web stock consisting of several thousand feet of coated multilayered photoreceptor is obtained after finishing the charge transport layer coating/drying process, it is seen to spontaneously curl upwardly. Hence, the anticurl back coating is applied to the backside of the substrate support, opposite to the side having the charge transport layer, to counteract the curl and render the photoreceptor web stock flatness. The exhibition of upward photoreceptor curling after completion of charge transport layer coating results from thermal contraction mismatch between the applied charge transport layer and the substrate support under the conditions of elevated temperature heating/drying the wet coating and eventual cooling down to room ambient temperature. Since the charge transport layer in a typical photoreceptor device has a coefficient of thermal contraction approximately 2 to 5 times larger than that of the substrate support, upon cooling down to room ambient, greater dimensional contraction occurs in the charge transport layer than in the substrate support. This yields the upward photoreceptor curling of the web stock.
[0009] Although, in a typical photoreceptor belt, it is necessary to apply an anticurl back coating to complete a typical photoreceptor web stock material package having the desired flatness, nonetheless the application of the anticurl back coating onto the backside of the substrate support (for counter-acting the upward curling and render photoreceptor web stock flatness) has caused the charge transport layer to instantaneously build-in an internal tension strain of from about 0.15% to about 0.35% in its coating material matrix. After converting the production web stock into seamed photoreceptor belts, the internal built-in strain in the charge transport layer is then cumulatively added to each photoreceptor bending induced strain as the belt flexes over a variety of belt module support rollers during photoreceptor belt dynamic cyclic function in a machine. The consequence of this cumulative strain effect has been found to cause the acceleration and early onset of photoreceptor belt fatigue charge transport layer cracking problem. Moreover, the cumulative charge transport layer strain has also been identified as the origin of the formation of bands of charge transport layer cracking when the photoreceptor belt is parked over the belt support module during periods of machine idling or overnight and weekend shut-off time, as the belt is under constant airborne chemical vapor and contaminants exposure. The bands of charge transport layer cracking are formed at the sites corresponding to photoreceptor belt bending over each of the belt supporting rollers. The crack intensity is also seen to be most pronounced for the band at the belt segment bent and parked directly over the smallest roller, since according to the fundamentals of material mechanics, the smaller the roller diameter the belt segment is bent over, the greater is the bending strain induced in the charge transport layer surface.
[0010] Thus, there is a need for a method of fabrication of improved flexible seamed photoreceptor belts, having a charge transport layer with little or no built-in internal tension and reduced bending strain as the belts flex during machine function or during static bent belt parking over the belt module support rollers under the periods of machine idling and shut-off. Such belts will enjoy extended mechanical functioning life and effect the suppression of premature onset of charge transport layer cracking problem as well.
[0011] U.S. application No. 09/973,351, filed Oct. 8, 2001, entitled STRESS RELEASE METHOD (D/A1414), and U.S. Pat. Nos. 5,606,396, 5,089,369, 5,167,987, and 4,983,481, the disclosures of which are hereby incorporated by reference, represent prior efforts toward alleviating the problems discussed above. These efforts yielded were successful to a point. However, resolution of one problem had often been found to create new ones. For example, charge transport layer cracking life extension through selection of a supporting substrate.
[0012] Thus, there is a continued need to improve the methodology for cost effectual production of flexible imaging members, particularly through innovative processing treatment approaches that effect charge transport layer internal tension strain reduction or elimination, as well as reduction the bending/flexing strain over belt module support rollers, in multilayered electrophotographic imaging member web stocks to yield mechanically robust imaging member belts.
[0013] Embodiments thus provide improved methodology for fabricating multiple layered electrophotographic imaging member web stocks that overcome the above noted deficiencies. For example, embodiments provide an improved process for carrying out flexible electrophotographic imaging member web stocks treatment. Additionally, embodiments provide an improved and refined methodology for processing flexible multilayered electrophotographic imaging member web stocks to effect reduction of charge transport layer internal strain. Advantageously, embodiments provide an improved and refined methodology for processing flexible multilayered electrophotographic imaging member web stocks to effect reduction of charge transport layer bending strain that is induced when imaging member belt flexes or parking over belt support rollers to thereby extend the mechanical service life of the imaging member.
[0014] An improved flexible multilayered electrophotographic imaging member web stock results from embodiments. Such web stock has a charge transport layer with reduction of both internal and bending strains for effectual suppression of early onset of imaging member belt charge transport layer cracking problem caused by dynamic belt fatigue during machine belt function or induced as a result of chemical contaminants exposure at the period belt parking when machine idling or shut-off.
[0015] Embodiments thus provide an improved treatment process for carrying out multilayered flexible electrophotographic imaging member web stock charge transport layer internal stress reduction that effects the elimination of the need of an anticurl back coating from the imaging member. Additionally, embodiments provide an improved flexible multilayered electrophotographic imaging member web stock having a strain/stress reduction charge transport layer through implementation of invention cost effective web stock stress-releasing treatment production process. A typical web stock comprises a flexible substrate support layer coated over with an electrically conductive ground plane, a hole blocking layer, an optional adhesive layer, a charge generating layer, a charge transport layer, and an anticurl back coating.
[0016] A stress-release process has improved and refined features for effectual heat treatment of electrophotographic imaging member web stock to substantially eliminate the internal tension strain from the charge transport layer material matrix, as well as to reduce bending strain prior to fabrication into flexible imaging member belts. To achieve this, embodiments direct the imaging member web stock is directed, with the transport layer facing outwardly, toward the surface of a circular metallic tube making entering contact at 12 o'clock with the tube, heating the transport layer surface to a temperature above its glass transition temperature (T g ), then cooling the web stock to a temperature below the Tg just before the web stock leaves the tube to complete imaging member web stock stress release processing treatment. Embodiments are equally applicable for fabricating electrographic imaging members as well (e.g., ionographic members).
[0017] The stress release treated flexible electrophotographic imaging member web stock is then formed into seamed flexible belts that generally comprise a flexible supporting substrate having an electrically conductive surface layer, an optional hole blocking layer, an optional adhesive layer, a charge generating layer, a charge transport layer, a ground strip layer, and may or may not need an anticurl back coating. The flexible substrate support layer should be transparent, and can have a thickness of between about 25 μm and about 200 μm. A thickness in the range of from about 50 μm to about 125 micrometer gives better light transmission and substrate support layer flexibility. The conductive surface layer coated over the flexible substrate support can comprise any suitable electrically conductive material such as, for example, aluminum, titanium, nickel, chromium, copper, brass, stainless steel, silver, carbon black, graphite, and the like. The electrically conductive surface layer coated above the flexible substrate support layer may vary in thickness over a substantially wide ranges depending on the desired usage of the electrophotographic imaging member. However, from flexibility and partial light energy transmission considerations, the thickness of the conductive surface layer may be in a range from about 20 Å to about 750 Å. It is, nonetheless, desirable that the conductive surface layer coated over the flexible substrate support layer be between about 50 Å and 120 Å in thickness to provide sufficient light energy transmission of at least 20% transmittance to allow effective imaging member belt back erase.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] A more complete understanding of the imaging device which subjected to the processing of the present invention treatment can be obtained by reference to the accompanying drawings wherein:
[0019] [0019]FIG. 1 illustrates a schematic partial cross-sectional view of a typical multiple layered flexible sheet of electrophotographic imaging member as seen along the width of the multi-layer member.
[0020] [0020]FIG. 2 shows a schematic representation of a prior art heat treatment processing employed to impart electrophotographic imaging member web stock charge transport layer stress release outcome.
[0021] FIGS. 3 to 6 show schematic representations of several present invention heat treatment processing variances that yield effectual high speed electrophotographic imaging member web stock charge transport layer stress release processing treatment result.
[0022] In the drawings and the following description, like numeric designations refer to components of like function.
DESCRIPTION
[0023] For a general understanding of the present invention, reference is made to the drawings. In the drawings, like reference numerals have been used throughout to designate identical elements.
[0024] For the sake of convenience, the invention will only be described for electrophotographic imaging members in flexible belt form even though this invention includes electrostatographic imaging members of different materials configuration. Although specific terms are used in the following description for the sake of clarity, these terms are intended to refer only to the particular structure of the invention selected for invention in the drawings, and are not intended to define or limit the scope of the invention.
[0025] A typical, negatively charged, multilayered electrophotographic imaging member of flexible web stock configuration is illustrated in FIG. 1. Generally, such a member includes a substrate support layer 32 on which a conductive layer 30 , a hole blocking layer 34 , a photogenerating layer 38 , and an active charge transport layer 40 are formed. An optional adhesive layer 36 can be applied to the hole blocking layer 34 before the photogenerating layer 38 is deposited. Other layers, such as a grounding strip layer 41 or an overcoat layer 42 can be applied to provide various characteristics, such as improve resistance to abrasion. On the opposite surface of substrate support 32 , an anticurl backing layer 33 can be applied to reduce the curling induced by the different coefficients of thermal expansion of the various layers of the belt.
[0026] Belts prepared from the imaging member web stock of the type shown in FIG. 1 are generally well known in the art, as are materials appropriate for their formation. Examples of electrophotographic imaging members having at least two electrically operative layers, including a charge generator layer and diamine containing transport layer, are disclosed in U.S. Pat. Nos. 4,265,990, 4,233,384, 4,306,008, 4,299,897, and 4,439,507, the disclosures thereof being incorporated herein in their entirety.
[0027] The thickness of the substrate support 32 can depend on factors including mechanical strength, flexibility, and economical considerations, and can reach, for example, a thickness of at least about 50 μm. A typical maximum thickness of about 150 μm can also be achieved, provided there are no adverse effects on the final electrophotographic imaging device. The substrate support 32 should not soluble in any of the solvents used in each coating layer solution, optically clear, and being thermally stable enable to stand up to a high temperature of about 150° C. A typical substrate support 32 used for the prior art imaging member fabrication has a thermal contraction coefficient ranging from about 1×10 −5 /° C. to about 3×10 −5 /° C. and with a Young's Modulus of between about 5×10 5 psi and about 7×10 5 psi. However, materials with other characteristics can be used as appropriate.
[0028] The conductive layer 30 can vary in thickness over substantially wide ranges depending on the optical transparency and flexibility desired for the electrophotographic imaging member. Accordingly, when a flexible electrophotographic imaging belt is desired, the thickness of the conductive layer can be between about 20 Å and about 750 Å, and more preferably between about 50 Å and about 200 Å for an optimum combination of electrical conductivity, flexibility and light transmission. The conductive layer 30 can be an electrically conductive metal layer formed, for example, on the substrate by any suitable coating technique. Alternatively, the entire substrate can be an electrically conductive metal, the outer surface thereof performing the function of an electrically conductive layer and a separate electrical conductive layer may be omitted.
[0029] After formation of an electrically conductive surface, the hole blocking layer 34 can be applied thereto. The blocking layer 34 can comprise nitrogen containing siloxanes or nitrogen containing titanium compounds as disclosed, for example, in U.S. Pat. Nos. 4,291,110, 4,338,387, 4,286,033, and 4,291,110, the disclosures of these patents being incorporated herein in their entirety.
[0030] An optional adhesive layer 36 can be applied to the hole blocking layer. Any suitable adhesive layer may be utilized, such as a linear saturated copolyester reaction product of four diacids and ethylene glycol. Any adhesive layer employed should be continuous and, preferably, have a dry thickness between about 200 μm and about 900 μm and, more preferably, between about 400 μm and about 700 μm. Any suitable solvent or solvent mixtures can be employed to form a coating solution of polyester. Any other suitable and conventional technique may be utilized to mix and thereafter apply the adhesive layer coating mixture of this invention to the charge blocking layer.
[0031] Any suitable photogenerating layer 38 can be applied to the blocking layer 34 or adhesive layer 36 , if such an adhesive layer 36 is employed, which can thereafter be overcoated with a contiguous hole transport layer 40 . Appropriate photogenerating layer materials are known in the art, such as benzimidazole perylene compositions described, for example in U.S. Pat. No. 4,587,189, the entire disclosure thereof being incorporated herein by reference. More than one composition can be employed where a photoconductive layer enhances or reduces the properties of the photogenerating layer. Other suitable photogenerating materials known in the art can also be used, if desired. Any suitable charge generating binder layer comprising photoconductive particles dispersed in a film forming binder can be used. Additionally, any suitable inactive resin materials can be employed in the photogenerating binder layer including those described, for example, in U.S. Pat. No. 3,121,006, the entire disclosure thereof being incorporated herein by reference.
[0032] The photogenerating layer 38 containing photoconductive compositions and/or pigments and the resinous binder material generally ranges in thickness of from about 0.1 μm to about 5 μm, is preferably to have a thickness of from about 0.3 micrometer to about 3 μm. The photogenerating layer thickness is related to binder content. Higher binder content compositions generally require thicker layers for photogeneration. Thicknesses outside these ranges can be selected providing the objectives of the present invention are achieved.
[0033] The active charge transport layer 40 can comprise any suitable activating compound useful as an additive dispersed in electrically inactive polymeric materials making these materials electrically active. These compounds may be added to polymeric materials which are incapable of supporting the injection of photogenerated holes from the generation material and incapable of allowing the transport of these holes therethrough. This will convert the electrically inactive polymeric material to a material capable of supporting the injection of photogenerated holes from the generation material and capable of allowing the transport of these holes through the active layer in order to discharge the surface charge on the active layer. Thus, the active charge transport layer 40 can comprise any suitable transparent organic polymer or non-polymeric material capable of supporting the injection of photogenerated holes and electrons from the trigonal selenium binder layer and allowing the transport of these holes or electrons through the organic layer to selectively discharge the surface charge. The active charge transport layer 40 not only serves to transport holes or electrons, but also protects the photoconductive layer 38 from abrasion or chemical attack and therefor extends the operating life of the photoreceptor imaging member. The charge transport layer 40 should exhibit negligible, if any, discharge when exposed to a wavelength of light useful in xerography, for example, 4000 Å to 9000 Å. Therefore, the charge transport layer is substantially transparent to radiation in a region in which the photoconductor is to be used. Thus, the active charge transport layer is a substantially non-photoconductive material which supports the injection of photogenerated holes from the generation layer. The active transport layer is normally transparent when exposure is effected through the active layer to ensure that most of the incident radiation is utilized by the underlying charge carrier generator layer for efficient photogeneration. The charge transport layer in conjunction with the generation layer in the instant invention is a material which is an insulator to the extent that an electrostatic charge placed on the transport layer is not conducted in the absence of illumination.
[0034] The charge transport layer forming mixture preferably comprises an aromatic amine compound. An especially preferred charge transport layer employed in one of the two electrically operative layers in the multi-layer photoconductor of this invention comprises from about 35 percent to about 45 percent by weight of at least one charge transporting aromatic amine compound, and about 65 percent to about 55 percent by weight of a polymeric film forming resin in which the aromatic amine is soluble. The substituents should be free form electron withdrawing groups such as NO 2 groups, CN groups, and the like, and are typically dispersed in an inactive resin binder.
[0035] The charge transport layer 40 should be an insulator to the extent that the electrostatic charge placed on the charge transport layer is not conducted in the absence of illumination at a rate sufficient to prevent formation and retention of an electrostatic latent image thereon. In general, the ratio of the thickness of the hole transport layer to the charge generator layer is preferably maintained from about 2.1 to 200:1 and in some instances as great as 400:1. Generally, the thickness of the transport layer 40 is between about 5 μm and about 100 μm, but thickness outside this range can also be used provided that there are no adverse effects. Typically, it has a Young's Modulus in the range of from about 2.5×10 5 psi to about 4.5×10 5 psi and with a thermal contraction coefficient of between about 6×10 ×5 /° C. and about 8×10 −5 /° C. Furthermore, the charge transport layer also typically has a glass transition temperature T g of between about 75° C. and about 100° C.
[0036] Other layers, such as conventional ground strip layer 41 comprising, for example, conductive particles dispersed in a film forming binder may be applied to one edge of the photoreceptor in contact with the conductive layer 30 , hole blocking layer, adhesive layer 36 or charge generating layer 38 . The ground strip 41 can comprise any suitable film forming polymer binder and electrically conductive particles. Typical ground strip materials include those enumerated in U.S. Pat. No. 4,664,995. The ground strip layer 41 may have a thickness from about 7 μm to about 42 μm, and preferably from about 14 μm to about 23 μm. Optionally, an overcoat layer 42 , if desired, can also be utilized to improve resistance and provide protection to imaging member surface abrasion.
[0037] The charge transport layer 40 typically has a great thermal contraction mismatch compared to that of the substrate support 32 . As a result, the prepared flexible electrophotographic imaging member exhibits spontaneous upward curling due to the result of larger dimensional contraction in the charge transport layer than the substrate support, especially as the imaging member cools down to room ambient after the heating/drying processes of the applied wet charge transport layer coating. An anti-curl back coating 33 can be applied to the back side of the substrate support 32 (which is the side opposite the side bearing the electrically active coating layers) to induce flatness. The anticurl back coating 33 can comprise any suitable organic or inorganic film forming polymers that are electrically insulating or slightly semi-conductive.
[0038] The anticurl back coating 33 should have a thermal contraction coefficient of at least about 1×10 −5 /° C. greater than that of the substrate support to be considered satisfactory. Typically, a substrate support has a thermal contraction coefficient of about 2×10 −5 /° C. However, anti-curl back coating with a thermal contraction coefficient at least +2×10 −5 /° C. larger than that of the substrate support is preferred to produce an effective anti-curling result. The selection of a thermoplastic film forming polymer for the anti-curl back coating application has to be satisfying all the physical, mechanical, optical, and importantly, the thermal requirements above. Polymer materials which can meet these invention requirements include a variety of polymers as is known in the art. These polymers can be block, random or alternating copolymers. Furthermore, the selected film forming thermoplastic polymer for anticurl back coating 33 application, if desired, can be of the same binder polymer used in the charge transport layer 40 .
[0039] The fabricated multilayered, flexible electrophotographic imaging member web stock of FIG. 1 is then cut into rectangular sheets and converted into imaging member belts. The two opposite edges of each imaging member cut sheet are then brought together by overlapping and may be joined by any suitable method, including ultrasonic welding, gluing, taping, stapling, and pressure and heat fusing to form a continuous imaging member seamed belt, sleeve, or cylinder. From the viewpoint of considerations such as ease of belt fabrication, short operation cycle time, and mechanical strength of the fabricated joint, the ultrasonic welding process is more advantageous. The prepared flexible imaging belt can therefore be employed in any suitable and conventional electrophotographic imaging process that utilizes uniform charging prior to imagewise exposure to activating electromagnetic radiation.
[0040] As known from the principles of material mechanics, as the flexible imaging member seamed belt bends over the exterior surfaces of rollers of a belt module within an electrophotographic imaging machine during dynamic belt cycling function, the bottom surface of the anticurl back coating 33 of the flexible imaging member belt is compressed. In contrast, the top surface of charge transport layer 40 is stretched and placed under tension. This is attributable to the fact that the top and bottom surfaces move in a circular path about the circular roller. Since the top surface of charge transport layer 40 is at greater radial distance from the center of the circular roller than the bottom surface of anticurl back coating 33 , the top surface must, travel a greater distance than the bottom surface in the same time period. Therefore, the top surface must be under tension relative to a generally central portion of the flexible imaging member seamed belt (the portion of the flexible imaging member seamed belt generally extending along the center of gravity of the flexible imaging member seamed belt). Likewise, the bottom surface must be compressed relative to the generally central portion of the flexible imaging member seamed belt (the portion of the flexible imaging member seamed belt generally extending along the center of gravity of the flexible imaging member seamed belt). Consequently, the bending stress at the belt top surface will be tension stress, and the bending stress at the belt bottom surface will be compression stress as the imaging member belt flexes over each belt module support roller under a machine functioning condition.
[0041] From fracture mechanics, it is known that compression stresses, such as that at the bottom belt surface, rarely cause mechanical failure. Tension stresses, such as that induced at the top belt surface, however, are a more serious problem. The tension stress, under constant belt fatiguing condition, has been determined to be the root cause that promotes the development of charge transport layer 40 cracking problem. The cracks, though initiated in the charge transport layer 40 , continue to propagate to the generator layer 38 , extend to the adhesive interface layer 36 , cut through the blocking layer 34 , and reach further to the conductive layer 30 .
[0042] However, multiple layer belts with significant difference between layer thermal contraction coefficients exhibit spontaneous upward imaging member curling, due in part to the dimensional contraction mismatch between these layers. The imaging members thus can require an anticurl back coating 33 applied to the back side of the substrate support layer 32 to balance the upward lifting force. This induces imaging member flatness prior to belt preparation, but yields belts with built-in internal strain. This internal strain can reach level of, for example, approximately 0.28%, and is additive to the bending strain induced during imaging member belt fatigue under machine operational conditions. The cumulative effect of internal strain plus bending strain further promotes the early onset of dynamic fatigue charge transport layer cracking during imaging member belt cyclic machine function. Moreover, bands of charge transport layer cracking caused by exposure to airborne chemical contaminants have also been found to form at imaging member belt segments parked/bent directly over each belt module support rollers over periods of machine idling and shut-off time.
[0043] Both dynamic belt fatigue and chemical contaminant exposure induced crackings in the charge transport layer 40 of the imaging member seamed belt are serious mechanical failures that should be resolved and/or avoided. These cracks manifest as copy printout defects, shortening the usefulness and service life of the flexible imaging member seamed belts.
[0044] To extend the charge transport layer cracking life, innovative imaging member web stock processing treatment has been successfully pursued and demonstrated to reduce the charge transport layer internal strain, as well as in reduction of imaging member belt bending strain over belt module support rollers, according to the exemplary stress-release processing representation of a prior art shown in FIG. 2. An electrophotographic imaging member, unwound from, for example, a supplied roll-up web stock 10 , and is directed with the charge transport layer facing outwardly, for example under a one pound per linear inch tension and a web stock transport speed of about 10 feet/min, toward a one-inch outer diameter free-rotation processing treatment metal tube 206 having an arcuate Teflon® coated outer surface 210 , and an annulus 209 with passing cool water to maintain constant treatment tube temperature. The imaging member web stock 10 under 25° C. ambient, makes an entering contact at 12 o'clock with the tube 206 and is conformed to the arcuate surface 210 . A powerful IR emitting tungsten halogen quartz heating source 103 , positioned directly above, brings upon an instant localized temperature elevation to the charge transport layer to about 10° C. above its glass transition temperature (T g ) to facilitate molecular motion of the polymer in the layer and effect instant charge transport layer stress-release while the segment of the webstock is under bending conformance contact over the arcuate surface 210 . The heat source 103 is an integrated unit having a length sufficiently covering the whole width of the imaging member web stock; it consists of a hemi-ellipsoidal cross-section elongated reflector 106 and a halogen quartz tube 105 positioned at one focal point inside the reflector 106 such that all the IR radiation energy emitted form tube 105 was reflected and converged at the other focal point outside the reflector 106 to give a 6 mm width focused heating region 108 that effects instant charge transport layer temperature elevation to beyond its T g . The heated segment of charge transport layer after exposure to the heating region 108 began to cool down to below the T g , through direct heat conduction to tube 206 and as well as heat transfer to ambient air, as the web stock in continuous motion is transported away from heat source 103 . A further and final charge transport layer cooling is assured by air impingement from an air knife 203 A (directing a high velocity, preferably super-sonic, narrow stream of cool air onto the surface of the web stock) positioned at 4 o'clock to tube 206 prior to the web stock segment emerging from the curved contacting zone region to complete the imaging member web stock stress-release treatment process. In this figure, the numerals 30 , and 30 A are paths where the transporting imaging member is freely suspended, while 40 and 40 A are contact zones at which the segment of the imaging member is intimately riding over the treatment tube 206 .
[0045] The material configuration of a typical electrophotographic imaging member web stock 10 , like that shown in FIG. 1, used for the stress release processing treatment according to the illustrative representation of FIG. 2 comprises a 3.5 mils flexible substrate support layer 32 , about 100 Angstrom thickness of the titanium conductive layer 30 , a 0.02 micrometer hole blocking layer 34 , a 0.03 micrometer adhesive layer 36 , a 0.08 micrometer photogenerating layer 38 , a 29 μm charge transport layer 40 , a 18 micrometer conventional electrically conductive ground strip 41 coated along one edge of the imaging member web stock adjacent to the charge transport layer 40 , and a 17 μm anticurl back coating 33 to give a complete imaging member web stock material package having reasonably good physical flexibility and flatness. With this imaging member web stock package, the processing treatment carried out though is seen to produce good charge transport layer stress releasing result, but only found to be effectual at a web stock transport speed of not to exceed 8 feet/min. The low web stock processing treatment speed limitation diminishes the practical value of the treatment process, making it less attractive for cost effective electrophotographic imaging member production implementation consideration. The impediments to high speed imaging member web stock processing treatment shown in FIG. 2 have been determined to be (1) insufficient heating capacity to substantially instantly, or at least extremely rapidly, bring the web stock segment up to the intended temperature target; (2) inadequate or insufficient cooling capacity to bring the segment temperature down quickly enough to effect charge transport layer stress release result prior to web stock exiting from the treatment roller 206 ; or, (3) insufficient capacity in both heating and cooling of web stock during treatment processing.
[0046] To overcome these deficiencies, embodiments provide a modified fine tuning treatment process that can provide reduce strain/stress in imaging member web stock at higher, more practical speeds. In particular, embodiments reduce strain/stress in a layer, such as a charge transport layer, of imaging member web stock. FIGS. 3 to 5 schematically illustrate embodiments that advantageously focus on effectual cooling capacity enhancement to enable high speed imaging member web stock processing. FIG. 6 schematically illustrates embodiments employing a combination of heating and cooling capacity enhance to reduce strain/stress. In addition, embodiments can advantageously employ a treatment tube 206 outer diameter of between about 0.5 inch and about 3 inches. An outer diameter in the range of from about 0.5 inch to about 2 inches can provide more advantageous processing operation control stress release.
[0047] [0047]FIG. 3 schematically illustrates embodiments employing a modification and refinement process related to that of FIG. 2 to enhance cooling capacity. This cooling capacity enhancement can improve imaging member web stock charge transport layer stress release processing. As shown in this figure, a cooling air stream is first bubbling and passed through a water medium 52 inside a container to bring along atomized liquid water mist to the air delivery knife 203 for impacting quick impinging air cooling result. Since air is a poor heat conductor and has low heat capacity, an air stream carrying atomized liquid water can provide the heat extraction capability increase by many times.
[0048] Referring to FIG. 3, which schematically illustrates an exemplary embodiment of a process of the present invention for treating a flexible multilayered electrophotographic imaging member web stock having material configuration identical to that of imaging member 10 described in FIG. 1. This invention process with the intent to effect the result of charge transport layer 40 internal stress release is carried out by continuous processing treatment. The imaging member 10 web stock is, for example, unwound from an imaging member supply roll with the charge transport layer 16 facing outwardly is directed toward a processing treatment free rotating tube 206 having an arcuate outer surface 210 and an annular chamber 209 . In embodiments, the roll can have around 6000 feet of web stock, and the speed can be around one pound per linear inch width. The imaging member 10 web stock, at ambient temperature of about 25° C., makes an entering contact at 12 o'clock and conforms to the arcuate surface 210 of tube 206 . As shown in the figure, a high power heat source 103 , such as an infrared emitting tungsten halogen quartz heating source, positioned directly above brings an instant localized temperature elevation in the charge transport layer 40 of the bending/contacting imaging. member 10 to between about 5° C. and about 25° C. over its glass transition temperature T g . The glass transition temperature, T g , is defined as the temperature at which the polymer material changes from a rigid to a flexible state. Heating the charge transport layer 40 to such a temperature range above its T g facilitates molecular motion in the polymer and effects release of the bending induced and internal built-in stress in the charge transport layer 40 while the segment of imaging member 10 is in bending conformance over the arcuate surface 210 . The heating source 103 can be, for example, an integrated unit having a length covering the width of the imaging member 10 and can include a hemi-ellipsoidal shaped cross-section elongated reflector 106 and a halogen quartz tube 105 positioned at a focal point inside the reflector 106 , such that all the infrared radiant energy emitted from tube 105 is reflected and converges at the other focal point outside the reflector 106 . A focused heating line 108 over the charge transport layer 16 surface can substantially instantaneously bring about temperature elevation. A line width of about 6 mm can provide sufficient heating in embodiments, though the dimensions and materials used in particular situations may require larger or smaller value.
[0049] The heated section of the charge transport layer 40 after exposure to the focused heating line 108 will then be gradually cooling down when the imaging member 10 is transported away from the heat source 103 , through direct heat conduction to tube 206 as well as convection to the surroundings, since the web stock has been set to motion in a constant processing treatment speed over the arcuate surface 210 . A final cooling down of the charge transport layer 40 and the web stock is facilitated by a cooling air stream delivered by an air knife positioned between about 4 o'clock and 6 o'clock to assure temperature lowering of the exiting imaging member section to a temperature of at least about 20° C. (preferably 40° C.) below the T g of the charge transport layer 40 to yield permanent stress release result. The cooling air stream is first bubbling and passed through a water medium 52 inside a container to bring along atomized liquid water mist to the air delivery knife 203 , such that the air stream impinging on the imaging member web stock can quickly be cooled down by the large heat extraction effect derived from both the large water heat capacity constant and its latent heat of evaporation. The annular chamber 209 of the treatment tube 206 can be filled with air, or can have a coolant passing therethrough such as water, liquid nitrogen, alcohol, or another suitable coolant.
[0050] An alternative cooling enhancement process of the present invention in embodiments is shown in FIG. 4. In this process, the air impingement cooling device can be replaced with a low durometer (about 10 Shore A hardness) soft free rotating silicone cooling nip-roller 50 , having a frictionless rotating shaft 51 , to impact quick imaging member web stock cooling and effect high speed treatment processing result, since solid conduction contact cooling is much more efficient than air stream cooling, since air is a relatively poor heat conductor. A water cooling bath 52 can be used to quickly cool the roll 50 . In such cases, the water cooling bath 52 with partial submersed silicone nip-roll 50 is controlled at a substantially constant temperature to ensure steady state treatment processing. Direct liquid water contacting an imaging member can weaken imaging member internal layer adhesion. However, since the silicone nip-roller 50 has a low surface energy of about 18 dynes/cm, direct liquid water wetting of the surface of imaging member web stock 10 , brought upon by the silicone roller, is safely prevented. Furthermore, it is preferred that the soft silicone roller material matrix also contain metallic particle dispersion to increase its heat conduction capability.
[0051] [0051]FIG. 5 is an embodiment invention processing variance modified from FIG. 4, in which the water cooling bath 52 and the frictionless shaft 51 are substituted with a metallic cooling tube 54 with cooling water passing through its annulus to control and maintain constant processing temperature as well as. providing quick imaging member web stock cooling down result.
[0052] [0052]FIG. 6 schematically illustrates embodiments that employ a combination of enhanced heating and enhanced cooling to accommodate high imaging member web stock transporting speed for achieving effective charge transport layer stress release outcome. A substantially frictionless or low friction heating roller 58 can be added and positioned a short distance from the treatment tube 206 to pre-heat the imaging member web stock. The added heating roller 58 can be a solid electrically heated roller having Teflon coating on the surface; otherwise it can be a free rotating Teflon coated surface metal tube with hot water passing through its annulus to provide heating. Alternatively, embodiments can employ an additional IR heating source, like that of 103 , for example, in which dual IR heating beams are employed. To enhance the cooling effect, the air knife 203 A is provided with an impinging cooled air stream, liquid nitrogen, CO 2 snow, sub-cooled alcohol, low temperature cooling water, or another suitable coolant to accelerate the real time impact for quick imaging member web stock temperature lowering effect. One added benefit of employing the added heating roller 58 (or heating tube) is also that the wrap angle of the imaging member web stock around the treatment tube 206 can thereby be conveniently increased to more than 180° and give more. surface area for achieving effectual treatment processing.
[0053] For electrographic imaging members, a flexible dielectric layer overlying the conductive layer can be substituted for the active photoconductive layers. Any suitable, conventional, flexible, electrically insulating, thermoplastic dielectric polymer matrix material may be used in the dielectric layer of the electrographic imaging member. If desired, the flexible belts preparation methods of embodiments can be applied to other purposes in which belt cycling durability, such as against fatigue surface cracking, is an important issue.
[0054] The invention will further be illustrated in the following non-limiting examples, it being understood that these examples are intended to be illustrative only and that the invention is not intended to be limited to the materials, conditions, process parameters and the like recited herein. All proportions are by weight unless otherwise indicated.
CONTROL EXAMPLE I
[0055] A flexible electrophotographic imaging member web stock, in reference to the illustration in FIG. 1, was prepared by providing a 0.01 μm thick titanium layer 30 coated onto a flexible biaxially oriented Polynaphthalate substrate support layer 32 (Kadalex®, available from ICI Americas, Inc.) having a thermal contraction coefficient of about 1.8×10 −5 /° C., a glass transition temperature Tg of 130° C., and a thickness of 3.5 mils or 88.7 μm, and applying thereto, by a gravure coating process, a solution containing 10 grams gamma aminopropyltriethoxy silane, 10.1 grams distilled water, 3 grams acetic acid, 684.8 grams of 200 proof denatured alcohol and 200 grams heptane. This layer was then dried at 125° C. in a forced air oven. The resulting blocking layer 34 had an average dry thickness of 0.05 μm measured with an ellipsometer.
[0056] An adhesive interface layer was then extrusion coated by applying to the blocking layer a wet coating containing 5 percent by weight based on the total weight of the solution of polyester adhesive (Mor-Ester 49,000®, available from Morton International, Inc.) in a 70.30 volume ratio mixture of tetrahydrofuran/cyclohexanone. The resulting adhesive interface layer 36 , after passing through an oven, had a dry thickness of 0.095 μm.
[0057] The adhesive interface layer 36 was thereafter coated with a photogenerating layer 38 . The photogenerating layer dispersion is prepared by introducing 0.45 grams of IUPILON 200® poly(4,4′-diphenyl)-1,1′-cyclohexane carbonate, available from Mitsubishi Gas Chemical Corp and 50 mL of tetrahydrofuran into a glass bottle. To this solution is added 2.4 grams of Hydroxygallium Phthalocyanine and 300 grams of ⅛ inch (3.2 mm) diameter stainless steel shot. This mixture is then placed on a ball mill for 20 to 24 hours. Subsequently, 2.25 grams of poly(4,4′-diphenyl)-1,1′-cyclohexane carbonate is dissolved in 46.1 grams of tetrahydrofuran, then added to this hydrogallium phthalocyanine slurry. This slurry is then placed on a shaker for 10 minutes. The resulting slurry was, thereafter, extrusion coated onto the adhesive interface 36 by extrusion application process to form a layer having a wet thickness of 0.25 mL. However, a strip about 10 mm wide along one edge of the substrate web bearing the blocking layer and the adhesive layer was deliberately left uncoated by any of the photogenerating layer material to facilitate adequate electrical contact by the ground strip layer that was applied later. This photogenerating layer was dried at 135° C. for 5 minutes in a forced air oven to form a dry thickness photogenerating layer 38 having a thickness of 0.41 μm layer.
[0058] This coated imaging member web was simultaneously co-extrusion overcoated with a charge transport layer 40 and a ground strip layer 41 . The charge transport layer was prepared by introducing into an amber glass bottle a weight ratio of 1:1 N,N′-diphenyl-N,N′-bis(3-methylphenyl)-1,1′-biphenyl-4,4′-diamine and Makrolon 5705®, a polycarbonate resin having a weight average molecular weight of about 120,000 commercially available from Farbensabricken Bayer A. G. The resulting mixture was dissolved to give a 15 percent by weight solids in 85 percent by weight methylene chloride. This solution was applied over the photogenerator layer 38 to form a coating which, upon drying, gave a charge transport layer 40 thickness of 29 μm, a thermal contraction coefficient of 6.5× 10 −5 /° C., and a glass transition temperature, T g , of about 85° C.
[0059] The approximately 10 mm wide strip of the adhesive layer 36 left uncoated by the photogenerator layer 38 was coated with a ground strip layer during a co-coating process. This ground strip layer 41 , after drying at 125° C. in an oven and eventual cooling to room ambient, had a dried thickness of about 19 μm. This ground strip was electrically grounded, by conventional means such as a carbon brush contact means during conventional xerographic imaging process. The electrophotographic imaging member web stock, at this point if unrestrained, would spontaneously curl upwardly into a tube due to the thermal contraction mismatch between the charge transport layer 40 and the substrate support layer 32 , resulting in greater charge transport layer 40 dimensional shrinkage than the substrate support layer 32 which thereby causing substantial internal stress built-in in the charge transport layer 40 . The curled electrophotographic imaging member web stock was used to serve as a control.
CONTROL EXAMPLE II
[0060] Another flexible electrophotographic imaging member web stock was prepared by following the procedures and using materials as described in the Control Example I, but with the exception that the imaging member web stock curling was controlled by application of an anticurl back coating 33 to render the desired imaging member web stock flatness.
[0061] An anticurl back coating solution was prepared by combining 8.82 grams of polycarbonate resin (Makrolon 5705®, available from Bayer AG), 0.72 gram of polyester resin (Vitel PE-200®, available from Goodyear Tire and Rubber Company) and 90.1 grams of methylene chloride in a glass container to form a coating solution containing 8.9 percent by weight solids. The container was covered tightly and placed on a roll mill for about 24 hours until the polycarbonate and polyester were dissolved in the methylene chloride to form the anticurl back coating solution. The anticurl back coating solution was then applied to the rear surface of the substrate support layer 32 (the side opposite the photogenerator layer and charge transport layer) of the imaging member web stock and dried at 125° C. to produce a dried anticurl back coating 33 thickness of about 17.5 μm. The resulting electrophotographic imaging member web stock had the desired flatness and with the same material structure as that schematically illustrated in FIG. 1 is a complete imaging member full device. The fabricated electrophotographic imaging member web stock was also used to serve as another imaging member control.
COMPARATIVE EXAMPLE I
[0062] The flexible electrophotographic imaging member web stock 10 full device of Control Example II was used for charge transport layer (CTL) heat stress release processing treatment according to the pictorial representation shown in FIG. 2. This invention concept, with the intent to reduce the internal stress in CTL 40 , was conducted through this continuous web stock heat treatment processing.
[0063] In essence, the imaging member web stock 10 was unwound from a 6,000 feet roll-up imaging member supply roll was directed (with the CTL 40 facing outwardly, under a one pound per linear inch width web tension, and a web stock transport speed of 10 feet per minute) toward a one-inch outer diameter free rotation processing treatment metal tube 206 having an arcuate outer surface 210 , a wall thickness, and an annulus 209 . The imaging member web stock 10 , under 25° C. ambient temperature, made an entering contact at 12 o'clock with the tube 206 and conformed to the arcuate surface 210 . A powerful infrared emitting tungsten halogen quartz heating source 103 , positioned directly above, brought upon an instant localized temperature elevation to the CTL 40 to 10° C. above its T g to facilitate molecular motion and effect instant stress release from the CTL 40 while the segment of the imaging member web stock 10 was in bending conformance contact over the arcuate surface 210 . The heating source 103 was an integrated unit having a length sufficiently covering the whole width of the imaging member segment; it consist of a hemi-ellipsoidal cross-section elongated reflector 106 and a halogen quartz tube 105 positioned at one focal point inside the reflector 106 such that all the infrared radiant energy emitted from tube 105 was reflected and converged at the other focal point outside the reflector 106 to give a 6 mm width focused heating line 108 that effected instant CTL 40 temperature elevation beyond its T g .
[0064] The heated segment of CTL 40 after exposure to the heating line 108 would begin to cool down, through direct heat conduction to tube 206 and heat transfer to ambient air, as the imaging member web stock in constant motion was transported away from heat source 103 . A further and final CTL 40 cooling was assured by air an impingement from an air knife positioned at 4 o'clock to the tube 206 prior to imaging member web stock segment 10 emerging from tube 206 to complete the treatment process. In this charge transport layer stress release processing treatment experimental demonstration, two different imaging member transporting speeds, a 7 feet/min. and a 15 feet/min., had been tried to assess invention processing effectiveness.
COMPARATIVE EXAMPLE II
[0065] The flexible electrophotographic imaging member web stock having no anticurl back coating layer, prepared according to Control Example I, was also subjected to the exact same CTL stress release processing treatment procedures by following the descriptions in the preceding Comparative Example I, again using same two different imaging member web stock transporting speeds.
COMPARATIVE EXAMPLE III
[0066] The flexible electrophotographic imaging member web stock having no anticurl back coating layer, prepared according to Control Example I, was also subjected to the exact same CTL stress release processing treatment procedures, by following the descriptions in the preceding Comparative Example I and again using same two different imaging member web stock transporting speeds. The air knife 203 A was impinging CO 2 snow instead of air to effect fast imaging member web stock cooling, and dual IR heating beams were employed to effect rapid CTL temperature elevation to at least 5° C. beyond its Tg.
MECHANICAL BELT CYCLING TEST EXAMPLE
[0067] The flexible electrophotographic imaging member web stocks of Control Examples I and II and Comparative Examples I to III were each cut to precise dimensions of 440 mm width and 2,808 mm in length. The opposite ends of each cut imaging member sheet were secured to give 1 millimeter overlap and ultrasonically welded, using 40 KHz horn frequency, in the long dimension, to form a seamed flexible imaging member belt for fatigue dynamic electrophotographic imaging test in a selected xerographic machine utilizing a belt module comprises numerous belt support rollers, in particular a small one inch diameter paper stripping roller.
[0068] The dynamic machine belt cycling test results obtained showed that the onset of fatigue induced charge transport layer cracking was found to be evident much earlier for both control imaging member belts prepared directly from Control Examples I and II than those seen for all the stress release processing treated imaging member belt counterparts of the Comparative Examples I, II, and III. Delaying of fatigue charge transport layer cracking was realized by subjecting the imaging member web stock through stress release processing treatment of embodiments. The cracking life extension gain was, however, slight for the higher web stock processing treatment speed of 15 feet/min., but significantly effectual only for the lower 7 feet/min. web stock speed imaging belt fabricated from Comparative Examples I and II, employing impinging air cooling. By comparison, when the impinging air knife 206 A was provided to deliver impinging CO 2 snow, according to Comparative Example III, the resulting imaging member belts prepared from both 7 feet/min. and 15 feet/min. web stock processing treatment speeds were seen to give approximately identical fatigue charge transport layer cracking life extension gain. These fatigue cycling belt life results obtained from machine testings are a definite indication that quick imaging member web stock cooling was significantly advantageous to bring about effective charge transport layer stress release outcome for life extension. Comparison of the functional belt life enhancement seen among all the imaging member belts, fabricated from web stocks through the processing treatment condition variances of the three Comparative Examples, leads one to conclude that the inventive processing treatment works. In particular, the treatment should use: (1) at least one high power heat source, such as a localized focused heating line, to substantially instantaneously and sufficiently bring about charge transport layer temperature above its T g for effectual stress releasing the charge transport layer while the imaging member web stock was bent over the treatment tube, and (2) a final cooling device directed over the charge transport layer should be employed to achieve rapid charge transport layer temperature lowering prior to web stock exiting at 6 o'clock position from the treatment tube. Such enhanced heating and cooling can enhance treatment and allow higher speed imaging member web stock processing treatment to effect charge transport layer stress release result and impact cracking life extension.
[0069] In summary, the integration of an efficient heat energy delivery system and in combination of employing an enhanced heat extraction capability technique for quick imaging member cooling to the invention process is advantageous and represents an effectual improvement over the prior art in achieving electrophotographic imaging member web stock stress release outcome for transporting motion of imaging member web stock at high speed.
[0070] While particular embodiments have been described, alternatives, modifications, variations, improvements, and substantial equivalents that are or may be presently unforeseen may arise to applicants or others skilled in the art. Accordingly, the appended claims as filed and as they may be amended are intended to embrace all such alternatives, modifications variations, improvements, and substantial equivalents.
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Multilayered web stock is directed toward a curved surface and at least one layer of the web stock is heated to a temperature above a glass transition temperature of the at least one layer of the web stock. The heating can occur just before or upon engaging the curved surface. The temperature of the at least one layer remains above the glass transition temperature while engaging the curved surface, allowing reshaping and/or realignment of the at least one layer relative to other layers of the web stock according to conformance to the curved surface. The web stock is cooled before it disengages from the curved surface. The heating can be done with a high power infrared lamp focused into a line across the web stock, and the cooling can be done with a cooled fluid jet. Additionally, a preheater can be employed, and a supplemental cooler can be used.
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FIELD OF THE INVENTION
This invention relates to a flat knitting machine comprising flexible shank needles arranged in the needle channels of the needle bed, each said needle having an anterior first needle butt always projecting from the needle bed and a posterior second needle butt which sinks into the needle bed under the resilience of its own flexible shank, jacquard jacks arranged rearwardly of the flexible shank needles for selective lifting of said second needle butts, and cam means movable over the needle bed and comprising interengageable needle, jacquard and selection cam units incorporating fixed and shiftable cam elements. One such flat knitting machine is known for example from the publication "Wirkerei- und Strickerei-Technik", Coburg, February 1960, No. 2, page 835.
Generally, fabric technology in modern flat knitting is based on the formation of stitches and tuck loops and upon the absence of knitting during the course of a row of knitting. From the combination possibilities of these three formation processes, in combination with the needle bed filling, stitch transfer and changes of colour, all patterns can be created. In order to be able to achieve an optimisation of these patterns, additional possibilities have been created which, on the one hand, by different withdrawal depths of the needles within a row of knitting, permit the production of prominent relief patterns for example, and which, on the other hand, by the formation of the needles with needle butts which are lowerable into the needle bed offer the possibility of not having to withdraw needles which are loaded with stitches but which are not operating in a given row of knitting, and consequently to take care of such stitches. In order to carry out all these techniques, the most varied combinations of needles and jacks are known.
With the presently known techniques which use needles having needle butts which are lowerable in the needle beds it is always necessary that the bottom of the needle channel in the needle bed is slotted on two different levels. The needle channels are slotted deeper in the needle bed space required for the lowering of the needle butts than in the needle bed space needed for the formation of stitches in the forward region immediately behind the abutment cams. The manufacture of such needle beds is considerably more complex and expensive than the cutting of needle channels in conventional flat knitting machines without lowerable needle butts, in which the needle channel cutting can take place in one pass and without stepping.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a flat knitting machine of the type first referred to above which permits all selection possibilities for the sinkable needle butts, and in which the cutting of the needle channels in the needle bed can be carried out without stepping, in other words in one cutting pass with constant cutting depth.
This is achieved in accordance with the present invention, in a flat knitting machine of the type first referred to above, in that
(a) behind each flexible shank needle there is provided a displaceable arresting jack having both an arresting jack butt and also a coupling portion at its forward end for coupling to the flexible shank of the flexible shank needle and for simultaneously lifting said second needle butt from the needle bed,
(b) behind the arresting jack there is displaceably mounted a jacquard jack which has a first, operating butt and a second, selection butt, and
(c) in the needle cam unit, at least in the region of said second needle butt, and symmetrically arranged with respect to the central longitudinal axis of the cam means, there are provided two needle sinkers displaceable in the plane of the cam means and two cam units shiftable into and out of the plane of the cam means for extending the needles for the formation of stitches.
Preferably, in the needle cam unit, in the region of said first needle butt, and symmetrically arranged with respect to the central longitudinal axis of the cam means, there are provided two needle sinkers displaceable in the plane of the cam means and two cam units shiftable into and out of the plane of the cam means for extending the needles for the formation of stitches, and also a shiftable needle sinker cam unit provided in the region of one of said needle sinkers. Four selectively shiftable selection keys may be provided in the selection cam unit and symmetrically with respect to the central longitudinal axis of the cam means.
With the flat knitting machine of the present invention, in combination with a flexible shank needle, all arresting and selection jacks with the associated cam means create the possibility of a needle selection which covers the full spectrum of the fabric technology as described above, including transfer of stitches and knitting with different withdrawal depths within one row of knitting, with a very simple and cost-effective needle bed with a compact cam structure. The second needle butt occupies the position raised up from the needle bed always immediately against the arresting jack and consequently is supported strongly by the bottom of the needle channel.
In one simplified embodiment of the invention, in which no selective differential needle withdrawals can be achieved in one row of knitting, the displaceable needle sinkers in the needle cam unit in the region of the first needle butts are replaced by fixed cam units and said two shiftable cam units are omitted.
According to a further alternative within the scope of the invention, the shiftable needle sinker cam unit in the needle cam unit in the region of the first needle butt is omitted and the displaceable needle sinkers are arranged to be retractable, for example pivotable.
Preferably, at the underside of each said second needle butt, there is an arresting cam with two oppositely directed inclined cam surfaces, while the coupling portion of each arresting jack has a latching groove for receiving the arresting cam and is provided at its forward end with two further oppositely directed inclined cam surfaces. By this means one achieves a particularly compact and functionally reliable coupling and uncoupling of the flexible shank needle and arresting jack.
The jacquard jack is preferably arranged to be slidable in part on the arresting jack.
Furthermore, the active operating region of the arresting jack butt preferable extends over the width of a lengthwise recess in the upper surface of the needle bed.
The selection butts of successive jacquard jacks and the associated selection keys are preferably arranged staggered in the lengthwise direction of the needle channels.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be described in more detail with reference to a number of embodiments which are given by way of example and which are illustrated in the drawings. In the drawings:
FIG. 1 is a cross-sectional view through a needle bed, taken along the length of a needle bed channel, with a flexible shank needle shown in its basic, inactive position and with an arresting jack and jacquard jack also inactive;
FIG. 2 is a cross-sectional view, as in FIG. 1, with the jacquard jack located in its basic position and having its selection butt brought into the selection zone;
FIG. 3 is a cross-sectional view, as in FIG. 1, in which the arresting jack is shown immediately before its coupling with the flexible shank needle;
FIG. 4 is a cross-sectional view, as in FIG. 1, in which the arresting jack is coupled to the flexible shank needle;
FIG. 5 is a schematic plan view of a preferred embodiment of cam system according to the invention;
FIG. 6 is a plan view, as in FIG. 5, shifted for the formation of stitches of equal withdrawal length;
FIG. 7 is a plan view, as in FIG. 5, shifted for the formation of tuck loops of equal withdrawal length;
FIG. 8 is a plan view, as in FIG. 5, shifted for working by the three-path technique for the formation of tuck loops and stitches with the same withdrawal length;
FIG. 9 is a plan view, as in FIG. 5, shifted for the donation of stitches in the transfer process;
FIG. 10 is a plan view, as in FIG. 5, shifted for the acceptance of stitches in the transfer process;
FIG. 11 is a plan view, as in FIG. 5, shifted for the formation of short and long stitches;
FIG. 12 is a plan view, as in FIG. 5, shifted for the formation of short and long tuck loops;
FIG. 13 is a plan view, as in FIG. 5, shifted for working by the three-path technique for the formation of short stitches and long tuck loops;
FIG. 14 is a plan view of a simplified cam system according to the invention with constant needle withdrawal during one row of knitting, shifted for the three-path technique for the formation of equal length tuck loops and stitches; and,
FIG. 15 is a schematic plan view of a further embodiment of cam system in accordance with the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIGS. 1 to 4 there are shown cross-sectional views through a needle bed 1, taken along the length of the needle channel, illustrating various different positions of a flexible shank needle 2, an arresting jack 3 and a jacquard jack 4 relative to one another, before the coupling of the flexible shank needle 2 to the arresting jack 3, as well as showing the coupled state of these two latter components.
In FIG. 1 the flexible shank needle 2 is shown in the level-cams position where it is inactive (basic position); the arresting jack 3 and the jacquard jack 4 are also inactive.
The needle channels in the needle bed 1 are all formed with the same depth and with the same depth throughout their length. The flexible shank needles 2, the arresting jacks 3 and the jacquard jacks 4 are held in the needle bed by cover strips 5,6 and 7 respectively.
Each flexible shank needle 2 has a first needle butt and a second needle butt 9. The first, anterior needle butt 8 always projects from the needle bed 1. The second needle butt 9 is arranged at the rear end of a flexible shank 10 of the flexible shank needle 2 and is inactive in its basic position, i.e. it disappears into the needle bed 1 by virtue of the springiness of its own flexible shank 10.
At the underside of the second needle butt 9 there is provided an arresting cam 11 which, in its basic position, rests upon the bottom of the needle channel. The arresting cam 11 has two oppositely directed inclined cam surfaces 12 and 13 which are required for the coupling of the flexible shank needle 2 to the arresting jack 3.
At its anterior end the arresting jack 3 has a coupling portion 14 which is formed with two further oppositely directed inclined cam surfaces 15 and 16. Behind the coupling portion 14 there is a latching groove 25 to receive the arresting cam 11 of the flexible shank needle 2. Additionally, the arresting jack 3 has an arresting jack butt 17 whose active working zone extends over the width of a lengthwise recess 18 in the upper surface of the needle bed 1. The arresting jack butt 17 projects above the bottom of the lengthwise recess 18 but not however above the upper surface of the needle bed 1.
The jacquard jack 4, which is arranged in part to be slidable on the arresting jack 3, is provided with a first, operating butt 19 and a second, selection butt 20. The selection butts 20 of adjacent jacquard jacks 4 are staggered in their respective positions, i.e. are arranged there with different repeating spacings from the cover strip 7.
When the carriage of the flat knitting machine, with its cams, is moved over the needle bed 1, then one cam unit 21 engages the operating butt 19 of the jacquard jack 4 and brings the jacquard jack 4 from the position shown in FIG. 1 to the position shown in FIG. 2, in which latter position the jacquard jack 4 occupies its basic position. In this position of the basic setting the jacquard jack 4 has its anterior end 23 resting directly against the arresting jack butt 17, and has its selection butt 20 brought into the selection zone in which an actuated or chosen selection key (lifting triangle) 22 (indicated in FIGS. 5 to 15 at 37, 38, 39 and 40) can strike the selection butt 20.
The position of the jacquard jack 4, as it is shown in FIG. 1, can be captured within the cam in the region of maximum withdrawal by all needle sinkers of the cam, but before the cam relinquishes this position and is brought back again to the position shown in FIG. 2, in connection with which reference is also made to FIGS. 5 to 15.
If now a flexible shank needle 2 is to be selected, then the jacquard jack 4, which has been brought by the cam unit 21 (see also FIG. 5 ) into the position shown in FIG. 2, is extended by the chosen selection key 22 (37 to 40) so far until the arresting jack butt 17 of the arresting jack 3 can be engaged by a cam unit 24 (FIG. 3). The arresting jack 3 thus chosen now has its inclined cam surface 15 confronting the needle cam surface 13. The cam unit 24 moves the arresting jack 3 further forward, and a cam unit 65 is positioned in front of the first needle butt 8 which always projects from the needle bed 1 and prevents any sliding away of the flexible shank needle 2 upon the then following coupling movement between arresting jack 3 and flexible shank needle 2. In this coupling movement the inclined cam surface 15 of the arresting jack rides on the inclined cam surface 13 of the needle, lifts the springy needle shank 10 at the second needle butt 9 and enables the arresting cam 11 to drop into the latching groove 25 FIG. 4). The second needle butt 9 emerges from the needle bed 1 and comes into the zone of the cam units shown in FIGS. 5 to 15 which move the flexible shank needles 2 for operation.
The uncoupling of the flexible shank needle 2 and the arresting jack 3 follows in the inverse manner, with a withdrawal element 26 moving the arresting jack 3 downwards (and to the left) and a cam unit 27 holding the flexible shank needle 2 fast by its first needle butt 8, so that the uncoupling can take place (FIG. 2).
A preferred embodiment of cam system which is appropriate for the aforesaid movements is shown in FIGS. 5 to 13. This cam system comprises five shiftable cam units 28,29,30,31 and 32 as well as four needle sinkers 33,34 35 and 36 which are displaceable in the plane of the cams. Lifting triangles or selection keys 37,38,39 and 40 can be brought into action or taken out of action by means of magnets for the purpose of needle selection. The remaining cam units (shown by vertical hatching) are stationary and are not shiftable. The central longitudinal axis of the system of cam units is indicated at M.
In the embodiment of cam system shown in FIGS. 5 to 13 one can knit in one row of knitting either selected stitches or tuck loops or knit with the three-path technique with selectively chosen needles and with different size stitches and tuck loops. Furthermore, with this cam system, any transfer can be made, in both directions of traverse of the carriage, to the rear needle bed or to the forward needle bed or to both needle beds at the same time.
FIG. 5 shows this preferred first embodiment of cam system with the most important reference numbers present.
FIG. 6 shows the shifting of the cam system for a carriage movement from right to left and for a needle pass and jack pass for the production of equal size stitches. The selection key 38 and the cam unit 29 are shifted into action. The needles and jacks occupy their basic positions. The second needle butt 9 remains sunk in the needle bed 1, in other words outside the relevant cam zone. The needle sinker 34 is brought to the withdrawal position and the needle sinker 35 is set manually or by stepping motors to the same withdrawal depth or to the level-cams position. Here, as in the following Figures, the coupling zone within the cam system is indicated by a and the uncoupling zone within the cam system as indicated by b.
Each arresting jack butt 17 is brought again into the initial position by a stationary cam unit 41 which moves it positively downwards and by a following stationary lifting cam unit 42 which engages against the operating butt 19 of the jacquard jack 4. These movements are required successively on account of maximum withdrawal depth and are carried out automatically in the advancing sense for these reasons.
The selection key 38 comes into action and, by means of the selection butt of the jacquard jack 4, moves the arresting jack butt 17 into the zone of a cam unit 43 in whose lifting zone 44 the coupling between the arresting jack 3 and the flexible shank needle 2 takes place, in other words in the coupling zone a. A stationary cam unit 45 holds the flexible shank needle 2 by means of its first needle butt 8 in its position, so that the needle cannot deflect upwards upon coupling. The second needle butt 9 comes into action upon coupling, and is engaged by a fixed cam unit 46 as well as by the active cam unit 29, and the flexible shank needle 2 is extended to the stitch matrix level. A fixed cam unit 47 limits the lifting of the flexible shank needle 2 upwards and, together with the needle sinker 34, complemented by the action of the needle sinker 35, guarantees in known manner the withdrawal of the needle for laying in the thread and for the formation of the stitch.
The arresting jack 3 causes the movement of the flexible shank needle 2 forcibly as far as fixed cam units 48 and 49, into the uncoupling zone b for the uncoupling of them both. By this means the cam unit 49 limits the movement of the flexible shank needle 2 downwards by engagement against the first needle butt 8, and consequently upon the downward movement of the arresting jack 3, moved by the engagement of the cam unit 48 against the arresting jack butt 17, the uncoupling can take place. Finally, the jacquard jack 4 is displaced forcibly into the initial position by engagement against its operating butt 19.
FIG. 7 shows the shifting of the cam system of FIG. 6 under the same conditions, but for equal size tuck 1oops. Here again the selection key 38 is active and the needle sinker 34 has been brought to the withdrawal position. The needle sinker 35 occupies the same setting or higher. The selection of the flexible shank needles which are to form the tuck loop is the same as has been described above with reference to FIG. 6 in connection with the formation of stitches. The cam unit 29 is not brought into action however, so that the selected flexible shank needles 2 are extended by the cam unit 46 to the tuck level and remain there until the subsequent withdrawal, with the further needle pass and jack pass being the same as described above in connection with FIG. 6.
FIG. 8 shows the embodiment according to FIG. 6 shifted to the cam setting for the three-path technique and for the production of equal size tuck loops and stitches. The cam units 29 and 32 are shifted into action. The selection keys 37 and 38 are appropriately controlled by selection magnets; selection key 37 chooses that flexible shank needle 2 which is to form the tuck loop, and selection key 38 chooses that flexible shank needle 2 which is to form the stitch. The needle sinker 34 is brought to the withdrawal position and the needle sinker 35 is brought to the same withdrawal position.
The flexible shank needles 2 forming tuck loops are coupled by fixed cam units 50 and 51 in the coupling zone a to the selected arresting jacks 3, and subsequently, by a fixed cam unit 59 engaging against the active needle butts 9, have their first needle butts 8 extended into the operating zone of a fixed cam unit 52, and are extended by this to the tuck level. Upon lifting by the cam unit 52 and by a holding of the arresting jack butt 17 against a fixed cam unit 53, the selected flexible shank needles 2 are uncoupled in the uncoupling zone b. Their second needle butts 9 disappear into the needle bed and can then no longer be engaged by the following cam units. The withdrawal of these flexible shank needles 2 selected for the formation of tuck loops then follows by means of the needle sinker cam unit 32 and the needle sinker 35.
The flexible shank needles forming stitches are chosen by the selection key 38. The further pass movement of these flexible shank needles 2 chosen for the formation of stitches corresponds to that shown in FIG. 6 and described above, with the exception that the needle withdrawal is effected by the needle sinker cam unit 32 and then first by the needle sinker 34.
If, with the cam shift according to FIG. 8 in the three-path technique, one wishes to produce knitting with small tuck loops and large stitches, then the needle sinker 34 must be deeper than the needle sinker 35. The needle butts 8 of the flexible shank needles 2 chosen for the formation of tuck loops are then withdrawn to a lesser depth, since their needle butts 9 are sunk again into the needle bed 1 and consequently cannot be engaged by the needle sinker 34. The flexible shank needles 2 chosen for the formation of stitches are withdrawn deeper by the needle sinker 34 by way of their high-standing needle butts 9. Their needle butts 8 can be affected by the needle sinker 35 only up to withdrawal to the lesser depth.
FIG. 9 shows the cam shift of the cam system shown in FIGS. 5 to 8 for carriage movement from right to left for the donation of stitches in the stitch transfer process. The selection key 37 and the needle sinker cam unit 32 are shifted into action. The needle sinkers 33 and 36 are displaced downwardly in the plane of the cam unit sufficiently far that the needle butts 9 of the flexible shank needles 2 selected for the donation are engaged by the needle sinker 33 in the advancing sense and the needle butts 8 of the flexible shank needles 2 which are not selected cannot be engaged by the needle sinker 36 and consequently the unselected flexible shank needles 2 run through the cam unit in the level-cams position without being lifted or withdrawn. The first needle butts 8 of the flexible shank needles 2 selected for the donation, which have been extended by the needle sinker 33 in the advancing sense and which have been brought into the zone of a fixed donor cam unit 54, are extended in known manner for the donation by this donor cam unit 54 and subsequently are withdrawn to the level-cams position by a fixed withdrawal cam unit 55 and a fixed donor cam unit 56 as well as by the active needle sinker cam unit 32. The needle sinkers 34 and 35 stay at the level-cams position or, if necessary, somewhat deeper.
FIG. 10 shows the cam shift of the cam system of FIGS. 5 to 9 into the setting for acceptance of stitches with a carriage traverse from right to left. The selection key 38 is active. In the transfer from front needle bed to rear needle bed, the needle sinker cam unit 32 can be brought into action. With transfer from rear needle bed to front needle bed, or with a transfer in both directions at the same time, the needle sinker cam unit 32 must in general be put into action since after the donation of the stitch the needle must either be withdrawn at the same time or the donor needle must be withdrawn earlier than the accepting needle.
This is dependent however on which positions the needles occupy in the front needle bed and in the rear needle bed for the transfer operation, i.e. the needles in the front needle bed slide past the needles in the rear needle bed to the left or to the right. The needle pass movement and jack pass movement effected by the cams is, in its essential parts, the same as described above in connection with FIG. 7.
FIG. 11 shows the cam shift of a cam system according to FIGS. 5 to 10 for the formation of large and small stitches during a traverse of the carriage from right to left. Cam shift and needle and jack pass movements are essentially the same as described above in connection with FIG. 8, and the formation of large stitches and small tuck loops is as described above, with the difference that the cam unit 30 is additionally shifted into action. The flexible shank needles chosen by the selector key 37 are then likewise extended to stitch level.
FIG. 12 shows the cam shift of a cam system according to FIGS. 5 to 11 with traverse of the carriage from right to left for the formation of small and large tuck loops. The cam shift and the needle and jack pass movements are the same as in connection with FIG. 8 for the formation of small tuck loops and large stitches, with the difference that the cam unit 29 is here inactive. The flexible shank needles 2 chosen by the selection key 38 are then likewise extended only to tuck level.
FIG. 13 shows the cam shift of a cam system according to FIGS. 5 to 12 for the three-path technique and for the formation of small stitches and large tuck loops with traverse of the carriage from right to left. Cam shift and needle and jack pass movements are the same as described above in connection with FIG. 12, with the difference that the cam unit 31 is shifted into action and consequently the flexible shank needles 2, which have been chosen by selection key 37 and which have been uncoupled again in the uncoupling zone b by the cam units 52 and 53, are extended by way of their needle butts 8 to matrix level.
The following selective needle and jack pass movements are possible with the cam system described with reference to FIGS. 5 to 13;
(a) Formation of equal size stitches, FIG. 6,
(b) Formation of equal size tuck loops, FIG. 7,
(c) Three-path technique, formation of equal size tuck loops and stitches, FIG. 8.
(d) Three-path technique, formation of small tuck loops and large stitches, FIG. 8 modified,
(e) Donation of stitches, FIG. 9,
(f) Acceptance of stitches, FIG. 10,
(g) Formation of small and large stitches, FIG. 11,
(h) Formation of small and large tuck loops, FIG. 12, and,
(i) Three-path technique, formation of small stitches and large tuck loops, FIG. 13.
FIG. 14 shows a simplified embodiment of a cam system by means of which no selective differential needle withdrawal can be achieved. In this embodiment the shiftable cam units 30 and 31 as well as the needle sinkers 35 and 36 are absent, while fixed cam units 57 and 58 are added. The shiftable needle sinker cam unit 32 is only required for the transfer process. For the rest, the needle and jack pass movements correspond to those of FIGS. 6, 7, 9 and 10.
FIG. 15 shows a further embodiment of a cam system. In this cam system the shiftable needle sinker cam unit 32 is absent. The displaceable needle sinkers 35 and 36 are retractable, for example by being arranged pivotably. With the needle and jack pass movements according to FIGS. 6 and 7, the needle sinker 35 is inactive, and with the needle and jack pass movements of FIGS. 8,9,10,11,12 and 13 the needle sinker 35 is active. For the rest, similar needle and jack pass movements can be effected as the needle and jack pass movements effected according to FIGS. 6 to 13.
Generally speaking, in order to achieve a higher knitting output, a plurality of cam systems can be arranged next to one another.
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A flat knitting machine comprises flexible shank needles arranged in the dle channels of the needle bed, and, arranged behind these, jacquard jacks as well as a cam system which is movable over the needle bed and which comprises interengageable needle, jacquard and selection cam units which have fixed and shiftable cam elements. In order to create the possibility of selection for the flexible shank needles with sinkable needle butts, and in which the needle channel cutting is without interruption, i.e. can be produced with constant depth by one cutting pass, the flexible shank needles have an anterior first needle butt always projecting from the needle bed and a posterior second needle butt which sinks into the needle bed under the resilience of its own flexible shank. Behind each flexible shank needle there is provided a displaceable arresting jack having an arresting jack butt as well as a coupling portion at its forward end for coupling to the flexible shank of the flexible shank needle and for simultaneously lifting the second needle butt from the needle bed. Behind the arresting jack there is displaceably mounted a jacquard jack which has a first, operating butt and a second, selection butt. In the needle cam unit, at least in the region of the second needle butt, and symmetrically arranged with respect to the central longitudinal axis of the cam system, there are provided two needle sinkers displaceable in the plane of the cam system and two cam units shiftable into and out of the plane of the cam system for extending the needles in the formation of stitches.
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FIELD OF THE INVENTION
[0001] The present invention relates to human physiology, and in particular to a method and system of biofeedback allowing a human subject to consciously control physiological processes, more particularly, it allows a human subject to achieve synchronization of one's breathing cycle with one's natural heart rate cycle.
BACKGROUND OF THE INVENTION
[0002] The human heart is known to have its own nervous system and its own natural tendency toward rhythm. For purposes of this invention, there are two primary aspects to this rhythm, the heartbeat rate, and the rate at which the heartbeat rate changes otherwise known as heart rate variability. Heartbeat rate is usually specified in absolute number of heartbeats occurring during a specified period. Heartbeat rate variability, otherwise know as heart rate variability is the change in heartbeat rate as occurs during a specified period. Henceforth, heartbeat rate variability will be referred to as heart rate variability.
[0003] While the heart has its own tendency toward rhythm, it is closely coupled to breathing. The relationship is such that as inhalation occurs, the heartbeat rate tends to increase and as exhalation occurs, the heartbeat rate tends to decrease. It is important to note that while the heartbeat rate and breathing rate influence each other, the relationship is an asynchronous one, that is, they are independent rhythms that influence but do not directly control each other.
[0004] It is generally recognized that heart rate variability is an indicator of physiological and emotional state, that is, irregular incoherent heart rate variability indicates a condition of physiological/psychological stress. Alternatively, highly coherent heart rate variability is indicative of a condition of physiological/psychological harmony.
[0005] Accordingly, it is highly desirable to achieve and maintain a highly coherent heart rate variability as life circumstances permit. This having been said, with proper training and the application of the method and apparatus of the present invention, it is possible for a human subject to rapidly achieve the desired state of high coherence of heart rate variability and to monitor and reinforce the accuracy and performance of said coherence on an ongoing basis.
[0006] The present invention takes advantage of the relationship between the breathing cycle and the natural heart rate variability cycle to bring heart rate variability to the desired state of coherence and the human subject to the resultant state of physiological and emotional harmony. It accomplishes this via conscious synchronization of the breathing cycle with the natural heart rate variability cycle.
SUMMARY OF THE INVENTION
[0007] As previously described, a relationship exists between the heartbeat rate specified in terms of heart rate variability, and the breathing cycle. While the heart has its own tendency toward a natural variable rhythm, there is a strong correlation with breathing according to this specific relationship: as inhalation occurs, there is a tendency for the heartbeat rate to increase, as exhalation occurs, there is a tendency for the heartbeat rate to decrease. It is important to note that the relationship between the natural heart rate variability cycle and the breathing cycle is indirect. This is to say that while the heart rate variability cycle/breathing cycle relationship exists, in untrained subjects, their alignment appears highly random. Consequently, these same subjects exhibit a highly incoherent heart rate variability pattern. As previously stated, maximal coherence of the heart rate variability is achieved when the cycle of breathing is synchronized with the natural heart variability cycle in time and amplitude. The most direct and effective manner of achieving this alignment is for the human subject to consciously align them via biofeedback, i.e., present the human subject with a biofeedback signal that indicates exactly when to inhale and exactly when to exhale such that the breathing cycle achieves exacting alignment with the natural heart rate variability cycle. The present invention achieves this by asserting a biofeedback signal to exhale just after the peak positive heartbeat rate has been reached and a biofeedback signal to inhale just after the peak negative heartbeat rate has been reached. Closely aligning the natural heart rate peaks with breathing peaks is critical to achieving an overall synchronization and resulting high degree of coherence of the heart rate variability pattern.
[0008] For purposes of the present invention, we can consider the cycles of heart rate variability, the periodicity of increasing and decreasing of heartbeat rate, and the breathing cycle, the periodicity of inhalation and exhalation, to be two independent cycles as depicted in FIG. 1 . The relative synchronization of these cycles can vary between 0 and 180 degrees. When these cycles are completely out of phase, heart rate variability is maximally incoherent, when these cycles are completely in phase heart rate variability is maximally coherent.
[0009] The invention defines the system and method of the application of biofeedback for purposes of providing a human subject the ability to consciously control their inhalation and exhalation so as to achieve the desired coherence of heart rate variability. A present objective is to achieve maximal alignment. As this is an emerging field of inquiry, it is entirely likely that applications of value will be found for other alignments, for example maximal misalignment, 45 degree out of phase, etc. It is understood that these alternative alignments are also within the scope of the present invention.
[0010] Because the heart rate variability signal of the untrained subject is typically highly erratic and synchrony of said signal may be difficult to detect, a specific instructive method employing other biofeedback devices and methods is specified. Via the application of this instructive method, the human subject is led to achieve a detectable level of synchrony of their heart rate variability signal. Once detected, the present invention can be readily used to achieve optimal alignment of the subject's breathing cycle with their natural heart rate variability cycle.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
[0011] The accompanying drawing figures incorporated in and forming a part of this specification illustrate several aspects of the invention, and together with the description serve to explain the principles of the invention.
[0012] FIG. 1 depicts the relative relationship between the natural heart rate cycle and breathing cycle.
[0013] FIG. 2 depicts the natural heart rate cycle and breathing cycle moving from misalignment to alignment and resultant heart rate variability pattern.
[0014] FIG. 3 depicts a primary example of the moment of biofeedback signal generation according to a preferred embodiment of the present invention.
[0015] FIG. 4 depicts specific criterion for biofeedback signal generation associated with the primary example of the moment of biofeedback signal generation of FIG. 3 .
[0016] FIG. 5 depicts the physical system of the preferred embodiment of the present invention.
[0017] FIG. 6 depicts the algorithm for the preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0018] The embodiments set forth below represent the necessary information to enable those skilled in the art to practice the invention and illustrate the best mode of practicing the invention. Upon reading the following description in light of the accompanying drawing figures, those skilled in the art will understand the concepts of the invention and will recognize applications of these concepts not particularly addressed herein. It should be understood that these concepts and applications fall within the scope of the disclosure and the accompanying claims.
[0019] The present invention allows a human subject to achieve maximal regularity and coherence of heart rate variability by synchronizing the breathing cycle with the natural heart rate variability cycle. This is accomplished by providing a biofeedback signal in the form of an audible, visual, or sensory stimulus, to indicate when the subject should begin inhalation and a second signal to indicate when the subject should begin exhalation. These signals are unique so the subject is able to clearly distinguish the beginning of inhalation from the beginning of exhalation.
[0020] With reference to FIG. 1 , the heart has its own nervous system and a tendency toward its own natural rhythm. FIG. 1 depicts the heart rate variability cycle, 101 , and the breathing cycle, 102 . The positive peak of the heart rate variability cycle, 103 , indicates peak positive heart rate or the maximum number of heart beats per minute. For the purposes of discussion the peak positive rhythm is defined as 80 beat per minute (BPM). The negative peak of the heart rate variability cycle, 104 , indicates peak negative heart rate or the minimum number of heart beats per minute. For the purposes of discussion the peak positive rhythm is defined as 50 beat per minute (BPM). Let it be clear that 80 beats per minute as the positive peak and 50 beats per minute as the negative peak are merely used for purposes of example. The breath is under control of the human central nervous system and operates with a largely independent rhythm. Yet, there is a strong correlation between the breath cycle and the natural heart rate variability cycle as described prior.
[0021] FIG. 2 depicts the breathing cycle 201 and the natural heart rate cycle 202 moving from misalignment to alignment and the resultant heart rate variability cycle 203 moving from incoherence 204 to coherence 205 . The synchrony between the natural heart rate variability cycle and the cycle of breathing is highly variable ranging from being highly synchronous (in-phase) to being highly asynchronous (out of phase). This results in a highly periodic and coherent heart rate variability pattern 205 vs. a highly aperiodic and incoherent heart rate variability pattern 204 , respectively. A primary yet not limiting application of the present invention is to lead a human subject to the preferred state of highly periodic and coherent heart rate variability both in time and amplitude.
[0022] FIG. 3 , depicts the natural heart rate cycle and the moments of biofeedback signal generation indicating exhalation 301 and inhalation 302 . The desired state of highly periodic and coherent heart rate variability is brought about by aligning the cycle of breathing with the natural heart rate cycle. This is accomplished by monitoring the heart rate signal and providing biofeedback to the human subject so as to allow the subject to synchronize their inhalation and exhalation so as to be in phase with their heart rate pattern. This requires that the human subject begin inhaling as the natural heart rate signal begins increasing from its negative peak, and conversely, to begin exhaling as the natural heart rate begins decreasing from its positive peak.
[0023] It should be noted that for purposes of biofeedback generation, the exact moment of alerting occurs slightly after the positive and negative peaks are reached. This will be explained in greater detail below.
[0024] It must be further explained that while FIG. 3 depicts the primary application of the present invention, that being the maximal alignment of the heart rate variability cycle and the breathing cycle, all other alignments are also provided for and are within the scope of the present invention.
[0025] FIG. 4 depicts the exacting means of identifying positive and negative heart rate peaks. With reference to FIG. 4 , in order to achieve maximal desired effect, it is necessary to achieve a very exacting timing. Here it is important to point out that via biofeedback, the human subject is trained to identify the subjective state and associated sensation that relates to maximal alignment. If the human subject begins either inhaling or exhaling just slightly before the natural heart rate begins to increase or decrease respectively, the periodicity and coherence of the resulting heart rate variability pattern is significantly degraded. This suboptimal coherence of heart rate variability can be consciously perceived by the practitioner. To address this matter of accuracy, in this example, the “exhale” biofeedback signal is generated just after the positive peak, in this case 80 beats per minute (BPM), when the signal drops to 79 beats per minute (BPM) 401 . Likewise, the “inhale” biofeedback signal is generated just after the negative peak, in this case 50 beats per minute (BPM), when the signal increases to 51 beats per minute (BPM) 402 . Because, in order to achieve the desired maximal effect this timing must be exacting, the present invention allows for the exact moment of biofeedback to be adjusted so that timing may be optimized on a personal basis. This would allow for slightly differing physiologies if such differences are found to exist. Programmability of biofeedback signal generation is also provided to accommodate other useful alignments of the natural heart rate cycle and breathing cycle should such useful alignments be found to exist With reference to FIG. 5 , the primary physical system of the preferred embodiment of the present invention is quite simple consisting of a human subject 500 , a pulse sensor of adequate accuracy 502 , a pulse monitor of adequate accuracy 504 , a positive and negative peak rate detector 507 , a function for setting feedback criterion and comparing it 509 , and a function for generating feedback signals to the human subject 512 .
[0026] A detailed discussion of the physical system will now ensue. Human subject 500 is outfitted with a pulse sensor 502 of any adequately accurate variety, via connection 501 . Sensor 502 and associated connection 501 may be of any adequately accurate type including electronic, pneumatic, acoustic, etc. The sensor may be any style of device such as a wristband, a finger cradle, an ear clip, etc. The only requirement is that it be able to accurately sense and transmit individual heart beat pulses to pulse monitor 504 via connection 503 . Connection 503 may also be of any adequately performing type including electronic, pneumatic, acoustic, optical, radio frequency, etc. Pulse monitor 504 monitors real time rate and count. Heartbeat count is used as an alternative means of feedback for purposes of allowing the human subject to synchronize their breathing based on heartbeat count as opposed to a predetermined threshold. For example, instead of using the inhale/exhale signal as the basis of controlling the breathing cycle, a human subject may desire to count 1-2-3-4-5-6-begin exhaling-1-2-3-4-5-begin inhaling, etc. Pulse monitor 504 sends this information to positive and negative peak rate detector 507 via connector 505 and to feedback and criteria settings and comparator 509 . Positive and negative peak rate detector 507 detects when peak pulse rate occurs, and signals to feedback criteria settings and comparator 509 via connector 508 that, a) peak pulse rate has occurred and b) the value of the peak pulse rate. Based on the receipt of the peak pulse rate signal via connector 508 , criteria settings and comparator 509 , begins comparing peak pulse rate vs. present pulse rate against previously established settings to determine the moment when the biofeedback signal associated with the positive peak or negative peak should be asserted to audible, visual, or sensory stimulus function 512 , via connectors 510 and 511 , 510 relating to positive peak and 511 relating to negative peak. Upon receipt of positive peak signal via connector 510 , audible, visual, or sensory stimulus generator 512 , generates a biofeedback signal to human subject 500 via positive peak connector 514 indicating exhale. Likewise, upon receipt of negative peak signal via connector 511 , audible, visual, or sensory stimulus generator 512 , generates a biofeedback signal to human subject 500 via negative peak connector 513 indicating “inhale”. This system applies to any adequately accurrate analog or digital method of sensing, measuring, decision making, and feedback generation. Programmability of biofeedback signal generation occurs on the basis of peak positive and peak negative heart beat rates and on the basis of peak positive and peak negative heart beat rates plus respective offsets. Programmable offsets are provided on the basis of the present heart beat rate as a percentage of the peak heart beat rate, on the basis of the present heart beat rate vs. peak heart beat rate, on the basis of the absolute number of heart beats since peak heart beat rate, and on the basis of individual heart beats. Unique programmability applies to positive negative peaks, that is, to exhalation and inhalation phases, respectively.
[0027] With reference to FIG. 6 , for clarity, the algorithm of the preferred embodiment of the present invention shall now be discussed. The heartbeat rate of a human subject 600 is sensed via sensor 602 via connector 601 . Sensor 602 detects the heartbeat rate and transmits its analog or digital equivalent with adequate accuracy to monitor 604 via connector 603 . Monitor 604 derives the real time heartbeat rate, heartbeat count, and transmits its analog or digital equivalent to peak rate detector 607 and settings and comparator function 611 via connectors 605 and 606 respectively. Peak rate detector 607 determines the exact moment of peak rate by analyzing the present rate for maximum positive rate minus 1 heart beat per minute (BPM) and maximum negative rate plus 1 heart beat per minute (BPM) for positive and negative peaks respectively. At the moment of detection, peak rate detector 607 sends the rate 608 and a flag 609 to the settings and comparator function 612 . Upon receipt of the flag 609 , the settings and comparator function 612 begins comparing manual settings 610 via 611 with the peak rate 608 vs. present rate 606 . When the threshold is achieved, settings and comparator function 612 sends a positive peak threshold signal 613 or a negative peak threshold signal 614 to audible, visual, or sensory stimulus generator 615 . This threshold is totally programmable and may be programmed in: a) number of heartbeats or, b) percent of peak rate. Upon receipt, audible, visual, or sensor stimulus generator 615 generates a signal to exhale 617 or signal to inhale 616 respectively. This programmability is provided for both positive and negative peaks. This is to say, that offsets associated with the positive peak and with beginning exhalation and offsets associated with the negative peak and with the beginning of inhalation are individually programmable. For example, the offset associated with the positive peak may be “zero” and the offset associated with the negative peak may be 10%.
[0000] Instructive Method:
[0028] Typically, the heart rate variability pattern of the untrained subject is highly irregular and may resemble random noise. For this reason, it may be difficult to detect the moments of peak positive and peak negative heart rate with a regularity that can be discerned and employed by the human subject Therefore, the present instructive method is specified to bring a human subject to an initial physiological/psychological state such that the present invention may be employed effectively.
[0029] The heart rate variability signal is generally considered to represent the relative balance of sympathetic and parasympathetic nervous systems. For this reason, the heart rate variability pattern is highly indicative of the psycho-physiological state of the human subject with this general relationship: anxiety and tension result in incoherence of the heart rate variability pattern, harmony and calm result in coherence of the heart rate variability pattern. It is often necessary for an untrained human subject to reduce their level of anxiety and tension before an adequately coherent heart rate variability pattern can be detected and used effectively for specifying when to inhale and when to exhale. This tension and anxiety is most easily assessed and reduced via application of electromyographic (EMG) and electroencephalographic (EEG) biofeedback methods and apparatus as tension and anxiety follow this general relationship with EMG and EEG:
[0030] EMG: as tension and anxiety increase, muscle activation increases with a resultant increase in measured voltage.
[0031] EEG: as tension and anxiety increase, brainwaves in the high beta bands (frequencies between 19 Hertz and 33 Hertz) increase in amplitude.
[0032] Therefore, to bring the human subject to an adequate state of coherence of the heart rate variability pattern, the following steps are specified:
[0033] Step 1: The human subject is asked to position themselves comfortably in a chair in an upright posture. The apparatus of the present invention is connected to the subject and the coherence of the heart rate variability signal or lack thereof is established. If the signal is not adequately coherent to effectively detect positive and negative heart rate peaks, an electromyographic measurement device is placed on the skin just over the major muscle of the jaw on either side of the face in the general vicinity of the superficial portion of the masseter muscle. The electrical signal resulting from this tension is presented to the subject using electromyographic apparatus. The subject is requested to consciously relax this area as deeply as possible. After the subject has demonstrated the ability to reduce the tension in this area to an acceptable level, the present invention is once again applied and coherence of the heart rate variability is once again assessed. If adequate coherence is detected, the human subject is asked to spend some time consciously examining the relationship between tension in the area of the masseter muscle and the coherence of their heart rate variability signal as indicated by the regularity of biofeedback indications to inhale and exhale. If adequate coherence is detected, the subject is asked to begin following biofeedback cues to inhale and exhale accordingly.
[0034] Step 2: If an acceptable EMG signal is achieved during the prior step but an adequately coherent heart rate variability is still not detected, an electroencephalograph is employed using conventional electrode placement. The subject's high beta brainwave bands are monitored, and feedback is provided. The subject is first asked to consciously lower the amplitude of high beta frequencies centered around 26 Hertz. This process is aided via helpful suggestions by the practitioner. When the subject has achieved an adequately low amplitude in this frequency band, the apparatus of the present invention is applied and the coherence of the heart rate variability signal is assessed. If adequate coherence is detected, the subject is requested to examine the relationship between their beta amplitude and their heart rate variability signal. If adequate coherence is detected, the subject is requested to begin following biofeedback cues to inhale and exhale accordingly.
[0035] Step 3: If an acceptable EEG in the 26 Hertz band is achieved but an adequately coherent heart rate variability is still not detected, the same process is repeated for the next lower beta band centered around 20 Hertz.
[0036] Step 4: By the end of this process, the subject will most likely achieve adequate coherence of heart rate variability as detected by the apparatus of the present invention. Once this is achieved, the subject is requested to begin following biofeedback cues to inhale and exhale accordingly.
[0037] Once the human subject has become proficient in establishing and maintaining the desired coherence of heart rate variability, in principle, the apparatus may be utilized whenever and wherever the subject desires. It is assumed that the apparatus is fully capable and of a size making it fully portable.
[0038] Given that this is an emerging field of investigation, it is highly likely that it will be found that other physiological and psychological functions can be enhanced by synchronizing them with this fundamental bio-resonance. For example, synchronization of running, walking, cycling, talking, exercising, thinking, meditating, etc. Those skilled in the art will recognize improvements and modifications to the preferred embodiments of the present invention. All such improvements and modifications are considered within the scope of the concepts disclosed herein and the claims that follow.
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The present invention provides a biofeedback system and method for the purpose of allowing a human subject to consciously synchronize one's rhythm of breathing with one's natural heart rhythm for purposes of maximizing coherence of one's heart rate variability pattern and consequent enhancement of physiological/psychological well being. It accomplishes this by facilitating a biofeedback signal that indicates to the human subject precisely when to inhale and exhale such that the breathing cycle will achieve a high degree of alignment with the natural heart rate cycle. It also specifies an instructive method for bringing a human subject to an adequately coherent heart rate variability pattern such that the preferred embodiment of the invention can be applied.
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This application is a 371 of PCT/US99/16409 filed Jul. 21, 1999 which is a CIP of U.S. Ser. No. 09/127,051 filed Jul. 31, 1998 now abandoned.
FIELD OF INVENTION
The present invention relates to fusion products prepared by recombinant DNA procedures. The products are comprised of a soluble protein of interest and an insoluble proteinaceous tag. More particularly, the invention relates to the separation of such products from a cellular host in which the products have been expressed by utilization of the insolubility of the tag.
BACKGROUND OF THE INVENTION
Fusion techniques are popular for the preparation and recovery of recombinantly produced proteins of interest which are soluble in the host cell in which they are expressed. The proteins, which term herein also includes peptides, are of interest for research, diagnostic, or pharmaceutical use because of actual or supposed biological activity.
Preparation of fusion products involves ligating a fragment containing the DNA sequence coding for the protein of interest and a fragment containing the DNA sequence coding for a second protein commonly termed the “tag” into a vector. The vector is then introduced into a host cell, such as an insect cell, and the fusion product (protein of interest fused to the tag) is expressed. After expression, the cell is lysed thereby releasing the fusion product and other cellular proteins into the lysate solution. The fusion product is then separated from the lysate solution and subjected to further manipulation which can include cleavage and separation of the protein of interest from the tag.
A function of the tag in a fusion technique as above set forth is to facilitate separation of the fusion product from the host cell lysate solution. Separation techniques based on the well known principals of chromatography, in particular affinity chromatography, have commonly been employed; with affinity chromatography the tag functioning as a receptor having specific attraction for a ligand which typically is immobilized on a solid matrix. Contacting the lysate solution containing the fusion product with the solid matrix results in selective adsorption of the product onto the matrix. After washing the matrix to remove non-binding substances, the fusion product can be recovered by various elution techniques such as those based on pH, ionic strength or ligand competition.
Descriptions of the preparation of fusion products and the recovery and separation thereof by chromatographic techniques from host cell lysate solution are illustrated in the following U.S. patents and other publications, the disclosures of which are hereby incorporated by reference: 5,643,758; 5,654,176; 5,179,007; 4,879,236, 4,745,051, Biochem. J. (1986) 240, 1-12, Methods in Enzymology, Vol. 182, Guide to Protein Purification, and Methods in Molecular Biology, Vol. 59, Protein Purification Protocols. U.S. Pat. No. 5,496,934 is also so referenced as illustrating an affinity separation procedure where the tag (cellulose binding domain) binds directly to the matrix (cellulose), thus avoiding the use of a separate ligand bound to a matrix.
A problem associated with chromatographic techniques for the separation of fusion products from their cellular lysate solutions is that they are time consuming, involving as they do multiple steps including binding to a matrix, washing to remove non-specifically bound cellular components and subsequent elution. Also, the degree of binding of the fusion product to a matrix can be interfered with by various factors such as pH, ion concentration detergents and the like which can reduce the yield of fusion product.
SUMMARY OF THE INVENTION
One aspect of the present invention provides an improvement in those recognized processes for the preparation of a recombinantly expressed fusion product comprised of a proteinaceous tag and a soluble protein of interest and the subsequent separation of the fusion product from the host cell in which it is expressed. The process to which the improvement described herein pertains involves (1) preparing a vector containing the DNA sequence coding for the protein of interest and the DNA sequence coding for the tag, (2) introducing the vector into a host cell and expressing the fusion product, (3) lysing the host cell to liberate cellular proteins and then (4) utilizing the characteristics of the tag to separate the fusion product from the lysate solution. The improvement to this process provided by the present invention is the use, as the tag, of a protein which is insoluble in a normal lysate solution, which typically is at a pH of about 7-8. Accordingly, the fusion product containing the tag precipitates from the lysate solution and the precipitated fusion product can then be separated from the lysate solution by centrifugation or filtration.
Advantages accompanying the use of the process described herein include the fact that the separation of fusion product from lysate solution is a simple, one-step centrifugation or filtration procedure and that the expressed fusion product can be recovered in high yield from the host cell. An additional and particularly surprising advantage of the present process is that the level of expression or the fusion product in the host cell is increased above what would normally be expected.
An additional aspect of the present invention resides in providing a new and improved vector useful in practicing the foregoing process. Yet a further feature of this invention is to provide a recombinantly expressed fusion product comprised of a soluble protein of interest and an insoluble proteinaceous tag, the insolubility of the tag permitting the fusion product to precipitate from the host cell in which it is expressed.
A still further aspect of this invention resides in providing a easy process for cleaving the fusion product to separate the tag from the protein of interest and the subsequent recovery of the protein. In this respect, after the insoluble, precipitated fusion product is centrifuged or filtered from the lysate solution, it is dissolved in an aqueous medium at a basic pH of about 9-11, thus solubilizing the product. The tag can then be released from the protein of interest by cleaving with a site specific protease such as enterokinase. The pH of the solution containing the tag and protein is then reduced to about 7-8 by addition of an acidic buffer, thus causing precipitation of the tag which can then again be removed from solution by centrifugation or filtration; the protein of interest remaining in solution.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 . schematically represents three types of separation techniques for fusion products containing soluble proteins of interest (depicted by the fish) and a tag. The Type I system embodies most of the existing separation systems for such fusion products. An affinity ligand is immobilized on a matrix such as agarose to separate the product from solution utilizing, as a tag, an entity having specific affinity for the ligand. The Type II system uses cellulose to separate a fusion product containing as the tag, cellulose binding domain (CBD). The Type III system illustrates the present invention and uses an insoluble protein tag (IPT) to separate the fusion product from soluble cellular proteins.
FIG. 2 . schematically represents the construction of a vector, designated pUSE, which carries the coding for the insoluble protein tag, uricase (IPTu), which is illustrative of a tag useful in practicing the present invention.
FIG. 3 schematically represents the construction of the vector, designated pHD, which carries the coding for the insoluble tag, baculovirus polyhedrin (IPTp), which is illustrative of another tag useful in practicing the present invention.
FIG. 4 schematically represents the construction of expression vectors for fusion products containing, as the protein of interest, the nuclear hormone receptor, rat peroxisome proliferator-activated receptor (PPAR), and the tags identified in FIGS. 2 and 3. PPAR is an important transcription factor which regulates gene expression in mammalian cells.
FIG. 5 represents SDS-PAGE analysis of the expression of the insoluble protein tags IPTu and IPTp alone and with their soluble fusion partner PPAR in insect Sf9 cells infected with recombinant baculoviruses generated from pUSE, pUSE-PPAR, pHD, pHD-PPAR, and pVL1392-PPAR, respectively. pVL1392 is a baculovirus transfer vector uniformly used in the preparation of the IPT vectors described herein. The pVL1392-PPAR vector functions as a control in indicating efficiency of protein expression.
FIG. 6 represents an SDS-PAGE analysis of a one-step procedure for purification of PPAR fused to IPTu or IPTp tags. Uricase (IPTu, panel A) and polyhedrin (IPTp, panel B) alone or fused to PPAR were expressed in insect cells and purified by a one-step “spin-down” procedure. Lanes: T, total cell lysates; S, supernatant; W, washed supernatant; P, pellets; M, molecular weight standard.
FIG. 7 . represents in bar graph form the detection of fusion protein by measuring uricase activity. IPTu-PPAR fusion protein from different purification steps was incubated with uric acid substrate in 0.1 M glycine (pH9.4) for 1 hour at 37° C. After incubation, OD 295 was measured using a spectrophotometer. The legend represents the following: T, total cell lysates; S, supernatant; W, washed supernatant; P, pellets.
FIG. 8 illustrates the similarity of the amino acid sequences of uricase (SEQ ID NO:10) and polyhedrin (SEQ ID NO:9) accomplished using the MACVECTOR program from Oxford Molecular Group.
FIG. 9 illustrates the comparison of hydrophilicity between uricase and polyhedrin, again accomplished using the MACVECTOR program from Oxford Molecular Group.
DESCRIPTION OF THE INVENTION
Turning to the drawings, FIG. 2 illustrates the preparation of the vector pUSE by the technique of first cloning a uricase coding fragment in a baculovirus transfer vector pVL1392. Extra linker sequences between BglII and EcoRI were removed resulting in a modified plasmid pVL1392-UOX′. The uricase coding sequences together with baculovirus polyhedrin promoter sequences were then amplified by PCR. The amplified fragment was cloned into pGEM-T vector, and sequenced. The fragment was then cloned into the EcoRV and XhoI site of pAcSG2 plasmid to produce the pUSE vector.
Turning to FIG. 3, the construction of the pHD vector is illustrated. The polyhedrin coding sequences together with the polyhedrin promoter sequences were amplified by PCR from wild type AcNPV viral DNA. The amplified fragment was cloned into pGEM-T vector, and sequenced to confirm the authenticity. The fragment was then cloned into the EcoRV and XhoI site of pAcSG2 plasmid to produce the pHD vector.
The following Example I illustrates in more detail the preparation of the vectors which carry the DNA sequence for the insoluble tags, IPTu and IPTp, illustrated in FIGS. 1 and 2.
EXAMPLE I
Preparation of the vector, pUSE: The cDNA fragment coding for rat uricase was obtained by amplifying a rat liver cDNA library (CLONTECH Laboratory, Inc.) using a pair of primers consisting of sequences of GAA TTC CAT TCT TGA AAC CGA ATC TGA (SEQ ID NO:1) and CGG ATC CTA AAG ACA GAG TCT (SEQ ID NO:2) according to GenBank Database M24396 (Alvares et al. 1989). The amplification was performed by adding 1 ul of the cDNA library stock into 49 ul of H 2 O containing 50 pmol of each primer and further mixed with 50 ul of PCR master (BOEHRINGER MANNHEIM). The reaction was heated at 95° C. for 2 minutes, and followed by incubations at 60° C. for 1 minute, 68° C. for 1 minute, 95° C. for 30 seconds for a total of 30 cycles. At the end of amplification, the reaction was incubated at 68° C. for an additional 10 minutes, the amplified product was analyzed by electrophoresis on a 1% agarose gel.
A 1.3 kb fragment coding for rat uricase was recovered from the gel and subcloned into a pGEM-T vector using the pGEM-T cloning kit from Promega Corporation. The sequence of the insert was confirmed as rat uricase by DNA sequencing analysis provided by Ana-Gen Technologies Inc. The fragment cloned in pGEM-T vector was further subcloned into a baculovirus transfer vector pVL1392 (PharMingen) between EcoRI and BamHI sites. The resulting plasmid is named as pVL1392-UOX (see FIG. 2 ).
Subsequently for more convenient operation, the sequences between BglII and EcoRI sites in the vector were removed by double digestion, filling, and relegation. The resulting plasmid, PVL1392-UOX′, was used for further PCR amplification using a pair of primers (ACT AAT ATC ACA AAC TGG AAA TGT CTA TCA ATA (SEQ ID NO:3) and GAA TTC CTC GAG CTT ATC GTC ATC GTC GTG ATG GTG ATG GTG ATG CAG CCT GGA AGG CAG CTT CCT CCT CAC CGT CCC (SEQ ID NO:4)) to insert a six Histidine tag and an enterokinase recognition site.
The PCR amplified fragment was first cloned into pGEM-T vector, and verified by restriction digestion and sequencing (service provided Ana-gene Technology, INC.). The fragment was then released from the pGEM-T vector by digestion with EcoRV and XhoI, and inserted into the same sites of pAcSG2, a baculovirus transfer vector from Pharmingen. The final plasmid was characterized by restriction enzyme digestion as pUSE.
Preparation of the vector, pHD: Construction of this insoluble protein tag vector was accomplished using a procedure similar to that for pUSE. Wild type Baculovirus AcNPV C2 DNA (from PharMingen) was amplified using a pair of primers (ACT AAT ATC ACA TGG AAA TGT CTA TCA ATA (SEQ ID NO:5) and GAA TTC CTC GAG CTT ATC GTC ATC GTC GTG ATG GTG ATG GTG ATG ATA CGC CGG ACC AGT GAA CAG AGG TGC GTC TGG (SEQ ID NO:6)) according to GenBank database M25054. The amplification was performed by adding 0.1 μg of the Baculovirus DNA in 50 ul of H 2 0 containing 50 pmol of each primer and further mixed with 50 ul of PCR master (BOEHRINGER MANNHEIM). The reaction was heated at 95° C. for 2 minutes, and followed by incubations at 60° C. for 1 minute, 68° C. for 1 minute, 95° C. for 30 seconds for a total of 30 cycles. The PCR amplified fragment was first cloned into pGEM-T vector, and verified by restriction digestion and sequencing (service provided Ana-gene Technology, INC.). The EcoRV and XhoI fragment was then released from the pGEM-T vector, and inserted into pAcSG2, a Baculovirus transfer vector from Pharmingen. The final plasmid was characterized by restriction enzyme digestion as pHD.
Turning again to the drawings, FIG. 4 illustrates the use of the insoluble tag plasmids prepared above for the construction of transfer vectors which contain coding sequences for the tags and the protein of interest, rat peroxisome proliferator-activated receptor (PPAR). As shown, the fragment coding for the PPAR was first cloned in a baculovirus transfer vector pVL1392. The sequences between EcoRI and BamHI sites were released from pVL1392-PPAR and subcloned into the same sites of pUSE and pHD, respectively. The resulting plasmids, pUSE-PPAR and pHD-PPAR, were characterized by various restriction enzyme digestion and used, as described hereafter in Example III for cotransfection with Baculo-Gold™ baculovirus DNA into insect Sf9 cells.
EXAMPLE II
Construction of Pvl1392-PPAR: The rat peroxisome proliferator-activated receptor (PPAR) alpha coding sequence was obtained by amplification of the same rat liver cDNA library using a pair of primers (AAT GCG GCC GCT ATG CAT CAC CAT CAC CAT CAC ATG GTG GAC ACA GAG AGC CCC (SEQ ID NO:7) and AGC CCG GGG GAT CCG ATC AGT ACA TGT CTC TGT ATA (SEQ ID NO:8)) according to the GenBank database (M88592). The amplification was performed by adding 1 ul of the cDNA library stock into 49 ul of water containing 50 pmol of each primer and further mixed with 50 ul of PCR master (BOEHRINGER MANNHEIM). The reaction was heated at 95° C. for 2 minutes, and followed by incubations at 60° C. for 1 minute, 68° C. for 1 minute, 95° C. for 30 seconds for a total of 30 cycles. Amplified fragment was first cloned into pGEM-T vector (Promega), sequenced, and subcloned into Not I and EcoR I sites of Baculovirus transfer vector pVL-1392 (PharMingen).
Construction of the vectors, pUSE-PPAR and pHD-PPAR: The cDNA fragment encoding rat PPAR alpha was released from pVL1392-PPAR by digestion with the restriction enzymes, EcoRI and BamHI. The fragment, with the same open reading frame, was subcloned into EcoRI and BglII sites of pUSE and pHD, respectively. The resulting plasmids, pUSE-PPAR and pHD-PPAR, were characterized by restriction enzyme digestion with EcoRV/BglII, EcoRV/PstI, and EcoRV/HindIII. The inserts were correct in size and orientation.
In order to demonstrate and compare the expression level of the vectors prepared above (pUSE, pHD, pUSE-PPAR, pHD-PPAR and pVL1292-PPAR) and to illustrate other advantages of the present invention, linearized baculovirus DNA was used to generate recombinant viruses from these constructs and to infect insect Sf9 cells. Example III illustrates the preparation of the recombinant baculoviruses and Example IV illustrates the use of these recombinant viruses in the production of proteins, including the fusion products prepared according to the present invention.
As described above and in Example III, with insect cells the vector was introduced into the cells with linearized baculovirus DNA by means of co-transfection. Where, however, the host cell is another eukaryotic cell such as mammalian or if the host cell is prokaryotic such as bacteria then the construct vectors can be directly introduced into the host cell by well known techniques.
EXAMPLE III
Co-transfection of above constructs with linearized DNA into insect Sf9 cells: Insect Sf9 cells in monolayer cultures were grown in Grace medium containing 10% Fetal Bovine Serum (GIBCO-BRL). For each transfection, a 60 mm tissue culture plate was seeded with 2×10 6 Sf9 cells and kept at room temperature for 30 minutes. A mixture of 0.5 ug of linear baculovirus DNA (BaculoGold™ DNA from PharMingen) and 5 ug of plasmid DNA (i.e., pUSE, pUSE-PPAR, pHD, pHD-PPAR, and pVL1392-PPAR) was added into 1 ml of Transfection Buffer B (125 mM Hepes, pH 7.1, 125 mM CaCl2, 140 mM NaCl). The DNA/Transfection Buffer B solution was further added into 1 ml of Grace medium in the tissue culture plate drop-by-drop and incubated at 27° C. for 4 hours. At the end, the transfection solution was replaced by 4 ml of fresh Grace medium and the plate was kept at 27° C. for four days.
Purification of the recombinant virus by plaque assay: Four days after co-transfection, the supernatant containing recombinant virus from the co-transfected plates were collected and diluted 1:10, 1:100, 1:1,000, 1:10,000, and 1:100,000, respectively, with Grace medium. For infection, 2 ml of each of the dilutions were added in a 60 mm tissue culture plate containing 2×10 6 Sf9 cells and incubated at 27° C. for 1 hour. After infection, a mixture of 2% SeaPlaque agarose (from FMC) melted in water at 65° C. and 2×Grace medium containing 20% FBS at room temperature was overlayed on top of the infected cells and the plate was kept at 27° C. under humid conditions. For each of the constructs (e.g. pUSE, pUSE-PPAR, pHD, pHD-PPAR, and pVL1392-PPAR), four independent plaques were individually picked up using a 1 ml pipette tip and individually resuspended in 200 ul of Grace medium containing 10% FBS.
Amplification of the plaque purified recombinant viruses: A 24 well cell culture plate (from Corning) was seeded with 2×10 5 Sf9 cells in each well and plaques resuspended in 200 ul of the Grace medium were used to infect the cells. Four days after infection, the media were collected and used to infect 6×10 6 Sf9 cells seeded in 250 ml cell culture flasks. The amplified viral stocks containing approximately 3×10 8 PFU/ml were collected four days after infection and stored at 4° C. for further experiments. The remaining infected cells were assayed for recombinant protein expression by SDS-PAGE analysis using a precasted 4-20% gradient gel (Novex). One recombinant baculovirus clone was chosen from these four plaques to represent the original plasmid construct and used for subsequent experiments.
EXAMPLE IV
Expression of Fusion Protein (IPT-PPAR) in Insect Cells: The recombinant baculoviruses obtained as above described from the constructs of pUSE, pUSE-PPAR, pHD, pHD-PPAR, and pVL1392-PPAR were used to express the uricase (35 kDa) tag, the uricase-PPAR fusion protein (90 kDa), the polyhedrin tag (30 kDa), the polyhedrin-PPAR fusion protein (85 kDa), and PPAR (55 kDa), respectively. To compare the expression, 200 ul of the viral stock containing 3×10 8 PFU/ml were used to infect Sf9 cells grown in a 250 ml tissue culture flask at 80% confluence. Three days (72 hours) after infection, the infected cells were washed once with phosphate-buffered saline, lysed with SDS-PAGE sample buffer and then analyzed by SDS-PAGE using a precasted 4-20% SDS-PAGE gel (Novex). After electrophoresis, the gel was stained with Coomassie Blue and the results are shown in FIG. 5. A dominant recombinant protein band representing uricase (lane 1) tag, uricase-PPAR fusion protein (lane 2), polyhedrin tag (lane 3), polyhedrin-PPAR fusion protein (lane 4), respectively, were observed in the insect cell lysates (about 20-50% of the total cellular protein). In contrast, with PPAR alone, absent either insoluble tag (lane 5), no significant recombinant protein accumulations were observed. The recombinant PPAR protein, the expression of which is known to be very difficult, can only be detected by immunoblotting. The expression of PPAR in insect cells was reported at the low level of 10 mg/10 9 cells (Proc. Natl. Acad. Sci. USA, 90, 1440-1444). With uricase and polyhedrin tag, the expression reached a level of 500 and 100 mg/10 9 cells, respectively. Thus, the expression of PPAR was increased 10-50 fold by uricase and polyhedrin tag.
Example V illustrates purification of the fusion proteins expressed above by the one-step procedure of the present invention.
EXAMPLE V
The recombinant proteins, 0.5 g wet total protein of insect cells infected with respective recombinant baculovirus (prepared as in Example III) were resuspended in 5 ml of B-PER Reagent (Pierce Chemical Company) to lyse the cells according to manufacturer's instructions. The suspensions were stirred for 1 hour at 4° C. and then centrifuged at 12,000×g for 30 min and the pellets were washed once with the same reagent to eliminate possible contamination from membrane proteins. In order to obtain activity, the final pellets were solubilized by increasing pH to 11 by stirring with 0.1 M Na 2 CO 3 for 1 hour. Samples from each step were taken and analyzed by SDS-PAGE. As shown in FIG. 6, IPTu, IPTu-PPAR, IPTp, and IPTp-PPAR were the dominant proteins in the total cellular lysates.
As shown, after centrifugation, the respective purified proteins were removed from the supernatants. The washing step with the same reagent further removes possible contaminants. The recombinant fusion protein remains as a pellet and the purity is greater than 90% by this spin-down procedure as judged by SDS-PAGE analysis. Fusion proteins and tags exhibit similar patterns indicating that uricase and polyhedrin are capable of pulling down their fusion partner.
EXAMPLE VI
Detection of the IPTu-PPAR Fusion Protein by Measuring Uricase Activity: An additional benefit provided by the uricase tag is that the fusion protein can be monitored by a simple spectrophotometric assay. The total protein lysates, supernatant, washed supernatant, and final purified IPTu-PPAR fusion protein were 1:1 diluted in 0.1 M Glycine (pH 9.4). To detect the uricase activity, 100 ul of the diluted samples were incubated with 100 ul of uric acid (15 mg/ml in 0.1 M Glycine) at 37° C. for 1 hour. At the end of incubation, 20 ul of 50% TCA solution was added into the reaction and the proteins were removed from the sample by spin at 15,000 RPM with a microcentrifuge for 5 minutes. The supernatants were collected and added into 1 ml of 0.1 M Glycine. The absorption at OD 295 was recorded by a HITACHI U2000 spectrophotometer. As shown in FIG. 7, most of the uricase activity, by the illustrated disappearance of uric acid absorbance at 295, is retained in the pellet fraction. Thus uricase served as a dual functional tag for one-step purification and easy detection.
The following Example VII illustrates a procedure according to this invention for removing the insoluble tag, IPTu, from the protein, PPAR, and the subsequent recovery of the protein.
EXAMPLE VII
Approximately 20 ug of IPTu-PPAR fusion protein purified by the one-step procedure and solubilized in 20 ul of 0.1 M Na 2 CO 3 (pH 11), as described in Example V, were dialyzed against 50 ml of the dialysis buffer containing 50 mM Tris-HCl (pH8.8), 100 mM NaCl, and 5 mM DTT overnight at 4° C. After dialysis, the sample was digested with enterokinase to cleave off the tag by mixing with 3 ul of 10× EKMax Buffer and 4 ul of EKMax (from Invitrogen) at a total volume of 30 ul and incubated at 37° C. for 16 hours. After digestion, 10 ul of 200 mM Tris.HCI (pH 6.8) were added into the digested sample to adjust the pH to 7.5. At this neutral pH, the uricase tag is insoluble and precipitates out of the solution. The tag and any undigested fusion protein were removed by centrifugation at 15 k rpm for 15 minutes and approximately 8 ug of soluble PPAR were obtained by this procedure. The same procedure is also applicable with respect to the IPTp-PPAR fusion protein.
While the invention has been illustrated above with respect to PPAR as the soluble protein of interest, it is to be understood that the invention is applicable to other proteins which, as expressed, are soluble in aqueous lysate solutions, preferably solutions under physiological conditions, e.g., a pH of 7-8 and a temperature of 20°-37° C. Accordingly, many of those soluble proteins which have heretofore been separated from their lysate solutions in fused product form using conventional tags can now be more conveniently separated utilizing insoluble tags as illustrated in the present invention. Thus, lysate solutions at a pH and/or temperature other than that specified above may also be useful so long as the protein is soluble and the tag is insoluble.
In like fashion, while uricase and polyhedron have been shown as useful as particularly useful insoluble tags, the invention is also applicable to other tags which, as expressed, are insoluble in the chosen aqueous lysate solutions, preferably under physiological conditions. In particular, proteins similar to uricase and polyhedrin regions are considered to demonstrate the desired insolubility to be useful as tags for the purposes of the present invention. As shown in FIG. 8 (SEQ ID NOs:9 and 10), uricase and polyhedrin have a 15% identify in amino acid sequences (the “*” symbol) and a 12% similarity (the “.” symbol). Accordingly, proteins having a combined identity and similarity in amino acid sequences to uricase or polyhedrin of at least 25% and, preferably, at least 27% are considered to be useful herein as insoluble tags. As shown in FIG. 9, there is also a similarity in hydrophilicity between uricase and polyhedrin. While not quantitated, similarity in this characteristic is also considered to be useful in the selection of an insoluble proteinaceous tag. Accordingly, truncated versions of uricase and polyhedrin which are insoluble in the lysate solution are also deemed useful.
10
1
27
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of a sense primer used for amplification of rat urate
oxidase
1
gaattccatt cttgaaaccg aatctga 7
2
21
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of an antisense primer used for amplifcation of rat urate
oxidase
2
cggatcctaa agacagagtc t 21
3
33
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of a sense primer used for construction of pUSE
3
actaatatca caaactggaa atgtctatca ata 33
4
78
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of an antisense primer used for construction of pUSE
4
gaattcctcg agcttatcgt catcgtcgtg atggtgatgg tgatgcagcc tggaaggcag 60
cttcctcctc accgtccc 78
5
30
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of a sense primer used for construction of pHD
5
actaatatca catggaaatg tctatcaata 30
6
78
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of a sense primer used for construction of pHD
6
gaattcctcg agcttatcgt catcgtcgtg atggtgatgg tgatgatacg ccggaccagt 60
gaacagaggt gcgtctgg 78
7
60
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of a sense primer used for amplification of PPAR
7
aatgcggccg ctatgcatca ccatcaccat caccatcaca tggtggacac agagagcccc 60
8
36
DNA
Artificial Sequence
Description of Artificial Sequence DNA
sequence of an antisense primer used for amplification of PPAR
8
agcccggggg atccgatcag tacatgtctc tgtaga 36
9
245
PRT
Baculovirus transfer vector pBacPAK-His1
9
Met Pro Asp Tyr Ser Tyr Arg Pro Thr Ile Gly Arg Thr Tyr Val Tyr
1 5 10 15
Asp Asn Lys Tyr Tyr Lys Asn Leu Gly Ala Val Ile Lys Asn Ala Lys
20 25 30
Arg Lys Lys His Phe Ala Glu His Glu Ile Glu Glu Ala Thr Leu Asp
35 40 45
Pro Leu Asp Asn Tyr Leu Val Ala Glu Asp Pro Phe Leu Gly Pro Gly
50 55 60
Lys Asn Gln Lys Leu Thr Leu Phe Lys Glu Ile Arg Asn Val Lys Pro
65 70 75 80
Asp Thr Met Lys Leu Val Val Gly Trp Lys Gly Lys Glu Phe Tyr Arg
85 90 95
Glu Thr Trp Thr Arg Phe Met Glu Asp Ser Phe Pro Ile Val Asn Asp
100 105 110
Gln Glu Val Met Asp Val Phe Leu Val Val Asn Met Arg Pro Thr Arg
115 120 125
Pro Asn Arg Cys Tyr Lys Phe Leu Ala Gln His Ala Leu Arg Cys Asp
130 135 140
Pro Asp Tyr Val Pro His Asp Val Ile Arg Ile Val Glu Pro Ser Trp
145 150 155 160
Val Gly Ser Asn Asn Glu Tyr Arg Ile Ser Leu Ala Lys Lys Gly Gly
165 170 175
Gly Cys Pro Ile Met Asn Leu His Ser Glu Tyr Thr Asn Ser Phe Glu
180 185 190
Gln Phe Ile Asp Arg Val Ile Trp Glu Asn Phe Tyr Lys Pro Ile Val
195 200 205
Tyr Ile Gly Thr Asp Ser Ala Glu Glu Glu Glu Ile Leu Leu Glu Val
210 215 220
Ser Leu Val Phe Lys Val Lys Glu Phe Ala Pro Asp Ala Pro Leu Phe
225 230 235 240
Thr Gly Pro Ala Tyr
245
10
303
PRT
Rattus rattus
10
Met Ala His Tyr His Asp Asp Tyr Gly Lys Asn Asp Glu Val Glu Phe
1 5 10 15
Val Arg Thr Gly Tyr Gly Lys Asp Met Val Lys Val Leu His Ile Gln
20 25 30
Arg Asp Gly Lys Tyr His Ser Ile Lys Glu Val Ala Thr Ser Val Gln
35 40 45
Leu Thr Leu Arg Ser Lys Lys Asp Tyr Leu His Gly Asp Asn Ser Asp
50 55 60
Ile Ile Pro Thr Asp Thr Ile Lys Asn Thr Val His Val Leu Ala Lys
65 70 75 80
Phe Lys Gly Ile Lys Ser Ile Glu Thr Phe Ala Met Asn Ile Cys Glu
85 90 95
His Phe Leu Ser Ser Phe Ser His Val Thr Arg Ala His Val His Val
100 105 110
Glu Glu Val Pro Trp Lys Arg Phe Glu Lys Asn Gly Val Lys His Val
115 120 125
His Ala Phe Ile His Thr Pro Thr Gly Thr His Phe Cys Asp Val Glu
130 135 140
Gln Val Arg Asn Gly Pro Pro Ile Ile His Ser Gly Ile Lys Asp Leu
145 150 155 160
Lys Val Leu Lys Thr Thr Gln Ser Gly Phe Glu Gly Phe Ile Lys Asp
165 170 175
Gln Phe Thr Thr Leu Pro Glu Val Lys Asp Arg Cys Phe Ala Thr Gln
180 185 190
Val Tyr Cys Lys Trp Arg Tyr Gln Asn Arg Asp Val Asp Phe Glu Ala
195 200 205
Thr Trp Gly Ala Val Arg Asp Ile Val Leu Lys Lys Phe Ala Gly Pro
210 215 220
Tyr Asp Arg Gly Glu Tyr Ser Pro Ser Val Gln Lys Thr Leu Tyr Asp
225 230 235 240
Ile Gln Val Leu Thr Leu Ser Gln Leu Pro Glu Ile Glu Asp Met Glu
245 250 255
Ile Ser Leu Pro Asn Ile His Tyr Phe Asn Ile Asp Met Ser Lys Met
260 265 270
Gly Leu Ile Asn Lys Glu Glu Val Leu Leu Pro Leu Asp Asn Pro Tyr
275 280 285
Gly Lys Ile Thr Gly Thr Val Arg Arg Lys Leu Pro Ser Arg Leu
290 295 300
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A process is disclosed for the preparation of a recombinantly expressed fusion product comprised of a proteinaceous tag and a soluble protein of interest and the separation of the fusion product from the host cell in which it is expressed. The tag and in turn the fusion product is insoluble in the host cell lysate solution and the fusion product is separated therefrom by centrifugation or filtration.
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RELATED APPLICATION
This application is a continuation of U.S. patent application Ser. No. 13/248,279, filed Sep. 29, 2011, now U.S. Pat. No. 8,579,931, which is a continuation of U.S. patent application Ser. No. 12/335,118, filed Dec. 15, 2008, now U.S. Pat. No. 8,052,708, which is a continuation of U.S. patent application Ser. No. 10/421,517, filed Apr. 23, 2003, now U.S. Pat. No. 7,569,065, which is a divisional of U.S. patent application Ser. No. 09/596,160, filed Jun. 16, 2000, now U.S. Pat. No. 6,575,991, which claims the priority of U.S. Provisional Patent Application Ser. No. 60/139,580, filed Jun. 17, 1999.
BACKGROUND OF THE INVENTION
Field of the Invention
This invention relates generally to an apparatus for the percutaneous positioning of a radiopaque marker for identifying the location of a lesion in a stereotactic biopsy procedure. More particularly, the invention relates to an introducer having a hollow cannula in combination with a movable stylet and a radiopaque marker disposed within the cannula and ejected from it by movement of the stylet.
Related Art
Tissue biopsies are commonly performed on many areas and organs of the body where it is desirable to ascertain whether or not the biopsied tissue is cancerous. Often, a lesion or other tissue to be biopsied is identified through use of an imaging technique such as a computerized axial tomography (CAT) scan, ultrasonography, and mammography.
One problem commonly encountered, especially in breast biopsies, is that the lesion is so small that the biopsy reduces its size to the extent that it is no longer visible by the imaging method employed. In such circumstances, it is desirable to place a radiopaque marker at the site of the biopsy to enable the medical practitioner subsequently to locate the lesion quickly and accurately in the event complete removal of the affected tissue is indicated. This problem is currently met by placing a radiopaque marker at the biopsy area by means of a cannula or similar device housing the marker.
More particularly, one of the markers heretofore in use is a staple-type clip. The clip is introduced through a large-diameter cannula, specifically one of 11 gauge.
Some practitioners employ an embolization coil as a marker. This requires them to find a cannula or hollow needle of a size to receive the coil and some means to force the coil through the needle, all the while trying to keep these components together and sterile.
Prior devices for marking a biopsy area have several other disadvantages. A significant disadvantage is that the marker is not always completely ejected from the cannula or can be drawn back into or toward the cannula by the vacuum created upon the withdrawal of the cannula, which results in the marker being moved from the intended site, leading to inaccurate identification of the location of the biopsy area. A second major disadvantage is that current markers have a tendency to migrate within the tissue, also causing error in determining the biopsy location.
SUMMARY OF THE INVENTION
The present invention provides a biopsy marking apparatus for the percutaneous placement of a marker at a biopsy site in a tissue mass to facilitate subsequent determination of the location of the biopsy site. The biopsy marking apparatus comprises an introducer having a handle to be grasped by a user, a cannula, a stylet, and a radiopaque marker. The cannula has a proximal end mounted to the handle and a distal end defining an insertion tip. The stylet is slidably received within the cannula for movement between a ready position in which a distal end of the stylet is spaced inwardly from the cannula tip to form a marker recess between the distal end of the stylet and the cannula tip, and an extended position in which the distal end of the stylet extends at least to the cannula tip to effectively fill the marker recess.
A plunger is movably mounted to the handle and operably engages the stylet, the plunger being movable between a first position and a second position for moving the stylet between the ready position and the extended position.
A latch is provided for fixing the stylet in the extended position to prevent retraction of the stylet from that position.
A radiopaque marker is disposed within the marker recess, whereby, when the plunger is moved between the first and second positions, the stylet is moved from the ready to the extended position to eject the radiopaque marker from the marker recess, and the latch fixes the stylet in the extended position to prevent the return of the marker to the marker recess.
The latch preferably comprises a detent on either the plunger or the handle and a catch on the other, the catch being receivable within the detent as the plunger is moved from the first to the second position.
In another aspect, the invention also provides a radiopaque marker having a marker body and an anchor extending away from the body for fixing the location of the radiopaque marker in a tissue mass by the tissue mass prolapsing about the anchor. Preferably, the body has an interior hollow portion forming an air trap to enhance the ultrasound characteristic of the radiopaque marker.
Other features and advantages of the invention will be apparent from the ensuing description in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a plan view of an introducer used to place a radiopaque marker at a biopsy location in accordance with the invention;
FIG. 2 is an enlarged sectional view of the area II of FIG. 1 , illustrating the position of a radiopaque marker within the introducer prior to ejection;
FIG. 3 is an enlarged sectional view of the area III of FIG. 1 , illustrating the arrangement of a handle, a plunger, and a stylet of the introducer;
FIG. 4 is a sectional view taken along line 4 - 4 of FIG. 1 and illustrating the introducer in a ready condition;
FIG. 5 is a sectional view taken along line 4 - 4 of FIG. 1 and illustrating the introducer in a discharged condition;
FIG. 6 is an enlarged view of a first embodiment of a radiopaque marker according to the invention;
FIG. 7 is an enlarged view of a second embodiment of a radiopaque marker according to the invention;
FIG. 8 is an enlarged view of a third embodiment of a radiopaque marker according to the invention;
FIG. 9 is an enlarged view of a fourth embodiment of a radiopaque marker according to the invention;
FIG. 10 is a partially broken away perspective view, greatly enlarged, of a fifth embodiment of a radiopaque marker according to the invention;
FIG. 11 is a plan view of the radiopaque marker of FIG. 10 ;
FIG. 12 is a greatly enlarged view of a sixth embodiment of a radiopaque marker according to the invention;
FIG. 13 is a greatly enlarged view of a seventh embodiment of a radiopaque marker according to the invention;
FIG. 14 is a greatly enlarged view of an eighth embodiment of a radiopaque marker according to the invention; and
FIG. 15 is a greatly enlarged view of a ninth embodiment of a radiopaque marker according to the invention.
DETAILED DESCRIPTION
FIGS. 1 to 4 illustrate a biopsy marking apparatus 10 according to the invention, which is capable of the percutaneous placement of a radiopaque marker at the location of a tissue biopsy. The biopsy marking apparatus 10 comprises an introducer 12 and a radiopaque marker 14 ( FIG. 2 ) contained within the introducer 12 . The introducer 12 includes a handle 16 having a hollow interior 18 . The handle 16 comprises a grip portion 20 from which extends a tapered nose portion 22 . The grip portion 20 defines a rear opening 24 that provides access to the hollow interior 18 . A pair of detents 26 are formed in the grip portion 20 near the rear opening 24 . Channels 28 are formed on the interior surface of the grip portion 20 and extend from the rear opening 24 to the detents 26 .
The nose portion 22 comprises a guide passage 30 extending from the tip of the nose portion 22 to the hollow interior 18 of the handle 16 . The guide passage 30 decreases in diameter inwardly from the tip of the nose portion to form a cannula seat 32 . Alternatively, the diameter of the guide passage 30 may be substantially equal to or slightly smaller than the outer diameter of a cannula 34 , which in any case is press-fit within the cannula seat 32 . As is customary, the cannula is formed with a hollow interior 36 and a sharpened tip 38 .
A stylet 40 comprising a shaft 42 and a base 44 is received within the hollow interior 18 of the handle 16 in a manner such that the shaft 42 extends through the guide passage 30 and into the cannula interior 36 and the stylet base lies within the hollow interior 18 .
A plunger 50 comprises a cylindrical body 52 from which extend a pair of catches 54 at diametrically opposed positions. The cylindrical body 52 is sized so that it is slidably received within the rear opening 24 of the handle 16 , where it is so oriented with respect to the handle that the catches 54 are aligned with the guide channels 28 .
It will be recognized that the foregoing construction provides a biopsy marking apparatus which may be preassembled as a unit and prepackaged, all under sterile conditions, thereby affording the practitioner substantially greater convenience and reliability. Such a construction also permits use of a narrower cannula, which may be of 14 gauge or smaller.
In operation, the introducer 12 begins in the ready condition shown in FIG. 4 . In this condition, the stylet shaft is received within the cannula but does not extend to the cannula tip 38 , thereby forming a marker recess 46 within the cannula 34 , the radiopaque marker 14 is disposed within the marker recess 46 , and the plunger 50 is in a position relative to the handle 20 in which the catches are outside the handle; that is, they are not received within the detents 26 . However, the plunger 50 is so oriented with respect to the handle that the catches 54 are aligned with the guide channels 28 .
With the introducer in the ready condition, the cannula is positioned so that its tip is at or near the location of a tissue mass where a biopsy has been taken. Preferably, the cannula tip is positioned by using imaging systems. The cannula tip 38 can be designed for enhanced visibility using common imaging systems, such as CAT scan, ultrasonography and mammography. Suitable cannula tips are disclosed in U.S. Pat. No. 5,490,521, issued Feb. 13, 1996 to R. E. Davis and G. L. McLellan, which is incorporated by reference. Ultrasound enhancement technology is also disclosed in U.S. Pat. No. 4,401,124, issued Aug. 30, 1983 to J. F. Guess, D. R. Dietz, and C. F. Hottinger; and U.S. Pat. No. 4,582,061, issued Apr. 15, 1986 to F. J. Fry.
Once the cannula is positioned at the desired location, the plunger 50 is moved from its first or ready condition as illustrated in FIGS. 1 to 4 to a second or discharged condition in which the catches 54 are received within the detents 26 to lock the plunger 50 in the discharged condition and the stylet shaft extends beyond the cannula tip 38 . The catches 50 and detents combine to function as a latch for locking the plunger in the discharged condition. As the plunger 50 is moved from the ready condition to the discharged condition, the plunger 50 drives the stylet base 44 forward to advance the stylet shaft 42 within the cannula interior 36 . As the stylet shaft 42 is advanced, the radiopaque marker 14 is ejected from the marker recess 46 through the cannula tip 38 and into the tissue at the biopsy location.
It is preferred that the stylet shaft 42 be sized in a manner such that when the plunger 50 is in the discharged condition the stylet shaft 42 extends beyond the cannula tip 38 to ensure the complete ejection of the radiopaque marker 14 from the marker recess 46 . The extension of the stylet shaft 42 beyond the cannula tip 38 also prevents the radiopaque marker 14 from being drawn back into the marker recess upon the removal of the introducer 12 from the tissue mass, which can occur as the tissue mass collapses and is drawn towards and into the cannula by the resilient nature of the tissue mass and the creation of a vacuum by the cannula as it is withdrawn from the tissue.
The rate at which the plunger 50 is moved from the ready condition to the discharged condition is preferably manually controlled by the user to control the rate at which the marker 14 is ejected into the tissue mass. Manual control of the ejection rate of the radiopaque marker provides the user with the ability to adjust the position of the cannula tip as the marker is being ejected and thereby permits additional control of the final location of the marker within the tissue mass. In other words, “on-the-fly” adjustment of the cannula tip during positioning of the marker 14 enables a more accurate placement of the marker.
The biopsy marking apparatus 12 may be placed in a safety condition (not shown) before packaging or use by rotationally orienting the plunger 50 with respect to the handle 16 so that the catches 54 are out of alignment with the guide channels 28 , whereby the plunger cannot be depressed or advanced within the handle. It will be apparent that the marking apparatus can be placed in the ready condition previously described simply by rotating the plunger relative to the handle until the catches 54 are aligned with the guide channels 28 .
It will also be apparent that the biopsy marking apparatus 10 may incorporate or be fitted with any one of several known trigger devices, some of them spring-loaded, for advancement of the plunger 50 . Such a trigger device is disclosed, for example, in U.S. Pat. No. 5,125,413, issued Jun. 30, 1992 to G. W. Baran.
It should be noted that as a variation of the foregoing procedure the cannula employed during the biopsy procedure might be left in place with its tip remaining at the site of the lesion. The introducer 12 of the present invention would then be directed to the site through the biopsy cannula or, alternatively, the marker 14 of the present invention would be introduced to the biopsy cannula and ejected from its tip into the tissue mass by fitting the biopsy cannula to the introducer 12 in place of the cannula 34 .
The radiopaque marker 14 used in combination with the introducer 12 to mark the location of the tissue biopsy should not only be readily visible using contemporary imaging techniques but it should not migrate within the tissue from the position in which it is initially placed. FIGS. 6 to 15 disclose various embodiments of radiopaque markers 14 that are highly visible using contemporary imaging techniques and are resistant to migration in the tissue.
FIG. 6 illustrates a first embodiment 60 of a radiopaque marker comprising a coil spring 62 from which extend radiopaque fibers 64 . The coil spring 62 is preferably made from platinum or any other material not rejected by the body. The coil spring 62 is wound to effectively form a hollow interior comprising one or more air pockets, which are highly visible using contemporary ultrasound imaging techniques. The radiopaque fibers 64 are preferably made from Dacron, which is also highly visible using current imaging techniques.
The radiopaque marker 60 is highly visible using any of the commonly employed contemporary imagining techniques because of the combination of reflective surfaces formed by the coils, the hollow interior and the air pockets of the coil spring 62 , as well as the radiopaque fibers 64 .
The coil spring 62 is pre-shaped prior to being loaded into the marker recess 46 so that it tends to form a circular shape as shown in FIG. 6 after it is ejected from the marker recess 46 . The circular shape tends to resist migration within the tissue.
FIG. 7 illustrates a second embodiment 70 of a radiopaque marker having a star-burst configuration comprising a core 72 with multiple fingers 74 extending from the core.
FIG. 8 illustrates a third embodiment 80 of a radiopaque marker that is similar to the star-burst marker 70 in that it comprises a core 82 from which extend three fingers 84 . Each of the fingers includes radiopaque fibers 86 , which are preferably made from Dacron or a similar material.
FIG. 9 illustrates a fourth embodiment 90 of a radiopaque marker having a generally Y-shaped configuration comprising an arm 92 from which extend diverging fingers 94 . The arm and fingers 92 , 94 are preferably made from a suitable resilient metal such that the fingers can be compressed towards each other and the entire radiopaque marker 90 stored within the marker recess 46 of the cannula. Upon ejection of the marker 90 from the marker recess 46 into the tissue mass, the fingers 94 will spring outwardly to provide the marker 90 with an effectively greater cross-sectional area.
In addition to providing the marker 90 with an effectively greater cross-sectional area, the tips of the fingers 94 , together with the free end of the arm 92 , effectively form points of contact with the surrounding tissue mass that help to anchor the marker 90 in its release condition to prevent migration through the tissue mass.
FIG. 10 illustrates a fifth embodiment 100 of a radiopaque marker having a wire-form body in a horseshoe-like configuration comprising a rounded bight portion 102 from which extend inwardly tapering legs 104 , each of which terminate in curved tips 106 . The entire marker 100 preferably has a circular cross section defining a hollow interior 108 . The hollow interior provides for the trapping of air within the marker 100 to improve the ultrasound characteristics of the marker 100 .
The curved bight portion 102 and legs 104 preferably lie in a common plane. However, the tips 106 extend away from the legs 104 and out of the common plane so that the tips 106 will better function as anchors for the tissue that prolapses about the tips 106 once the marker 100 is ejected from the marker recess 46 and the introducer 12 is withdrawn from the tissue mass.
FIG. 12 illustrates a sixth embodiment 110 of a radiopaque marker that is similar to the horseshoe-like fifth embodiment marker 100 in that it comprises a bight portion 112 from which extend legs 114 , which terminate in tips 116 . The legs 114 of the marker 110 are crossed relative to each other, unlike the legs of the marker 100 , providing the marker 110 with an effectively larger cross-sectional diameter. The tips 116 are oriented at approximately 90° relative to the legs 114 to form anchors. The marker 110 also has a hollow interior 118 for enhanced radiopaque characteristics.
Though, as illustrated in FIG. 12 , the tips 116 of the marker 110 are oriented at approximately 90° with respect to the legs 114 , it is within the scope of the invention for the tips 116 to extend at substantially any angle with respect to the legs 114 . The tips 116 also need not extend away from the legs in the same direction. For example, the tips 116 could extend in opposite directions from the legs 114 .
FIG. 13 illustrates a seventh embodiment 120 of a radiopaque marker having a generally helical configuration comprising multiple coils 122 of continuously decreasing radius. The helical marker 120 is preferably made from a radiopaque material and has a hollow interior 124 to enhance its radiopaque characteristics. The decreasing radius of the coils 122 provides the marker 120 with multiple anchor points created by the change in the effective cross-sectional diameter along the axis of the helix. In other words, since the effective cross-sectional diameter of each coil is different from the next and each coil is effectively spaced from adjacent coils at the same diametric location on the helix, the tissue surrounding the marker 120 can prolapse between the spaced coils and each coil effectively provides an anchor point against the tissue to hold the marker 120 in position and prevent its migration through the tissue mass.
FIG. 14 illustrates an eighth embodiment 130 of a radiopaque marker comprising a cylindrical body 132 in which are formed a series of axially spaced circumferential grooves 134 . The spaced grooves 134 form a series of ridges 136 therebetween on the outer surface of the cylindrical body 132 . The cylindrical body 132 preferably includes a hollow interior 138 .
The alternating and spaced ridges 136 and grooves 134 provide the marker 130 with a repeating diameter change along the longitudinal axis of the cylindrical body 132 . As with the helical marker 120 , the grooves 134 between the ridges 136 provide an area in which the tissue surrounding the marker 130 can prolapse thereby enveloping the ridges 136 , which function as anchors for preventing the migration of the marker 130 in the tissue mass.
FIG. 15 illustrates a ninth embodiment 140 of a radiopaque marker comprising a cylindrical body 142 having an axial series of circumferential grooves 144 whose intersections with adjacent grooves form ridges 146 . The cylindrical body 142 preferably includes a hollow interior 148 . An anchor 150 extends from the cylindrical body 142 . The anchor 150 comprises a plate 152 connected to the cylindrical body 142 by a wire 154 .
The grooves 144 and ridges 146 of the maker 140 provide anchors in the same manner as the grooves 134 and ridges 136 of the marker 130 . The anchor 150 further enhances the non-migrating characteristics of the marker 140 by permitting a large portion of the surrounding tissue mass to prolapse between the plate 150 and the cylindrical body 142 .
The fifth through the ninth embodiments all preferably have a wire-form body. The various wire-form body shapes can be formed by stamping the shape from metal stock or the bending of a wire.
It should be noted that virtually all of the embodiments of the radiopaque marker described as being hollow can be made without a hollow interior. Similarly, those without a hollow interior can be made with a hollow interior. The hollow interior improves the ultrasound characteristics of the particular marker beyond the inherent radiopaque and ultrasound characteristics attributable to the marker shape and material. In practice, the use of the hollow interior is limited more by manufacturing and cost considerations rather than by performance.
Also, the shape of each marker can be altered to improve or enhance its non-migrating characteristics by adding an express anchor such as that disclosed in connection with the marker 140 or by modifying the marker to provide more anchor points as may be compatible with the basic configuration of the marker.
The combination of the enhanced radiopaque characteristics of the markers and the enhanced non-migrating features result in markers that are superior in use for identifying biopsy location after completion of the biopsy. The ability to accurately locate the biopsy site greatly reduces the amount of tissue that must be removed in a subsequent surgical procedure if the biopsy is cancerous. Additionally, the marker further enhances the ability to use percutaneous methods for removing the entire lesion, reducing the trauma associated with more radical surgical techniques.
The radiopaque markers described and illustrated herein are smaller than the staple-type clip and embolization coil used heretofore, thereby permitting a cannula of 14 gauge or less.
While the invention has been specifically described in connection with certain specific embodiments thereof, it is to be understood that this is by way of illustration and not of limitation, and the scope of the appended claims should be construed as broadly as the prior art will permit.
PARTS LIST
10
biopsy marking apparatus
12
introducer
14
radiopaque marker
16
handle
18
hollow interior
20
grip portion
22
nose portion
24
rear opening
26
detents
28
guide channels
30
guide passage
32
cannula seat
34
cannula
36
cannula interior
38
cannula pointed tip
40
stylet
42
stylet shaft
44
stylet base
46
marker recess
48
50
plunger
52
cylindrical body
54
catch
56
58
60
radiopaque marker
62
coil spring
64
radiopaque fibers
66
68
70
second embodiment radiopaque
marker
72
core
74
markers
76
78
80
third embodiment radiopaque
maker
82
core
84
fingers
86
88
90
fourth embodiment radiopaque
marker
92
arm
94
fingers
96
98
100
fifth embodiment radiopaque
marker
102
curved bight portion
104
legs
106
tips
108
110
sixth embodiment radiopaque
marker
112
curved bight portion
114
legs
116
tips
118
hollow interior
120
seventh embodiment radiopaque
marker
122
coil
124
126
128
130
eighth embodiment radiopaque
marker
132
cylindrical body
134
grooves
136
ridges
138
hollow interior
140
ninth embodiment radiopaque
marker
142
cylindrical body
144
grooves
146
ridges
148
hollow interior
150
anchor
152
plate
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A biopsy marking apparatus for placing a radiopaque marker at the location of a percutaneous biopsy. The biopsy marking apparatus comprises an introducer in combination with a radiopaque marker. The introducer ejects the radiopaque marker at the location of the biopsy. The introducer is configured to completely eject the radiopaque marker and prevent it from being subsequently drawn into the introducer as the introducer is removed from the biopsied tissue mass. The radiopaque marker has enhanced radiopaque characteristics and enhanced non-migration characteristics.
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This application is a File Wrapper Continuation of application Ser. No. 08/779,496, filed Jan. 8, 1997, now abandoned.
BACKGROUND OF THE INVENTION
In general, this invention is related to the fields of (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compounds and processes that use (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compounds.
The production of polymers that comprise ethylene is a multi-billion dollar enterprise. Many different catalysts can be used to polymerize ethylene. However, very few of these catalysts are of commercial importance. Currently, millions of dollars have been spent on research to make metallocene catalysts more commercially viable, and thus, more commercially important. This is because the polymers produced by such metallocene catalysts have properties that currently no other single polymer can reproduce. However, one of the technical problems associated with these metallocene catalysts is that they are homogenous with the polymerization medium. That is, they are soluble in the medium in which the polymerization is conducted. This is a drawback to the use of such metallocene catalysts because most commercially important polymerization processes use heterogenous catalysts. Therefore, in order to make metallocene catalysts more commercially important, heterogenous metallocene catalysts must be produced. Additionally, it is very important to have a metallocene catalyst that produces polymers that have a high molecular weight.
SUMMARY OF THE INVENTION
An object of this invention is to provide an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound.
Another object of this invention is to provide a process to polymerize monomers, especially ethylene, with an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound.
In accordance with one embodiment of this invention an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound is provided.
In accordance with another embodiment of this invention a process to polymerize monomers, especially ethylene, with an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound is provided. This process comprises (or optionally consists essentially of, or consists of): using an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound to polymerize monomers into polymers.
The objects and advantages of this invention are further described and defined in the following description and claims. It should be noted that the invention described herein can be practiced without any components or steps not specifically detailed herein.
DETAILED DESCRIPTION OF THE INVENTION
In general, (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compounds are those compounds having the general formula indicated in Box One.
In this general formula, R is an (R 1 ) 2 C═C(R 1 )—(C(R 1 ) 2 ) n —C(R 1 ) 2 —group (where n is from 0 to about 20). In this group, each R 1 can be any substituent that does not substantially, and adversely, interfere with any of the processes disclosed herein. For example, each R 1 can be a hydrocarbyl having from 1 to about 20 carbon atoms. However, it is preferred that each R 1 have from 1 to 10 carbon atoms, and it is even more preferred that each R 1 have from 1 to 6 carbon atoms. Further examples of R 1 are hydrogen, alkyl, aryl, alkoxy, and aryloxy. Currently, it is most preferred if R 1 is hydrogen.
The R group is attached to a cyclopentacarbyl group (R 0 ) which can be either substituted or unsubstituted, and which can form a metallocene compound with a transition metal. The substituents of the cyclopentacarbyl group can be any substituent that does not substantially, and adversely, interfere with any of the processes disclosed herein. Examples of cyclopentacarbyl groups are substituted and unsubstituted cyclopentadiene groups and substituted and unsubstituted indenyl groups. Currently it is preferred if the cyclopentacarbyl group (R 0 )is an indenyl.
The cyclopentacarbyl group is attached to a silane bridging group that can be substituted or unsubstituted. The substituents (R 3 ) of the silane bridging group can be any substituent that does not substantially, and adversely, interfere with any of the processes disclosed herein. Examples of such substituents are hydrogen, alkyl, aryl, alkoxy, and aryloxy. Currently, it is preferred if each R 3 is alkyl or aryl, however, it is most preferred if R 3 is aryl, such as, for example, phenyl.
The fluorenyl group in the general formula can be substituted or unsubstituted. The substituents of the fluorenyl group can be any substituent that does not substantially, and adversely, interfere with any of the processes disclosed herein. Examples of such substituents are hydrogen, alkyl, aryl, alkoxy, and aryloxy. Currently, it is preferred if the substituents are hydrogen.
In the general formula, M is a transition metal selected from the group consisting of titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, and the lanthanides. Currently, the preferred transition metals are zirconium and hafnium.
In the general formula, X is an alkyl, aryl, alkoxy, aryloxy, amides, hydride, or halogen. Currently, it is most preferred if X is a halogen. However, it is most preferred if X is chlorine.
This (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) metallocene compound can be produced by first taking a cyclopentacarbyl compound and reacting it with an organometal compound such as, for example, n-butyllithium, to form a cyclopentacarbyl metal compound. In general, the metal in the organometal compound is any Group I metal and the organo part of the compound is an alkyl. The cyclopentacarbyl compound is any compound that has at least five carbon atoms arranged in a cyclic structure. This cyclopentacarbyl compound can be either substituted or unsubstituted. Additionally, this cyclopentacarbyl compound can form a metallocene compound with a transition metal. The substituents of the cyclopentacarbyl compound can be any substituent that does not substantially, and adversely, interfere with any of the processes disclosed herein. Examples of cyclopentacarbyl compounds are substituted and unsubstituted cyclopentadiene groups and substituted and unsubstituted indenyl groups. In general, the reaction of the cyclopentacarbyl compound with an organometal compound to produce a cyclopentacarbyl metal is conducted at any suitable temperature and pressure. Currently, a temperature of about −80° C. to about 160° C. and a pressure of about 0 to about 100 atmospheres are preferred. However, a temperature of about −80° C. to about 60° C. and a pressure of about 1 atmosphere are more preferred. The molar ratio of cyclopentacarbyl compound to the organometal compound can be any suitable ratio. Currently, molar ratios of 1 to 1 are preferred.
This cyclopentacarbyl metal compound is then reacted with a haloalkene to produce an (omega-alkenyl) cyclopentacarbyl compound. In general, the reaction of the cyclopentacarbyl metal compound with a haloalkene to produce an (omega-alkenyl) cyclopentacarbyl compound is conducted at any suitable temperature and pressure. Currently, a temperature of about −80° C. to about 160° C. and a pressure of about 0 to about 100 atmospheres are preferred. However, a temperature of about −80° C. to about 60° C. and a pressure of about 1 atmosphere are more preferred. The molar ratio of cyclopentacarbyl metal compound to the haloalkene can be any suitable ratio. Currently, molar ratios of 1 to 1 are preferred.
Once the (omega-alkenyl) cyclopentacarbyl compound is produced it can be reacted with an organosilane to produce an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) compound. In general, the reaction of the (omega-alkenyl) cyclopentacarbyl compound with an organosilane to produce an (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) compound is conducted at any suitable temperature and pressure. Currently, a temperature of about −80° C. to about 160° C. and a pressure of about 0 to about 100 atmospheres are preferred. However, a temperature of about −80° C. to about 60° C. and a pressure of about 1 atmosphere are more preferred. The molar ratio of cyclopentacarbyl metal compound to the haloalkene can be any suitable ratio. Currently, molar ratios of 1 to 1 are preferred.
Once the (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) compound is produced it can be used to produce metallocene compounds wherein the (omega-alkenyl) cyclopentacarbyl portion of the (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) compound is one of the ligands of the metallocene compound.
Various methods are known in the art to bind a ligand to a transition metal in order to produce a metallocene compound. For example, the following references can be consulted: U.S. Pat. Nos. 5,436,305; 5,498,581; 5,565,592; and European Application 524,624 (the entire disclosures of which are hereby incorporated by reference). In general, however, metallocene compounds that contain an (omega-alkenyl) (cyclopentacarbyl) can be prepared by reacting the (organo) ((omega-alkenyl) cyclopentacarbyl) (silane bridged) compound with an alkali metal alkyl compound to produce a ligand salt that is then reacted with a transition metal compound to yield a metallocene compound.
These metallocene compounds can be used to polymerize various olefins. The particular polymerization conditions employed using these compounds can vary depending upon the particular results desired. Usually these compounds are used with organoaluminoxane compounds, such as, for example, methylaluminoxane, to form better polymerization catalysts. The ratio of the transition metal to the organoaluminoxane composition can vary widely depending upon the particular composition selected and the results desired. Typically, the atomic ratio of aluminum in the organoaluminoxane composition to the transition metal is in the range of about 1/1 to about 20000/1, preferably about 15/1 to about 5000/1, and more preferably about 100/1 to about 1000/1.
Examples of some monomers for polymerization include ethylene and alpha-olefins having 3 to 20 carbon atoms, such as propylene, 1-butene, 3-methyl-1-butene, 3-methyl-1-pentene, 3-ethyl-1-hexene, 1-hexene, 4-methyl-1-pentene, 1-octene, 1-hexadecene, cyclopentene, norborene, styrene, 4-methyl styrene, vinyl cyclohexane, butadiene, and the like and mixtures thereof.
The present invention is particularly useful in slurry type polymerizations since it allows one to carry out such polymerizations more effectively than has heretofore been possible. A particularly preferred type of slurry polymerization involves the continuous loop reactor type polymerization wherein monomer, catalyst, and diluent, if employed, are continuously added to the reactor as needed and polymer product is continuously or at least periodically removed. Generally, in such processes, ethylene is polymerized in the presence of a suitable liquid diluent, a higher alpha-olefin comonomer, and optionally, hydrogen. The polymerization temperature can vary over the range which will allow for slurry polymerization. Often slurry polymerization will be conducted at a temperature in the range of about 50° C. to about 100° C., although higher and lower temperatures can be used.
One of the benefits of this invention is that during polymerization the metallocene compound is incorporated into the polymer chain thereby forming a heterogenous metallocene catalyst. As discussed above, this is a very important result because it increases the commercial importance of metallocene compounds. For example, a heterogenous metallocene catalyst can be formed by prepolymerizing these metallocene compounds with a monomer, such as, for example, ethylene, to form a prepolymer supported metallocene compound. Examples of such techniques are disclosed in U.S. Pat. No. 5,498,581, the entire disclosure of which is hereby incorporated by reference.
The following examples are provided to further illustrate this invention. However, the invention should not be construed to be limited to the particular embodiments in these examples.
EXAMPLES
All examples were carried out using standard Schlenk techniques with the exclusion of oxygen and air moisture under argon. The solvents were dried over either: (a) Na/K alloy for ether, hexane, pentane, tetrahydrofuran, and toluene; (b) P 4 O 10 for methylene chloride; or (c) magnesium for methanol; and then distilled under argon.
Example One
P REPARATION OF AN ((O MEGA -A LKENYL ) C YCLOPENTACARBYL ) C OMPOUND
Example 1-1
Ten mL (85.7 mmol) of indene, which is a cyclopentacarbyl compound, was added to a container that contained 150 mL of diethyl ether and 15 mL of tetrahydrofuran to form a first mixture. This first mixture was then reacted with 53.6 mL (85.7 mmol) of n-butyllithium (1.6 M in hexane) to form indenyllithium, which is a cyclopentacarbyl metal compound. This reaction took place at −78° C. A yellow solution was formed. This yellow solution was then stirred at room temperature (about 25° C.) for four hours and then cooled again to −78° C. An equivalent quantity of 1-bromopropene, a haloalkene compound, was added dropwise to the yellow solution to form a second mixture. This second mixture was then stirred overnight at room temperature (about 25° C.). Thereafter, this second mixture was then hydrolyzed with 50 mL of water to form an organic phase and a water phase. The organic phase was dried over sodium sulfate and then the solvent was evaporated under a vacuum to produce a third mixture. This third mixture was then distilled using a high vacuum (10 −2 torr) to obtain a product. The product obtained was allyl-1-indene, which is an ((omega-alkenyl) cyclopentacarbyl) compound.
Example 1-2
Ten mL (85.7 mmol) of indene, which is a cyclopentacarbyl compound, was added to a container that contained 150 mL of diethyl ether and 15 mL of tetrahydrofuran to form a first mixture. This first mixture was then reacted with 53.6 mL (85.7 mmol) of n-butyllithium (1.6 M in hexane) to form indenyllithium, which is a cyclopentacarbyl metal compound. This reaction took place at −78° C. A yellow solution was formed. This yellow solution was then stirred at room temperature (about 25° C.) for four hours and then cooled again to −78° C. An equivalent quantity of 1-bromohexene, a haloalkene compound, was added dropwise to the yellow solution to form a second mixture. This second mixture was then stirred overnight at room temperature (about 25° C.). Thereafter, this second mixture was then hydrolyzed with 50 mL of water to form an organic phase and a water phase. The organic phase was dried over sodium sulfate and then the solvent was evaporated under a vacuum to produce a third mixture. This third mixture was then distilled using a high vacuum (10 −2 torr) to obtain a product. The product obtained was 5-hexenyl-1-indene, which is an ((omega-alkenyl) cyclopentacarbyl) compound.
Example Two
P REPARATION OF AN (O RGANO ) (( OMEGA -A LKENYL ) C YCLOPENTACARBYL ) S ILANE C OMPOUND
Example 2-1
Ten mmol of allyl-1-indene (in 60 mL of diethyl ether) was reacted with 6.25 mL of butyllithium (1.6 M solution in hexane) to form a first mixture. This first mixture was then stirred for four hours. After stirring, 2.58 grams (10 mmol) of (9-fluorenyl) (dimethyl) (chloro) silane, which is an organosilane, was added to the first mixture to form a second mixture. This second mixture was then stirred overnight. The second mixture was then hydrolyzed with 50 mL of water to form a water phase and an organic phase. The organic phase was then dried over sodium sulfate followed by evaporation of the organic phase to leave the product, which was a yellow oil. This product was ((3-allyl) indenyl) (dimethyl) (9-fluorenyl) silane, which is an (organo) ((omega-alkenyl) cyclopentacarbyl) silane compound.
Example 2-2
Ten mmol of 5-hexenyl-1-indene (in 60 mL of diethyl ether) was reacted with 6.25 mL of butyllithium (1.6 M solution in hexane) to form a first mixture. This first mixture was then stirred for four hours. After stirring, 2.58 grams (10 mmol) of (9-fluorenyl) (dimethyl) (chloro) silane, which is an organosilane, was added to the first mixture to form a second mixture. This second mixture was then stirred overnight. The second mixture was then hydrolyzed with 50 mL of water to form a water phase and an organic phase. The organic phase was then dried over sodium sulfate followed by evaporation of the organic phase to leave the product, which was a yellow oil. This product was ((3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane, which is an (organo) ((omega-alkenyl) cyclopentacarbyl) silane compound.
Example 2-3
Ten mmol of allyl-1-indene (in 60 mL of diethyl ether) was reacted with 6.25 mL of butyllithium (1.6 M solution in hexane) to form a first mixture. This first mixture was then stirred for four hours. After stirring, 3.83 grams (10 mmol) of (9-fluorenyl) (diphenyl) (chloro) silane, which is an organosilane, was added to the first mixture to form a second mixture. This second mixture was then stirred overnight. The second mixture was then hydrolyzed with 50 mL of water to form a water phase and an organic phase. The organic phase was then dried over sodium sulfate followed by concentration of the organic phase. The product was precipitated as a white powder. This product was ((3-allyl) indenyl) (diphenyl) (9-fluorenyl) silane, which is an (organo) ((omega-alkenyl) cyclopentacarbyl) silane compound.
Example 2-4
Ten mmol of 5-hexenyl-1-indene (in 60 mL of diethyl ether) was reacted with 6.25 mL of butyllithium (1.6 M solution in hexane) to form a first mixture. This first mixture was then stirred for four hours. After stirring, 3.83 grams (10 mmol) of (9-fluorenyl) (diphenyl) (chloro) silane, which is an organosilane, was added to the first mixture to form a second mixture. This second mixture was then stirred overnight. The second mixture was then hydrolyzed with 50 mL of water to form a water phase and an organic phase. The organic phase was then dried over sodium sulfate followed by concentration of the organic phase. The product was precipitated as a white powder. This product was ((3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane, which is an (organo) ((omega-alkenyl) cyclopentacarbyl) silane compound.
Example Three
P REPARATION OF A M ETALLOCENE C OMPOUND THAT C ONTAINS AN ( ORGANO ) (( OMEGA -A LKENYL ) C YCLOPENTACARBYL ) S ILANE C OMPOUND
Example 3-1
One gram of ((3-allyl) indenyl) (dimethyl) (9-fluorenyl) silane was mixed with 40 mL of diethyl ether to form a first mixture. This first mixture was stirred with 2 equivalents of n-butyllithium (1.6M in hexane) for about eight hours at room temperature (about 25° C.) to form a second mixture. Thereafter, an equivalent of zirconium tetrachloride was added to the second mixture and stirred overnight to form a first product. This second product was (1-(3-allyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride, a metallocene compound.
Example 3-2
One gram of ((3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane was mixed with 40 mL of diethyl ether to form a first mixture. This first mixture was stirred with 2 equivalents of n-butyllithium (1.6M in hexane) for about eight hours at room temperature (about 25° C.) to form a second mixture. Thereafter, an equivalent of zirconium tetrachloride was added to the second mixture and stirred overnight to form a first product. This second product was (1-(3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride, a metallocene compound.
Example 3-3
One gram of ((3-allyl) indenyl) (diphenyl) (9-fluorenyl) silane was mixed with 40 mL of diethyl ether to form a first mixture. This first mixture was stirred with 2 equivalents of n-butyllithium (1.6M in hexane) for about eight hours at room temperature (about 25° C.) to form a second mixture. Thereafter, an equivalent of zirconium tetrachloride was added to the second mixture and stirred overnight to form a first product. This second product was (1-(3-allyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride, a metallocene compound.
Example 3-4
One gram of ((3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane was mixed with 40 mL of diethyl ether to form a first mixture. This first mixture was stirred with 2 equivalents of n-butyllithium (1.6M in hexane) for about eight hours at room temperature (about 25° C.) to form a second mixture. Thereafter, an equivalent of zirconium tetrachloride was added to the second mixture and stirred overnight to form a first product. This second product was (1-(3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride, a metallocene compound.
Example Four
P OLYMERIZATION OF E THYLENE W ITH A M ETALLOCENE C OMPOUND T HAT C ONTAINS AN ( ORGANO ) (( OMEGA -A LKENYL ) C YCLOPENTACARBYL ) S ILANE C OMPOUND
Example 4-1
About 10 mg of (1-(3-allyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was mixed with 10 mL of methylaluminoxane (30 weight percent in toluene) to form a catalyst complex and then diluted with 10 mL of toluene. The polymerization of ethylene was carried out in a 1 L Buechi laboratory autoclave. The autoclave was filled with 500 mL of pentane and 7 mL of methylaluminoxane. An amount (about 1.8×10 −6 mol) of catalyst complex was then added to the autoclave. The autoclave thermostat was then set to 60° C. and a constant ethylene pressure of 10 bar was applied. The reactor was stirred at 800 rpm. The polymerization was stopped after one hour. About 71 grams of polyethylene was recovered. The molecular weight of the polymer was 350,000. This visometric mean molecular weight was determined with a precision capillary viscometer in Decalin at 135° C. Calibration curves were available for determination of the molecular weight. However, the insoluble components were separated before the measurement of the molecular weight therefore the value determined is not an absolute value, but does give an indication of the trend of the molecular weight. All of the following molecular weights were determined using this technique.
Example 4-2
About 10 mg of (1-(3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was mixed with 10 mL of methylaluminoxane (30 weight percent in toluene) to form a catalyst complex and then diluted with 10 mL of toluene. The polymerization of ethylene was carried out in a 1 L Buechi laboratory autoclave. The autoclave was filled with 500 mL of pentane and 7 mL of methylaluminoxane. An amount (about 1.7×10 −6 mol) of catalyst complex was then added to the autoclave. The autoclave thermostat was then set to 60° C. and a constant ethylene pressure of 10 bar was applied. The reactor was stirred at 800 rpm. The polymerization was stopped after one hour. About 45 grams of polyethylene was recovered. The molecular weight of the polymer was 385,000.
Example 4-3
About 10 mg of (1-(3-allyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride was mixed with 10 mL of methylaluminoxane (30 weight percent in toluene) to form a catalyst complex and then diluted with 10 mL of toluene. The polymerization of ethylene was carried out in a 1 L Buechi laboratory autoclave. The autoclave was filled with 500 mL of pentane and 7 mL of methylaluminoxane. An amount (about 1.5×10 −6 mol) of catalyst complex was then added to the autoclave. The autoclave thermostat was then set to 60° C. and a constant ethylene pressure of 10 bar was applied. The reactor was stirred at 800 rpm. The polymerization was stopped after one hour. About 40 grams of polyethylene was recovered. The molecular weight of the polymer was 580,000.
Example 4-4
About 10 mg of (1-(3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride was mixed with 10 mL of methylaluminoxane (30 weight percent in toluene) to form a catalyst complex and then diluted with 10 mL of toluene. The polymerization of ethylene was carried out in a 1 L Buechi laboratory autoclave. The autoclave was filled with 500 mL of pentane and 7 mL of methylaluminoxane. An amount (about 1.5×10 −6 mol) of catalyst complex was then added to the autoclave. The autoclave thermostat was then set to 60° C. and a constant ethylene pressure of 10 bar was applied. The reactor was stirred at 800 rpm. The polymerization was stopped after one hour. About 76 grams of polyethylene was recovered. The molecular weight of the polymer was 480,000.
Example Five
P OLYMERIZATION OF E THYLENE W ITH A M ETALLOCENE C OMPOUND T HAT C ONTAINS AN ( ORGANO ) (( OMEGA -A LKENYL ) C YCLOPENTACARBYL ) S ILANE C OMPOUND TO FORM A HETEROGENOUS C ATALYST C OMPLEX
Example 5-1
In a Schlenk tube (1-(3-allyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was mixed with methylaluminoxane and toluene to form a catalyst complex. This catalyst complex was then exposed to an ethylene pressure of 0.4 to 0.6 bar to incorporate the catalyst complex into an ethylene polymer chain thereby forming a heterogenous metallocene catalyst.
Example 5-2
In a Schlenk tube (1-(3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was mixed with methylaluminoxane and toluene to form a catalyst complex. This catalyst complex was then exposed to an ethylene pressure of 0.4 to 0.6 bar to incorporate the catalyst complex into an ethylene polymer chain thereby forming a heterogenous metallocene catalyst.
Example 5-3
In a Schlenk tube (1-(3-allyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride was mixed with methylaluminoxane and toluene to form a catalyst complex. This catalyst complex was then exposed to an ethylene pressure of 0.4 to 0.6 bar to incorporate the catalyst complex into an ethylene polymer chain thereby forming a heterogenous metallocene catalyst.
Example 5-4
In a Schlenk tube (1-(3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride was mixed with methylaluminoxane and toluene to form a catalyst complex. This catalyst complex was then exposed to an ethylene pressure of 0.4 to 0.6 bar to incorporate the catalyst complex into an ethylene polymer chain thereby forming a heterogenous metallocene catalyst.
Comparative Example
In a Schlenk tube (9-fluorenyl) (5-hexenyl) (1-indenyl) (methyl) silane zirconium dichloride was mixed with methylaluminoxane and toluene to form a catalyst complex. This catalyst complex was then exposed to an ethylene pressure of 0.4 to 0.6 bar to incorporate the catalyst complex into an ethylene polymer chain thereby forming a heterogenous metallocene catalyst.
The polymerization of ethylene was carried out in a 1 L Buechi laboratory autoclave. The autoclave was filled with 500 mL of pentane and 7 mL of methylaluminoxane. An amount (about 1.8×10 −6 mol) of catalyst complex was then added to the autoclave. The autoclave thermostat was then set to 60° C. and a constant ethylene pressure of 10 bar was applied. The reactor was stirred at 800 rpm. The polymerization was stopped after one hour. About 52 grams of polyethylene was recovered. The molecular weight of the polymer was 270,000.
Discussion of the Examples
In Example 4-2, (1-(3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was used to polymerize ethylene. In the comparative example (9-fluorenyl) (5-hexenyl) (1-indenyl) (methyl) silane zirconium dichloride was used to polymerize ethylene. The main difference between these two compounds is that the former has an omega-hexene group on the indenyl, whereas, the latter has an omega-hexene group on the bridging silane group. While this difference might seem minor to those unskilled in the art, the difference in the molecular weight of the polymers produced by each catalyst is unexpected and unobvious. That is, the former compound polymerizes ethylene to form a polymer having a molecular weight 43 percent greater than the latter.
In Example 4-4, (1-(3-hex-5-enyl) indenyl) (diphenyl) (9-fluorenyl) silane zirconium dichloride was used to polymerize ethylene. In Example 4-2, (1-(3-hex-5-enyl) indenyl) (dimethyl) (9-fluorenyl) silane zirconium dichloride was used to polymerize ethylene. The main difference between these two compounds is that the former has phenyl groups on the bridging silane group, whereas, the latter has methyl groups on the bridging silane group. While this difference might seem minor to those unskilled in the art, the difference in the molecular weight of the polymers produced by each catalyst is unexpected and unobvious. That is, the former compound polymerizes ethylene to form a polymer having a molecular weight 25 percent greater than the latter.
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An (organo) ((omega-alkenyl) cyclopentacarbyl) (silane-bridged) metallocene compound is provided. Polymerization processes therewith are also provided.
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FIELD OF THE INVENTION
The present invention relates to a process for producing pitch (which is a raw material for producing carbon fibers having a high modulus of elasticity), using a petroleum heavy residual oil.
BACKGROUND OF THE INVENTION
In pitches which are used as a raw material for producing carbon fibers having excellent strength and excellent modulus of elasticity, optical anisotropy is observed by a polarizing microscope. More specifically, such pitches are believed to contain a mesophase as described in U.S. Pat. No. 3,974,264. Further, it has recently been disclosed in Japanese Patent Application (OPI) 160427/79 (The term "OPI" as used herein refers to a "published unexamined Japanese patent application)" that carbon fibers having a high modulus of elasticity can be produced with a pitch containing a neomesophase. By heating such pitches for a short time optical anisotropy is observed in them. Further, pitches used as a raw material for carbon fibers need not possess only optical anisotropy but must also be capable of being stably spun. However, it is not easy to produce pitches having both properties. In order to produce carbon fibers having excellent strength and excellent modulus of elasticity, it is not always possible to use any material as the raw material for making pitches. Materials having specified properties have been required.
It should be noted that in many published patents, for example, as described in U.S. Pat. Nos. 3,976,729 and 4,026,788, the raw material is not specified in the claims of patent specifications. Furthermore, such patents indicate that pitches used as a raw material for carbon fibers can be produced only by carrying out thermal modification of a wide variety of raw materials. However, according to the detailed descriptions and examples in such patents the desired pitches can only be produced by using specified raw materials.
For example, U.S. Pat. No. 4,115,527 discloses that substances such as chrysene, etc. or tarry materials byproduced in high temperature cracking of petroleum crude oil are suitable for producing the pitch, i.e., a carbon fiber precursor, but conventional petroleum asphalts and coal tar pitches are not suitable. Further, U.S. Pat. No. 3,974,264 discloses that an aromatic base carbonaceous pitch having a carbon content of about 92 to about 96% by weight and a hydrogen content of about 4 to about 8% by weight is generally suitable for controlling a mesophase pitch. It has been described that elements excepting carbon and hydrogen, such as oxygen, sulfur and nitrogen, should not be present in an amount of more than about 4% by weight, because they are not suitable. Further, Example 1 of the same patent publication discloses that the precursor pitch used has properties comprising a density of 1.23 g/cc, a softening point of 120° C., a quinoline insoluble content of 0.83% by weight, a carbon content of 93.0%, a hydrogen content of 5.6%, a sulfur content of 1.1% and an ash content of 0.044%. Even if a density of 1.23 g/cc in these properties is maintained, it should be noted that it is difficult to obtain conventional petroleum heavy oil having such a high density. Examples as described in the other U.S. Pat. Nos. 3,976,729, 4,026,788 and 4,005,183 also disclose that the pitch is produced with a specified raw material.
The properties of heavy petroleum oils depend essentially upon the properties of crude oils from which they were produced and the process for producing the heavy oil. However, generally, it is rare that heavy oils having the suitable properties described in the above described Examples are produced, and, in many cases, they can not be obtained. Accordingly, in order to produce carbon fibers industrially in a stabilized state, which have excellent strength and excellent modulus of elasticity with petroleum heavy oils, it is necessary to develop a process for producing a pitch wherein the finally resulting pitch has properties which are always within a specified range even if the properties of the raw material for the pitch vary.
SUMMARY OF THE INVENTION
Therefore, one object of this invention is to provide a process for producing a pitch useful as raw material for carbon fibers having an excellent strength and a high modulus of elasticity.
Another object is to provide a process for producing a pitch which can be used for producing carbon fibers having the above excellent properties industrially in a stabilized state.
Still another object is to provide a process for producing a pitch used as raw material for carbon fibers with an easily available petroleum heavy residual oil.
These objects of this invention are effectively accomplished with a process for producing a pitch used as a raw material for carbon fibers which comprises carrying out hydrogenation treatment of a reduced pressure distillate oil prepared by reduced pressure distillation of a petroleum heavy residual oil, carrying out catalytic cracking, distilling the resulting cracking oil to take out a high boiling point fraction having a boiling point of more than 300° C., and carrying out thermal modification thereof.
DETAILED DESCRIPTION OF THE INVENTION
Examples of petroleum heavy residual oils which are used in the present invention include atmospheric pressure distillation residual oils and heavy residual oils from a thermal cracking process such as visbreaking etc. The petroleum heavy residual oils having a boiling point of more than 300° C. is preferred. The atmospheric pressure distillation residual oils are most commonly used.
The above described petroleum heavy residual oils are processed by a reduced pressure distillation apparatus to obtain a distillate fraction. 95% or more of the distillate fraction has a boiling point of 300° to 550° C. (atmospheric pressure). The resulting heavy fraction is subjected to hydrogenation treatment in the presence of a conventional hydrogenating catalyst (e.g., a catalyst containing the sulfides or oxides of such combination of metals as nickel-molybdenum, cobalt-molybdenum, etc.) at a temperature of 300°-410° C., a pressure of 40-150 kg/cm 2 G, a liquid space velocity of 0.5-3.0 per hour, and a ratio of hydrogen/oil of 260-2,000 Nm 3 /Kl. By carrying out this treatment impurities such as sulfur, nitrogen or metals are removed from the reduced pressure distillate oil. The resulting hydrogenated oil preferably has a sulfur content of not more than 0.4% by weight.
When producing carbon fibers having a high modulus of elasticity, it is necessary to remove sulfur in the pitch, because a high modulus of elasticity can not be obtained if the sulfur content of the pitch is large. It is preferred to remove the sulfur prior to the final step, because it is difficult to remove sulfur from the pitch in the final step. It is also necessary to remove metals which form ash by carbonization. Such metals can cause deterioration of the strength or modulus of elasticity of carbon fibers.
The above described hydrogenated oil is subjected to a catalytic cracking reaction in the presence of a catalytic cracking catalyst comprising amorphous silica-alumina, silica-magnesia or zeolite catalysts. The catalytic cracking reaction is carried out at a temperature of 470°-540° C., a pressure of 0.5-5.0 kg/cm 2 G and a ratio of catalyst/oil of 5-15 parts by weight. A high boiling point fraction having a boiling point of more than 300° C. is obtained by distillation of the resulting cracking oil.
The resulting high boiling point fraction is subjected to thermal modification at a temperature of 390°-430° C. for 1-30 hours, by which a pitch which can be used as a raw material for making carbon fibers having a high modulus of elasticity can be produced. In the residual heavy fraction after the catalytic cracking reaction, the difference in properties due to any disparity in the raw material becomes smaller due to the effects of the catalytic reaction together with the above described hydrogenation treatment. Further, the residual heavy fraction developes a chemical composition comprising a large amount of aromatic compounds.
The actual conditions required to obtain the best results in the above described series of steps depend on the properties of the petroleum heavy residual oil which is used as a starting material as well as the properties of the pitch which will be used as a raw material for making carbon fibers as the final product. By carrying out a series of these steps any difference due to properties of the starting material becomes smaller. Therefore, by carrying out these steps, it is possible to keep the properties of the pitch which is used as a raw material for making carbon fibers within a specified range. Since the properties of the petroleum heavy residual oil (used as the starting material) are fairly different from others because of the crude oil, it is generally difficult to produce pitch (which can be successfully used to make carbon fibers having high strength and high modulus of elasticity and specified properties) by only carrying out the thermal modification of such petroleum heavy oil at 380° C. to 450° C.
However, in accordance with the present invention, a pitch which can be used as a raw material for carbon fibers having high modulus of elasticity can be produced industrially and stably with various kinds of petroleum heavy residual oils. The pitch is produced by carrying out a series of processings comprising reduced pressure distillation→hydrogenation treatment→catalytic cracking→distillation→thermal modification. By carrying out these steps it is possible to use a raw material which could not be used for producing a pitch for carbon fibers in accordance with prior processes.
In the following, the present invention is illustrated in greater detail by examples. However, this invention is not limited to these examples.
EXAMPLE 1
An atmospheric pressure distillation residual oil of Middle East crude oil (A) was subjected to reduced pressure distillation to obtain a fraction having a boiling point of 300°-550° C. (an atmospheric pressure). The resulting reduced pressure distillation fraction was subjected to hydrogenation treatment in the presence of a cobalt-molybdenum catalyst. The hydrogenation was carried out at a temperature of 370° C., a pressure of 60 kg/cm 2 G, a liquid space velocity of 1.9 per hour and a ratio of hydrogen to oil of 360 Nm 3 Kl. The hydrogenated oil was subjected to a catalytic cracking reaction with using a zeolite catalyst. The cracking was carried out at a temperature of 500° C., a pressure of 1.5 kg/cm 2 G and a catalyst/oil ratio of 9 parts by weight. The residual heavy oil obtained from the catalytic cracking reaction was distilled to obtain a high boiling point fraction having a boiling point of more than 300° C. The high boiling point fraction was subjected to thermal modification at a temperature of 410° C. for 20 hours to obtain a pitch which could be used as a raw material for making carbon fibers.
The properties of the atmospheric distillation residual oil of Middle East crude oil (A) used as a raw material, and the properties of the oil after hydrogenation treatment, as well as the properties of the high boiling point fraction after catalytic cracking and the properties of the resulting pitch are shown in Table 1.
Carbon fibers were obtained by melt spinning the above described pitch at 360° C., infusiblizing at 260° C. in air and carbonizing at 1,000° C. The resulting carbon fibers had a tensile strength of 11 tons/cm 2 and a modulus of elasticity of 1,300 tons/cm 2 . When carbonized fibers prepared by carbonizing at 1,000° C. were additionally graphitized at 1,900° C., the resulting carbon fibers had a tensile strength of 15 tons/cm 2 and a modulus of elasticity of 2,300 tons/cm 2 .
EXAMPLE 2
An atmospheric pressure distillation residual oil of Middle East crude oil (B) was subjected to reduced pressure distillation to obtain a fraction having a boiling point of 300°-550° C. (an atmospheric pressure). The resulting reduced pressure distillation fraction was subjected to hydrogenation treatment in the presence of a cobalt-molybdenum catalyst. The hydrogenation was carried out at a temperature of 380° C., a pressure of 60 kg/cm 2 , a liquid space velocity of 1.8 per hour and a ratio of hydrogen per oil of 400 Nm 3 /Kl. The hydrogenated oil was subjected to a catalytic cracking reaction with a zeolite catalyst. The cracking was carried out at a temperature of 500° C. and a pressure of 1.5 Kg/cm 2 and a catalyst/oil ratio of 9 parts by weight. The residual heavy oil obtained from the catalytic cracking reaction was distilled to obtain a high boiling point fraction having a boiling point of more than 300° C. The high boiling point fraction was subjected to heat treatment at a temperature of 420° C. for 10 hours to obtain a pitch which could be used as a raw material for making carbon fibers.
The properties of the atmospheric pressure distillation residual oil of Middle East crude oil (B) used as the raw material, and the properties of the oil after hydrogenation treatment, as well as the properties of the high boiling point fraction after catalytic cracking treatment and properties of the pitch are shown in Table 1.
COMPARATIVE EXAMPLE 1
An atmospheric pressure distillation residual oil of Middle East crude oil (A) was subjected to thermal modification at a temperature of 410° C. for 18 hours. The properties of the atmospheric pressure distillation residual oil of Middle East crude oil (A) used as a raw material and the properties of the pitch are shown in Table 1.
Fibers were obtained by melt spinning the pitch at 350° C., infusiblizing in the air and carbonizing at 1,000° C. The fibers obtained had a tensile strength of 1.9 tons/cm 2 and a modulus of elasticity of 140 tons/cm 2 .
COMPARATIVE EXAMPLE 2
An atmospheric pressure distillation residual oil of Middle East crude oil (A) was subjected to reduced pressure distillation to obtain a fraction having a boiling point in the range of 300°-550° C. The resulting reduced pressure distillation fraction was subjected to thermal modification at a temperature of 410° C. for 20 hours. The yield of the pitch obtained after the heat treatment was low and it was not possible to obtain the pitch in an amount necessary to examine its properties.
COMPARATIVE EXAMPLE 3
An atmospheric pressure distillation residual oil of Middle East crude oil (A) was subjected to reduced pressure distillation to obtain a fraction having a boiling point in the range of 300°-550° C. (an atmospheric pressure). The resulting reduced pressure distillation fraction was subjected to a catalytic cracking reaction using a zeolite catalyst. The cracking was carried out at a temperature of 500° C., a pressure of 1.5 kg/cm 2 G and a catalyst/oil ratio of 9 parts by weight without the hydrogenation treatment. The residual heavy oil obtained by the catalytic cracking reaction was distilled to obtain a high boiling point fraction having a boiling point of more than 300° C. The high boiling point fraction was subjected to thermal modification at a temperature of 410° C. for 20 hours to obtain a pitch.
The properties of the atmospheric distillation residual oil of Middle East crude oil (A) used as a raw material, the properties of the high boiling point fraction after catalytic cracking as well as the properties of the resulting pitch are shown in Table 1.
The pitch obtained was subjected to melt spinning at about 365° C. However, the fiber obtained by the melt spinning broke frequently as compared with the pitch used as a raw material of Example 1. Accordingly, the melt spinning was very difficult to carry out. Further, the melt-spun fiber was infusiblized at 260° C. in the air and then carbonized at 1,000° C. The resulting product had a tensile strength of 9 tons/cm 2 and a modulus of elasticity of 1,010 ton/cm 2 . When the carbonized fibers prepared by carbonized at 1,000° C. were additionally graphitized at 1,900° C., they had a tensile strength of 10 tons/cm 2 and a modulus of elasticity of 1,610 ton/cm 2 .
TABLE 1__________________________________________________________________________ Comparative Comparative Comparative Example Example example example exampleProperties 1 2 1 2 3__________________________________________________________________________Properties of atmosphericdistillation residual oilSpecific gravity @ 15/4° C. 0.969 0.990 0.969 0.969 0.969Kinematic viscosity @ 50° C. cSt 770 2189 770 770 770Sulfur content - wt % 2.9 4.3 2.9 2.9 2.9Residual carbon content wt % 9.9 14.1 9.9 9.9 9.9Ash wt % 0.01 0.01 0.01 0.01 0.01Properties after hydro-genation treatmentSpecific gravity @ 15/4° C. 0.881 0.887 0.915* 0.915*Kinematic viscosity @ 50° C. cSt 15.2 16.3 30.0* 30.0*Sulfur content wt % 0.3 0.3 1.8* 1.8*Residual carbon content wt % 0.05 0.06 0.27* 0.27*Ash wt % 0.00 0.00 0.00* 0.00*Properties of high boilingpoint fraction after catalyticcracking reactionSpecific gravity @ 15/4° C. 0.990 1.001 1.058Kinematic viscosity @ 50° C. cSt 10.2 13.1 14.5Residual carbon content wt % 1.9 2.0 5.2Sulfur content wt % 1.2 1.4 2.7Carbon content wt % 87.2 87.2 86.8Hydrogen content wt % 10.9 10.6 9.6Properties of pitchSpecific gravity @ 25/25° C. 1.31 1.32 1.32 1.32Softening point °C. 330 330 320 335Quinoline insoluble 20.1 22.5 23.4 24.0content wt %Spinnability good good bad bad__________________________________________________________________________ Note: *properties after reduced pressure distillation
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
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A process for producing a pitch is disclosed. The process involves distilling a heavy petroleum oil under reduced pressure to obtain a distillate, the distillate is hydrogenated to obtain a hydrogenated oil which is subjected to catalytic cracking. The cracked oil is subjected to distillation to obtain a high boiling point fraction having a boiling point of more than 300° C. The high boiling point fraction is subjected to thermal modification in order to obtain the pitch. The pitch can be utilized in order to produce carbon fibers of high quality. By utilizing the process a greater variety of starting materials can be utilized in order to produce the pitch which is utilized to produce high quality carbon fibers.
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BACKGROUND OF THE INVENTION
This invention relates to space dyeing apparatus and more particularly to apparatus for applying dye to a plurality of yarn strands in a preselected array or pattern of color, spacing and length in a continuous manner and for selectively controlling the array, spacing and amount of dye applied to the yarn.
In some fabrics, such as carpets, it is desirable to provide yarns which have a color pattern varying along their lengths. Such yarns have come to be known as space-dyed yarns, and apparatus and processes for coloring such yarn are known as space-dyeing apparatus and processes. Carpet fabrics made from yarns of this type generally have a multicolor effect with no visible pattern. Various space-dyeing methods and apparatus have been known in the prior for some period of time. See for example, Epstein U.S. Pat. No. 2,573,097. Such methods and apparatus include systems where a number of yarns pass over a series of dye applicator rollers or drums which are charged with dyes of various colors. The yarns generally are controlled during passage over the drums so as to maintain clearance with the surfaces except when it is desired to color a portion of the yarn. When a portion of the yarn is to be colored the yard is depressed by a presser member to cause the yarn to be pressed against the surface of the selected dye applicator roller. The presser member may be a piston or plunger reciprocating above the dye applicator roller for forcing the yarn directly against the periphery of the dye applicator roller as disclosed in Farrer et al U.S. Pat. No. 3,503,232 and Worth et al U.S. Pat. No. 3,879,966, or may be a series of pads mounted on a rotating drum, the pads forcing the yarn against the dye applicator roller as in Keown U.S. Pat. No. 3,541,958. Thus, in the prior art the yarn is stamped, impacted or hammered against the dye applicator roller. If the plunger or pad is held against the yarn for too long a time, the feeding of the yarn may be impaired. Thus, the amount of dye applied to the yarn during each impact is limited.
In Farrer et al and Worth et al the speed of the dyeing is limited because of the limitations on the reciprocating elements including the cycling and the acceleration forces involved.
In the Keown and Worth et al patents the yarn is precolored with a base color and the stamping effectively results in the dye applicator rollers applying spots of secondary color on the precolored yarn. Complicated control systems, both mechanical and electrical, are proposed for varying the spacing between the secondary colors applied. In Farrer et al random repeat may be obtained by an electro-mechanical system of cams and switches for controlling solenoids which act as plungers. Such complicated control systems were apparently proposed because the stamping, impacting or hammering of the yarn only applies color to the yarn during that limited portion of the cycle when the yarn is disposed between the piston, plunger or pad and the dye applicator roller.
When a pattern change or change in variegation of colors along the yarns is desired, Keown appears to require a major overhaul or replacement of elements and Worth et al requires replacement or reprogramming of electrical circuitry. Only Fatter et al requires a repositioning of mechanical members which form raised portions on the surface of cylindrical cams and thus can be performed by non-highly skilled maintenance personnel. However, such repositioning of cam elements merely effects the engagement of the plungers which force the yarns against the dye applicator rollers which include the aforesaid limitations. Moreover, since the cam elements act to control micro switches which activate the plungers, and the switches may open and close a number of times each revolution, switch maintenance and replacement may be common.
SUMMARY OF THE INVENTION
Consequently, it is a primary object of the present invention to provide space-dyeing apparatus wherein a plurality of yarn strands may be continuously colored by application of a number of different yarn colors to provide various color arrays along the yarn strands.
It is another object of the present invention to provide yarn space-dyeing apparatus wherein the pattern or array of colors along a plurality of strands of yarn fed through the apparatus may be readily and conveniently changed.
It is a further object of the present invention to provide space-dyeing apparatus wherein a plurality of yarn strands pass over a number of dye applicator rolls, each applicator roll being positioned within a dye pan containing a different respective color, the apparatus having pattern rolls including repositionable replaceable slats for deflecting the strands of yarn onto the peripheries of the dye applicator rolls.
It is a still further object of the present invention to provide space-dyeing apparatus wherein a plurality of yarn strands pass over a number of dye applicator rolls positioned within respective dye pans, the apparatus having pattern rolls including repositionable slats dispersed within selective slots in the peripheries thereof for engaging and deflecting the strands of yarn onto the peripheries of the dye applicator rolls, the amount of dye on the yarn and the spacing of the colors along the yarn being controlled by varying independently the speed of the dye applicator rolls and the speed of the pattern rolls while the placement of the colors is varied by changing the circumferential disposition of the slats on the pattern rollers.
Accordingly, the present invention provides a method and apparatus wherein a plurality of strands of yarn are fed and pass over a series of dye applicator or lick rolls, each of which is partly submerged in a dye pan or vat containing a different color and driven by a variable speed drive to apply dye to the yarn when the yarn is forced onto the dye applicator rolls. Depending upon the speed of the dye applicator rolls, different amounts of dye are applied to the yarns which travel in a horizontal plane. Above and offset relative to each dye applicator roll is a yarn pattern or control roll which carries slats in a circumferential array extending from the periphery of the respective pattern rolls for deflecting the yarn strands onto the respective dye applicator rolls. The slats in each roll may be positioned in various slots in the pattern rolls to determine the pattern of color on the yarn. Variable speed drive means drive the pattern rolls independently of variable speed drive means that drive the dye applicator rolls. The length of yarn colored by a particular color may be controlled by the speed of the pattern rolls relative to the speed that the yarns are fed, and the amount of dye applied to the yarn may be controlled by the speed of the dye applicator rolls relative to the speed at which the yarn is fed through the apparatus.
The slats are positionable within any of a plurality of slots formed longitudinally within the peripheries of the respective pattern rolls and may be changed readily to vary the pattern array. Since the slats deflect the yarn onto the surfaces of the dye applicator rolls rather than stamp the yarn against the rolls a greater amount of dye may be applied to the yarn while the length of the yarn containing a particular color may be increased without hammering the dye applicator rolls.
BRIEF DESCRIPTION OF THE DRAWINGS
The particular features and advantages of the invention as well as other objects will become apparent from the following description taken in connection with the accompanying drawings in which:
FIG. 1 is a side elevational view with portions thereof removed of dyeing apparatus constructed in accordance with the present invention illustrated in an inoperative position;
FIG. 2 is an enlarged vertical cross sectional view taken substantially along line 2--2 of FIG. 1 but with the apparatus in the operative position;
FIG. 3 is a fragmentary vertical cross sectional view taken substantially along line 3--3 of FIG. 2;
FIG. 4 is a fragmentary perspective view illustrating a pattern roll with the end caps removed; and
FIG. 5 is a fragmentary perspective view of a portion of the apparatus illustrating a pattern roll and a dye applicator roll.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, dyeing apparatus 10 constructed in accordance with the principles of the present invention include an upper head 12 and a lower head 14 carried on a supporting base plate 16. As illustrated, the base plate 16 together with the heads may have a substantially rectangular configuration, the base plate preferably including upstanding legs 18 supported on wheels 20 so that the apparatus may be mobile if desired. The upper head 12 includes a pair of laterally spaced apart beam members 22, 24 forming an upper frame while the lower head 14 includes a similar pair of laterally spaced apart beam members 26, 28 forming a lower frame. Each upper beam 22, 24 has an externally directed lateral flange 30, 32 respectively while each lower beam 26, 28 has a similar flange 34, 36 respectively, the flanges 30, 32 being disposed on the respective flange 34, 36 in the operative position illustrated in FIG. 2. In the inoperative position of the apparatus, the flanges 30, 32 are separated from the flanges 34, 36 as illustrated in FIG. 1. In order to raise and separate or lower and close the upper head relative to the lower head a lead screw 38 is provided adjacent each corner of the upper head 12 threaded through a number of blocks and collars in the upper head 12 and in the lower head 14 in conventional manner and secured to a stop collar 40 below the lower head. Each lead screw carries a sprocket 42 about which a chain 44 is trained. One of the lead screws, as illustrated in FIG. 1, is secured to a sleeve 46 which is formed together with a crank arm and handle 48 so that manual rotation of the handle 48 rotates all of the lead screws 38 and raises or lowers the upper head 12 selectively relative to the lower head 14.
Rotatably journalled in bearings, such as bearings 50 illustrated in FIG. 2, mounted on the interior face of the beams 26, 28 of the lower housing 14 is a plurality of pulleys 52 and 54. The axes of the pulleys 52 are disposed above and offset in staggered fashion relative to the axes of the pulleys 54 as illustrated in FIG. 1. Each pulley 52 is coupled to one end of a respective, preferably stainless steel, dye applicator roll 56 adjacent to and externally of each beam 26, 28, while the pulleys 54 alternate from one side to the other, i.e., alternate pulleys 54 are adjacent to and external of the beam 26 while the remaining pulleys are externally of the beam 28. Each dye applicator roll 56 is disposed between the beams 26 and 28 within a corresponding dye pan 58 having sidewalls 60 which are adjustably and removably supported on channel beams 62 fastened to the base plates 16. The rolls 56 have or are coupled to axles 64 which exit through the sidewalls of the respective pan in sealed fashion for coupling to the pulleys 52 as aforesaid. The pulleys 54 act as idler pulleys for purposes hereinafter made clear.
Mounted in the base below the base plate 16 is a variable speed motor 66, which may be a motor connected to a variable speed drive, which is coupled to a pulley 68 for driving the same. A timing belt 70 is trained about the pulley 68 and another pulley 72 journalled in the lower head 14 above the pulley 68, the pulley 72 being mounted on a common shaft with another pulley 74 disposed at the same side of the apparatus as the adjacent idler pulley 54, i.e., adjacent the beam 26 as illustrated in FIG. 1. A timing belt 75 is trained about the pulley 74, the adjacent idler pulley 54 and the adjacent applicator roll coupled pulley 52 thereby to rotatably drive the applicator roll 56 coupled thereto. The pulley 52 at the opposite end of that roll, i.e., the end adjacent the beam 28, drives the pulley on that same side of the next adjacent applicator roll by means of a belt trained about those two pulleys and the idler roll disposed therebetween. Each subsequent applicator roll 56 is driven in a similar manner from the preceding applicator roll, the driving pulley alternating from side-to-side. It may be noted that the applicator rolls rotate in the direction opposite to that in which yarn strands Y are fed at the upper periphery of the rolls, i.e., the yarns are fed from the left to the right in FIG. 1 while the rolls 56 rotate counter-clockwise. Although any number of selected applicator rolls may be utilized in the dyeing apparatus of the present invention, six such rolls are illustrated in the preferred embodiment illustrated in the drawings, each applicator roll 56 being disposed within a respective dye pan 58 containing a particular dye color which preferably differs in each pan.
Mounted in the lower housing behind each dye application roll 56 and in front of the first dye applicator roll is a yarn support member 76 of a small cylindrical form. Each yarn support member, which is preferably formed from stainless steel, is disposed with its upper peripheral surface at or slightly above that of the dye applicator rolls so that yarn may be fed over the members 76, without contacting the dye applicator rolls with pressure. Thus, the yarn may be fed over the dye applicator rolls without having dye applied to it.
Mounted on the beams 22 and 24 of the upper head 12 are a plurality of pairs of bearings 78, each of which rotatably supports a pulley 80 at each exterior side of the respective beam 22, 24 in a similar manner to the bearings 50 and the pulleys 52 of the lower head 14. Coupled to and between each pair of pulleys 80 and disposed intermediate the beams 24 is a respective pattern roll 82, there being one pattern roll 82 corresponding to each dye applicator roll 52 for reasons hereinafter described in detail. Additionally, a plurality of idler pulleys 84 similar to the idler pulleys 54 are mounted on respective axes above and offset from the axes of the pulleys 80, alternate idler pulleys 84 being disposed adjacent to and externally of the beam 22 and the others being disposed adjacent to and externally of the beam 24. A timing belt 86 is trained about each idler pulley 84 and the pulleys 80 of the two adjacent pattern rolls at the same side of the apparatus in the same manner as the pulleys and belts in the lower head. One of the pulleys 80 at one end of the apparatus, i.e, the rear end as illustrated in FIG. 1, is driven by a timing belt 88 trained about that pulley and another pulley 90 mounted on the output shaft of a variable speed motor 92, or a motor connected to a variable speed drive, secured by bracket means 94 to the beam at the corresponding side of the apparatus, such as the beam 22 as illustrated. Thus, the motor 92 drives the pattern rolls 82 at a selected speed independent of the speed at which the dye applicator rolls 56 are driven by the motor 66. The direction in which the rolls 82 rotate is the same as that of the dye applicator rolls 56 so that at the lower peripheries the rolls 82 move in the same direction as that in which the yarn is fed.
As illustrated in FIGS. 3 and 4, the pattern rolls 82 comprise cylindrical members having an integral axis 96 at each end and preferably formed from stainless steel. Machined radially into the periphery of each roll 82 extending longitudinally the length of the rolls is a plurality of equally spaced apart slots or grooves 98, each slot being adapted to receive a control slat 100. Although the number of slats may vary with the size of the roll and range up to approximately 36, in a prototype apparatus the diameter of the rolls 82 were in the order of approximately 3 inches and contained 24 slots, each slot having a depth of approximately 0.25 inch and a width of approximately 0.125 inch, while each slat was approximately 0.75 inch in width and seated in the selected slots so as to extend approximately 0.50 inch beyond the periphery of the rolls 82. The number of slats 100 and the selected slots within which the slats are positioned is dependent upon the dyeing or printing pattern to be applied to the yarn since the slats deflect and force the yarn against the dye applicator roll corresponding to that pattern roll.
In order to maintain the slats 100 within the selected slots 98, the periphery at the ends of the pattern rolls 82 are threaded as illustrated at 102 in FIGS. 2 and 4 for threadedly receiving a respective internally threaded cap 104, the cap having an annular rim 106 including an internal diameter adapted for receiving the slats 100 mounted in the roll 82 within the annulus. The caps 104 preferably are formed from two half or split ring members connected together by screw means (not illustrated) or the like so that the slats may be removed, additional slats inserted, and/or repositioned without disassembly and removal of the roll 82 from the upper housing.
As illustrated in FIG. 3, the axis of each pattern roll 82 is offset from the axis of the corresponding dye applicator roll 56. For a pattern roll with the aforesaid dimensions and a dye applicator roll having a diameter approximately equal to that of the dye applicator roll, the offset is approximately 1 inch. Thus, the slats 100 carried by a particular pattern roll 22 do not stamp or hammer the yarn into the dye applicator roll, but deflect the yarn Y from its normal path over the yarn supports 76 into engagement with the cooperating dye applicator roll 56. Thus, feeding of the yarn is not retarded when a series of adjacent slats deflect the yarn onto an applicator roll to effect a substantial amount of dye of a particular color distributed by wiping onto the yarn. Nor does it retard feeding nor stretching of the yarn when a first color is wiped on at a first station at substantially the same time as other colors are wiped on at other stations.
In practicing the method of the present invention, the yarn is fed through the apparatus by conventional means such as feed rolls 108 at a selected speed. The speed of the pattern rolls as effected by the drive system including the motor 92 in connection with the speed of the yarn through the apparatus determines the length or space colored by a particular dye. The speed of the dye applicator rolls 56 as determined by the lower head drive system including the motor 66 together with the speed of the yarn through the apparatus controls and determines the amount of dye applied to the yarn. If more dye is needed on the yarn, the speed of the applicator rolls 56 is increased and vice versa. If the space filled by a particular color on the yarn is to be shortened, the pattern roll speed is increased and vice versa. Repositioning slats so that more or less slats are disposed in a particular pattern roll and the position of the slats in a particular pattern roll, determines the location of a particular color and in conjunction with the speed of the pattern roll determines the space on the yarn filled by a particular color. The direction of rotation of the rolls 56 and the rolls 82 is the same so that the applicator rolls drive dye into the yarn fibers and the slats 100 deflect the yarn toward the rolls 56. Since the slats upon contact with the yarn strands move in the same direction as the yarn, wear on the slats is held to a minimum.
Accordingly, there is provided a dyeing apparatus which effects space dyeing of yarn and controls the pattern of the space dyeing by a simple mechanical control comprising replaceable slats in the surface of the pattern rolls. Additionally, the amount of dye and spacing of colors of yarn may be readily controlled merely by changing the speeds of the pattern rolls and the dye applicator rolls independently of each other.
Numerous alterations of the structure herein disclosed will suggest themselves to those skilled in the art. However, it is to be understood that the present disclosure relates to the preferred embodiment of the invention which is for purposes of illustration only and not to be construed as a limitation of the invention. All such modifications which do not depart from the spirit of the invention are intended to be included within the scope of the appended claims.
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A method and apparatus for space dyeing a plurality of strands of yarns which are fed over a series of dye applicator rolls. Each roll is rotated in a partly submerged condition in a dye pan containing a different color. Above and offset relative to each dye applicator roll is a yarn pattern roll which carries a number of slats in a circumferential array extending beyond the periphery of the pattern rolls for contacting the yarn strands. The slats sequentially engage and deflect the yarn strands onto the surface of the respective dye applicator rolls. The slats may be positioned in selected slots in the pattern rolls to determine the pattern of color applied to the yarn. Variable speed drives rotate the dye applicator rolls and the pattern rolls independently of each other to effect the spacing of the colors and the amount of dye received by the yarn strands.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
REFERENCE TO SEQUENCE LISTING, A TABLE, OR A COMPUTER PROGRAM LISTING COMPACT DISC/APPENDIX
[0003] Not Applicable
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] This invention relates to a method of cleaning rubber off of runways that is free of the environmentally-unpreferred surfactant class known as alkylphenol ethoxylates (“APE”) or more generally, alkylphenol alkoxylates (“APA”), utilizing a novel cleaning composition.
[0006] 2. Prior Art
[0007] It is well-known that when airplanes land on runways that at the moment of impact a differential in relative speed between the airplane's wheels and the runway causes some of the rubber to be transferred to the runway, making basically a skid mark on the runway surface. After enough landings, the number of skid marks gets so high that the frictional characteristics of the runway are reduced. When this happens, and the runway is wet, there is a very real danger of airplanes being unable to stop during landing, and crashing off the end of the runway, with loss of life, injury and damage to the airplane.
[0008] In the industry, there are two standard approaches to preventing this type of catastrophe. The first is high-pressure blasting utilizing ambient-temperature or high-temperature water, and the second is chemical solution cleaning, usually involving scrubbing with steel and/or nylon brushes followed by rinsing while scrubbing, but sometimes involving rinsing with pressurized water.
[0009] Typical water blasting operations use pressures ranging from 8,000 to 32,000 p.s.i. They literally blast away the build-up. Frequently,the pressure required to remove the rubber is greater than the cohesive strength of the concrete or asphalt binder. Therefore, this method of cleaning can cause damage to the pavement microtexture resulting in shortened runway life as well as reduced breaking action.
[0010] Therefore, in many situations, chemical cleaning is the preferred solution. As a non-destructive method of cleaning, alkaline chemical rubber removers have been increasingly used.
[0011] For a cleaning operation involving chemical cleaners, typically 100 to 600 gallons of runway cleaner is sprayed on the center 50 foot section of approximately 1,000-2,000 linear feet per runway end, for a rate of up to 0.055 gallons per square foot. This is enough to wet the runway, but not cause the cleaner to run off the runway.
[0012] The material is agitated for several hours with a runway broom or brooms. Then, the cleaner is rinsed to the edges using typically 50-100 gallons of rinse water per gallon of cleaner. Rinsing takes an additional one to three (1-3) hours, during which time the rinse water typically soaks into the grassy soil adjacent to the runway. Although the organic components of many runway cleaners will eventually biodegrade, some components are more easily handled by the environment than others.
[0013] Many cleaning compositions involve nonionic detergent components that are alkylphenol alkoxylates (“APA”), usually alkylphenol ethoxylates (“APE”), for example a propylene trimer-modified phenol with 9-10 moles of ethylene oxide per alkylphenyl unit. This material is known as nonylphenol ethoxylate, and a number after the initials NP designate the number of ethylene oxide units per NP unit, e.g. NP-9 or NP-10. Indeed, NP-10 is considered a workhorse nonionic surfactant.
[0014] However, the use of APA's or usually APE's in cleaning compositions is becoming increasingly unpopular from an environmental perspective. As an example, the EPA and several private groups have listed formulation parameters for “environmentally acceptable” cleaning formulations under the banner of “Design for the Environment” (“DfE”). In GS-37—Green-Seal Environmental Standard for General-Purpose, Bathroom Glass and Carpet Cleaners Used for Industrial and Institutional Purpose, Third Edition Feb. 27, 2006, Section 4.13—Prohibited Ingredients, alkylphenol ethoxylates are listed as a prohibited ingredient class. This means that any formulation containing them cannot pass this standard. Nonylphenol itself has been designated as a “marine pollutant” by the Department of Transportation, in 29 CFR Part 172.101 Appendix B.
[0015] Recently, these APE surfactants have also come under increasing scrutiny due to the potential of some members of the series, as well as possible biodegradation intermediates, to act as hormone minics and/or endocrine disruptors.
[0016] Thus, a cleaner without these powerful, effective, but increasingly environmentally-suspect workhorse raw materials is desirable. However, it is not obvious that there are ready replacements for them. The presence of both alkyl- and aryl components to the surfactants create some unique cleaning potential. Also, the more-acidic nature of the phenolic group ensures that the ethoxylates have a much narrower product distribution than, for example, linear alkyl ethoxylates (or in general alkoxylates—“LAA”'s). Thus LAA's typically have much more unreacted alcohol than APE's. This unreacted alcohol could potentially be a burden on the formulation as a whole, increasing the instability of it, and diverting some of the detersive action into simply preventing separation of the unreacted alcohol.
[0017] Therefore, although there are many decades of experience with APE's, an environmentally-preferable method of cleaning runways is desirable. It is the object of the instant invention to provide a method of chemically cleaning runways that does not involve APE's or more generally APA's.
BRIEF DESCRIPTION OF THE INVENTION
[0018] It is an object of the instant invention to provide a method of cleaning rubber off of rubber-soiled runway surfaces which does not employ APE's. This is surprisingly accomplished by utilizing the following method:
1) exposing a soiled runway surface to an APA-free cleaning composition by spraying, dumping or otherwise wetting the surface with the cleaner, 2) scrubbing for an efficacious amount of time using steel- and/or nylon-bristled brooms, followed by 3) rinsing using an appropriate amount of water while scrubbing, or alternatively after an efficacious amount of time of scrubbing, utilizing pressurized water to remove any detritus, or alternatively utilizing pressurized water to remove rubber and any detritus after exposing the runway to the APA-free cleaner without scrubbing, said APA-free cleaning composition comprising:
a. A linear alcohol alkoxylate (“LAA”) containing at least one carbon chain of length 4-20 and at least one oxyethylene or oxypropylene group, said LAA being from about 0.1 to about 10 percent by weight of the formulation as a whole, b. At least one coupling agent selected from the group consisting of: a phosphate ester of a linear alcohol alkoxylate containing at least one carbon chain of length 4-20 and at least one oxyethylene or oxypropylene group, the molecular ratio of LAA to phosphorous being from about 0.1 to about 2, alkylaromatic sulfonic acids and/or their salts, such as sodium xylene sulfonate; said coupling agent being from about 0.1 to about 10 percent by weight of the whole, c. At least one solvent selected from the group containing glycol ether solvents, solvent terpenes, alkyl esters, terpene alcohols, said solvent or solvent combination being from about 0.1 to about 10 percent by weight of the whole, d. At least one builder selected from the group containing hydroxides, silicates, phosphates, oligophosphates, polyphosphates, alkyl phosphonic acids, borates, carbonates or bicarbonates of sodium, potassium, lithium or cesium, said builder or builder combination being from about 0.1 to about 15 percent by weight (on an active ingredient basis) of the whole, e. Optional additional surfactants selected from the group containing cationic, anionic, nonionic, amphoteric, amine oxide or diethanolamide surfactants, said optional surfactant or surfactant combination being from about 0.1 to about 10 percent by weight of the whole, f. Optionally a hardness ameliorating agent selected from the group containing ethylenediamine tetra acetic acid, ethylenediamene triacetic acid, nitrilo-tris-acetic acid, glucuronic acid, gluconic acid, erythorbic acid, and citric acid and/or the sodium, potassium, lithium or cesium salts of these or mixtures and combinations of these, said hardness ameliorating agent being from about 0.1 to about 10 percent by weight of the whole, and g. The balance being water.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
[0029] Not Applicable
DETAILED DESCRIPTION OF THE INVENTION
[0030] It is an object of the instant invention to provide a method of cleaning rubber off of rubber-soiled runway surfaces which does not employ APE's. This is surprisingly accomplished by utilizing the following method:
1) exposing a soiled runway surface to an APA-free cleaning composition by spraying, dumping or otherwise wetting the surface with the cleaner, 2) scrubbing for an efficacious amount of time using steel- and/or nylon-bristled brooms, followed by 3) rinsing using an appropriate amount of water while scrubbing, or alternatively after an efficacious amount of time of scrubbing, utilizing pressurized water to remove any detritus, or alternatively utilizing pressurized water to remove rubber and any detritus after exposing the runway to the APA-free cleaner without scrubbing, said APA-free cleaning composition comprising:
a. A linear alcohol alkoxylate (“LAA”) containing at least one carbon chain of length 4-20 and at least one oxyethylene or oxypropylene group, said LAA being from about 0.1 to about 10 percent by weight of the formulation as a whole, b. At least one coupling agent selected from the group consisting of: a phosphate ester of a linear alcohol alkoxylate containing at least one carbon chain of length 4-20 and at least one oxyethylene or oxypropylene group, the molecular ratio of LAA to phosphorous being from about 0.1 to about 2, alkylaromatic sulfonic acids and/or their salts, such as sodium xylene sulfonate, and/or alkylamphoteric surfactants; said coupling agent being from about 0.1 to about 10 percent by weight of the whole, c. At least one solvent selected from the group containing glycol ether solvents, solvent terpenes, alkyl esters, terpene alcohols, said solvent or solvent combination being from about 0.1 to about 10 percent by weight of the whole, d. At least one builder selected from the group containing hydroxides, silicates, phosphates, oligophosphates, polyphosphates, alkyl phosphonic acids, borates, carbonates or bicarbonates of sodium, potassium, lithium or cesium, said builder or builder combination being from about 0.1 to about 15 percent by weight (on an active ingredient basis) of the whole, e. Optional additional surfactants selected from the group containing cationic, anionic, nonionic, amine oxide or diethanolamide surfactants, said optional surfactant or surfactant combination being from about 0.1 to about 10 percent by weight of the whole, f. Optionally a hardness ameliorating agent selected from the group containing ethylenediamine tetra acetic acid, ethylenediamene triacetic acid, nitrilo-tris-acetic acid, glucuronic acid, gluconic acid, erythorbic acid, and citric acid and/or the sodium, potassium, lithium or cesium salts of these or mixtures and combinations of these, said hardness ameliorating agent being from about 0.1 to about 10 percent by weight of the whole, and g. The balance being water.
[0041] The instant invention of necessity involves wetting of the surface to be cleaned, penetration of the cleaning solution between the rubber and the substrate if possible, suspension of detached particles and emulsification of the solvent(s) added to aid in the removal process. These functions are preferably performed by surfactants. An essential surfactant class for these purposes is nonionic in nature, that is, does not have any electrical charges, positive or negative. This type of surfactant has an alkyl (aliphatic) chain from about 6 to about 20 carbons, preferably from about 9 to about 18 carbons, and most preferably from about 12 to about 18 carbons. In a preferred embodiment, the alkyl chain portion of the nonionic surfactant consists of a mixture of alkyl chain lengths. In another preferred embodiment, the carbon chains are linear, with no branches in the chain, as these decrease biodegradability. In another preferred embodiment, the ethylene oxide (or in general alkylene oxide) portion of the nonionic surfactant comprises a range of ratios of alkylene oxide (“AO”) to active hydrogen compound (“AHC”).
[0042] Typically, the alkyl chain is supplied in the form of an alcohol, although other active hydrogen compounds (“AHC″s) are known, such as sulfhydryl, amino- or carboxylic acid groups. The AHC is then reacted with ethylene and/or propylene oxide, preferably ethylene oxide. The method of reacting alkylene oxides with poly AHCs is well-known to those skilled in the art. The method of making the ethoxylated derivatives of necessity produces a range of degrees of ethoxylation, ranging from zero (free AHC) to the tens of ethylene oxide units per AHC starting unit. This can be advantageous, but a narrower product distribution is better for some applications. These surfactants are characterized, by among other things, the balance between the hydrophilic (water-loving) and hydrophobic (water-fearing) portions of the molecule, known as the HLB. For the instant invention, nonionic surfactants having a HLB of between about 9 to about 14 is preferred, except for the diethanolamide portion, if present (see below).
[0043] The resultant reaction product is called an alcohol ethoxylate when starting with an alcohol and reacting it with ethylene oxide, and when the carbon chain is linear, a linear alcohol ethoxylate (LAE). The preferred embodiment of the nonionic portion of the cleaner is a LAE. In a most-preferred embodiment, the LAE has an average numbers of ethylene oxide per carbon chain from about 6 to about 10. Such products are exemplified by TOMADOL® surfactants by Air Products.
[0044] The LAE must be present in an efficacious amount, typically from about 0.1 to about 10 percent by weight, preferably from about 1 to about 3 percent by weight.
[0045] Another class of nonionic surfactants that find utility in the instant invention, in combination with other co-surfactants are diethanolamide surfactants. These are made from either a triglyceride or a fatty acid or a fatty acid methyl ester and an excess of diethanolamine. Examples of diethanolamides that find utility in the present invention include but are not limited to coconut, tall oil fatty acid, soybean oil fatty acid, and oleic diethanolamides. Typically, there is an excess of diethanolamine compared to the minimum required to make the diethanolamide, the extra having the purpose to drive the reaction to completion, leading to about a 6-30% concentration of diethanolamine in the final diethanolamide. If present, the diethanolamide is preferably in the range of 0.1-5% by weight, most preferably in the range of 1-3%.
[0046] Nonionic surfactants by themselves have limitations in cleaning compositions that often necessitate the addition of co-surfactants. For example, in the presence of salts frequently used to enhance the formulations' cleaning power, the nonionic surfactant may become insoluble above a certain temperature, called the cloud point. As the salt concentration goes up, typically the cloud point of the nonionic surfactant goes down. At the concentration of salts in many alkaline cleaning compositions, the cloud point may be below the maximum storage temperature or even below room temperature, leading to phase instability, resulting in a non-homogeneous product. This is unacceptable to customers.
[0047] One typical method of preventing this situation is to add co-surfactants that may not be as strong at cleaning as the nonionic surfactant, but whose presence raises the cloud point of the mixture to above that of the maximum storage temperature. Thus, product homogeneity is assured. A common class of surfactants utilized for this purpose is the phosphate esters of nonionic surfactants. These surfactants are made using methods known to those skilled in the art, and typically have a molar ratio of nonionic to phosphorous of about 1 to about 2, although polyphosphate esters are also frequently used. These coupling agents are made as free acids, and often sold that way, although sometimes the sodium or potassium salts are made prior to offering them for sale.
[0048] A preferred embodiment of this class of coupling agent is the ester of a LAE and phosphoric or polyphosphoric acids. A most-preferred embodiment is the ester of a LAE and phosphoric acid, with a mixture of phosphate esters with the number of LAE's to phosphoric acid being from about 1 to about 2. Another most-preferred embodiment is a phosphate ester utilizing a LAE having about 12 to about 18 carbons in the non-polar portion of the LAE and an average degree of ethoxylation from about 6 to about 10. The exact quantity of phosphate ester required is dependent on formulation parameters, but typically ranges from about 0.1 to about 10% by weight.
[0049] Other coupling agents that find utility in the instant invention are acids and/or salts of alkyl-aryl sulfonic acids, exemplified by sodium xylene sulfonate, sodium cumene sulfonate, sodium alkylnaphthalene sulfonate and related compounds. These are classic coupling agents. The exact quantity of sulfonate required is dependent on formulation parameters, but typically ranges from about 0.1 to about 10% by weight.
[0050] Other coupling agents are known to those skilled in the art. It is not uncommon to mix coupling agents in the same formulation. The coupling agents must be added in an amount sufficient to adjust the cloudpoint of the mixture to above the maximum storage temperature. The exact amount will depend on the formulation details, but typical amounts of coupling agents range from about 0.1 to about 10 percent by weight of the whole formulation (on a coupling agent active ingredient basis), if a coupling agent is required. Most preferably, the coupling agents will be from about 1 to about 5 percent by weight of the whole.
[0051] To adequately clean rubber, it is common to add a solvent or solvents to the cleaning composition. Solvents that find utility in the instant invention include, but are not limited to, glycol ethers, terpene hydrocarbons, alkyl esters, alkyl lactates, dialkoxymethanes and other alcohols such as benzyl alcohol.
[0052] Glycol ethers are compounds that include ethylene glycol, propylene glycol, diethylene glycol dipropylene glycol, triethylene glycol or tripropylene glycol, etherified at one end with an alkyl group, typically methyl, ethyl, propyl or butyl, although other alkyl groups also find utility in the instant invention. Glycol ethers of the “E” series, i.e. ethers of ethylene glycol or higher homologues, are increasingly being frowned upon due to toxicity and environmental concerns, and so are not preferred. Propylene-glycol based glycol ethers are therefore a preferred embodiment. Most-preferred are the methyl, ethyl, propyl or butyl ethers of propylene or dipropylene glycol. Glycol ethers are typically added and find utility in the instant invention at a concentration from about 0.1 to about 10% by weight of the whole formulation.
[0053] Although the glycol ethers can be powerful penetrating solvents, other solvents are useful as well, either by themselves or in combination with other solvents, such as the glycol ethers. An example of a solvent class which also find utility in the instant invention is the terpene hydrocarbons. Examples of terpene hydrocarbons that find utility in the instant invention include d-limonene and dipentene, from orange and pine tree processing, respectively. Dipentenes are complex mixtures which vary from location to location and also with the time of year. Terpenes are a preferred embodiment. Terpenes are typically added and find utility in the instant invention at a concentration from about 0.1 to about 10% by weight of the whole formulation.
[0054] Also, although not preferred embodiments, alkyl esters and terpene alcohols potentially find utility in the instant invention. Alkyl esters, such as the methyl ester prepared by transesterification of a vegetable oil such as soybean oil, or an animal-derived fat or oil such as chicken fat, or alternatively alkyl lactates, have useful solvent properties, but are unstable in alkaline solution, and so would limit the amount and kind of builders present. They are therefore not a preferred embodiment. If present, they too are typically added and find utility in the instant invention at a concentration from about 0.1 to about 10% by weight of the whole formulation.
[0055] Terpene alcohols, such as pine oil, have strong, often objectionable odors, and their solvency for non-polar substrates such as runway rubber is limited. Therefore they also are not a preferred embodiment. However, if present, they too are typically added and find utility in the instant invention at a concentration from about 0.1 to about 10% by weight of the whole formulation.
[0056] The solvent component or mixture of components of the instant invention should be present from about 0.1 to about 10 percent by weight. In a preferred embodiment, the solvent is present from about 1 to about 4 percent by weight. One skilled in the art can easily see that careful experimentation can lead to an optimum formulation. Other solvents may also find utility in the instant invention. The nature and optimal concentrations of these are known to those in the art. The discussion above is for purposes of example, not intended to be limiting.
[0057] As a general rule, builders are necessary for a good runway cleaner. Commonly used builders include lithium, sodium or potassium hydroxides, carbonates, bicarbonates, silicates, borates, phosphates, phosphonates or oligo- or polyphosphates. The lithium, sodium or potassium salts are preferred, although in certain situations lithium and perhaps even cesium salts find utility. In actual practice combinations of these builder classes are not uncommon. The builder or builder combination must be present in the range from about 0.1 to about 10 percent by weight of the formulation. In a preferred embodiment, the builder or builders are present from about 3 to about 8 percent by weight on an active ingredient basis.
[0058] Many builders react with calcium or magnesium to cause precipitates to form, removing them from the cleaning zone. Therefore, it is common to include chelating agents to ameliorate this “hardness” in the wash water. Many such chelating agents are known to those skilled in the art. Examples include but are not limited to ethylenediamine tetra acetic acid, ethylenediamene triacetic acid, nitrilo-tris-acetic acid, glucuronic acid, gluconic acid, erythorbic acid, and citric acid or the sodium, potassium, lithium or cesium salts or mixtures and combinations of these. The hardness ameliorating agent should be present from about 0.1 to about 10 percent by weight of the whole, preferably from about 0.1 to about 1 percent of the whole.
[0059] Optional additional surfactants may be added for optimization of the formulation. Examples of such additional surfactants come from the classes of cationic, anionic, amphoteric or amine oxide surfactants.
[0060] Examples of other nonioic surfactants that find utility in the instant invention include but are not limited to block copolymers of ethylene and propylene oxide, alkyl glucosides and alkyl glycosides.
[0061] Examples of anionic surfactants that find utility in the instant invention include, but are not limited to the acid or sodium or potassium salts of alkylbenzene sulfonic acid, tall oil fatty acid, carboxylated nonionics, alkyldiphenyloxide disulfonic acids, and/or mixtures and combinations of these. It is to be understood that the instant invention is an alkaline cleaner, so alkalinity must be added to compensate for any acids included in the formulation.
[0062] Examples of cationic surfactants which find utility in the instant invention are somewhat limited in their structure and/or useful concentration by the negative interaction of cationic surfactants and anionic surfactants or coupling agents. Examples of cationic surfactants which find utility in the instant invention include but are not limited to the cationic surfactants of U.S. Pat. No. 4,239,631 to Brown, included herein by reference and alkyldimethylhydroxyl ammonium chlorides.
[0063] Examples of zwitterionic surfactants which find utility in the instant invention include but are not limited to betaines, glycinates, amphopropionates and amphodipropionates, and mixtures and combinations of these.
[0064] The optional surfactant or surfactant combination should be added from about 0.1 to about 10 percent active by weight of the whole.
EXAMPLE
[0065] The following formulation was made using either (A), a nonylphenol ethoxylate with approximately 10 ethylene oxide units per nonylphenol unit, and a phosphate ester made from the same nonylphenol ethoxylate with an acid number of approximately 100 or (B) a Tomadol 91-6.5 linear alcohol ethoxylate with approximately a C-9-C-10 carbon chain linear alcohol ethoxylate and approximately 6.5 moles of ethylene oxide per alcohol unit, as well as T-MULZ 800, a phosphate ester of an aliphatic alcohol ethoxylate, made by Harcross Chemical.
[0000]
Material
A
B
Na4-EDTA, 40%
0.1%
0.1%
solution
Potassium
13.0%
13.0%
Hydroxide 45%
sodium silicate
4.5%
4.5%
2.0 ratio
trisodium
2.2%
2.2%
phosphate
crystal
alcohol ethoxylate
NP-10
2.0%
Tomadol 91-6.5
2.0%
phosphate ester
NP-10PE
5.0%
T-MULZ 800
5.0%
coconut oil
1.6%
1.5%
diethanolamide,
(26% DEA)
dipropylene
2.0%
2.0%
glycol methyl
ether
d-limonene
2.0%
2.0%
water
QS 100%
QS 100%
[0066] These two formulations were tested on a concrete runway that had extensive buildup of rubber. A spot was marked out for each, both spots being identical in length. The cleaner was spread out on the spot, approximately 2.0 ml each spot, producing a wetted area. After 1.5 hours, the spots were scrubbed using a clipped vehicle wash brush with rollers on it to allow equal pressure on both spots, using a 10 back-and-forth cycles on each spot. The spots were then sprayed thoroughly with water from a trigger sprayer bottle, and patted dry with paper towels. An otherwise identical spot was cleaned using only water as a comparison
[0067] The procedure was repeated for an additional 1.5 hrs, and digital pictures taken after the scrubbing/rinsing cycles. The digital image of the cleaned surface was converted to 16-bit black and white picture using Microsoft Paint. The image was then analyzed using the “Image J” freeware, available from the National Institutes of Health website. An identical uncleaned spot was similarly analyzed. The comparison analysis consisted of dividing the integrated “brightness” score of each spot by the brightness score of the uncleaned spot of equal area. Identical areas were utilized for each spot. In this manner, a reasonably objective measure of the effectiveness of each cleaner was obtained. The results are below.
[0000]
Sample
Count
Black
White
% White
Rank
NPE Version (A)
35415
23882
11533
33%
2
LAE Version (B)
35415
20657
14758
42%
1
Water
35415
34705
710
2%
3
[0068] As can be seen, the Environmentally-preferred formulation actually outperformed the traditional formulation containing NPE.
|
This invention relates to a method of cleaning rubber off of rubber-soiled runways that is free from the usual alkylphenol alkoxylates, which are becoming increasingly scrutinized and discouraged due to environmental considerations. Instead, it is surprisingly found that linear alcohol alkoxylates provide cleaning compositions that are actually more effective, while simultaneously providing an enhanced environmental profile to the formulation.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a ferritic heat-resisting steel, more particularly to a high-nitrogen ferritic heat-resisting steel containing chromium, and being appropriate for use in a high-temperature, high-pressure environment, and to a method of producing the same.
2. Description of the Prior Art
Recent years have seen a marked increase in the temperatures and pressures under which thermal power plant boilers are required to operate. Some plans already call for operation at 566° C. and 314 bar and it is expected that operation under conditions of 650° C. and 355 bar will be implemented in the future. These are extremely severe conditions from the viewpoint of the boiler materials used.
At operating temperatures exceeding 550° C., it has, from the viewpoints of oxidation resistance and high-temperature strength, been necessary to switch from ferritic 2·1/4 Cr-1 Mo steel to high-grade austenitic steels such as 18-8 stainless steel. In other words, it has been necessary to adopt expensive materials with properties exceeding what is required.
Decades have been spent in search of steels for filling in the gap between 2·1/4 Cr-1 Mo steel and austenitic stainless steel. Medium Cr (e.g. 9 Cr and 12 Cr) steel boiler pipes are made of heat-resisting steels that were developed against this backdrop. They achieve high-temperature strength and creep rupture strength on a par with austenitic steels by use of a base metal composition which includes various alloying elements for precipitation hardening and solution hardening.
The creep rupture strength of a heat-resisting steel is governed by solution hardening in the case of short-term aging and by precipitation hardening in the case of prolonged aging. This is because the solution-hardening elements initially present in solid solution in the steel for the most part precipitate as stable carbides such as M 23 C 6 during aging, and then when the aging is prolonged these precipitates coagulate and enlarge, with a resulting decrease in creep rupture strength.
Thus, with the aim of maintaining the creep rupture strength of heat-resisting steels at a high level, a considerable amount of research has been done for discovering ways for avoiding the precipitation of the solution hardening elements and maintaining them in solid solution for as long as possible.
For example, Japanese Patent Public Disclosures No. Sho 63-89644, Sho 61-231139 and Sho 62-297435 teach ferritic steels that achieve dramatically higher creep rupture strength than conventional Mo-containing ferritic heat-resisting steels by the use of W as a solution hardening element.
While the solution hardening by W in these steels may be more effective than by Mo, the precipitates are still fundamentally carbides of the M 23 C 6 type, so that it is not possible to avoid reduction of the creep rupture strength with prolonged aging.
Moreover, the use of ferritic heat-resisting steels at up to 650° C. has been considered difficult because of their inferior high-temperature oxidation resistance as compared with austenitic heat-resisting steels. A particular problem with these steels is the pronounced degradation of high-temperature oxidation resistance that results from the precipitation of Cr in the form of coarse M 23 C 6 type precipitates at the grain boundaries.
The highest temperature limit for use of ferritic heat-resisting steel has therefore been considered to be 600° C.
The need for heat-resisting steels capable of standing up under extremely severe conditions has grown more acute not only because of the increasingly severe operating conditions mentioned earlier but also because of plans to reduce operating costs by extending the period of continuous power plant operation from the current 100 thousand hours up to around 150 thousand hours.
Although ferritic heat-resisting steels are somewhat inferior to austenitic steels in high-temperature strength and anticorrosion property, they have a cost advantage. Furthermore, for reasons related to the difference in thermal expansion coefficient, among the various steam oxidation resistance properties they are particularly superior in scale defoliation resistance. For these reasons, they are attracting attention as a boiler material.
For the reasons set out above, however, it is clearly not possible with the currently available technology to develop ferritic heat-resisting steels that are capable of standing up for 150 thousand hours under operating conditions of 650° C. and 355 bar, that are low in price and that exhibit good steam oxidation resistance.
Based on the foregoing knowledge and as described in Japanese Patent Application No. Hei 2-37895, the inventors earlier disclosed that a high-nitrogen ferritic heat-resisting steel estimated by linear extrapolation to exhibit a creep rupture strength of not less than 147 MPa under operating conditions of 650° C. and 355 bar for 150 thousand hours can be obtained by using a pressurized atmosphere to add nitrogen exceeding the solution limit and thus inducing precipitation of the excess nitrogen in the form of fine nitrides and carbo-nitrides. The gist of their disclosure was a ferritic heat-resisting steel characterized in comprising, in weight per cent, 0.01-0.30% C, 0.02-0.80% Si, 0.20-1.00% Mn, 8.00-13.00% Cr, 0.50-3.00% W, 0.005-1.00% Mo, 0.05-0.50% V, 0.02-0.12% Nb and 0.10-0.50%N and being controlled to include not more than 0.050% P, not more than 0.010% S and not more than 0.020% O, and optionally comprising (A) one or both of 0.01-1.00% Ta and 0.01-1.00% Hf and/or (B) one or both of 0.0005-0.10% Zr and 0.01-0.10% Ti, the balance being Fe and unavoidable impurities, and a method of producing the steel wherein the steel components are melted and equilibrated in an atmosphere of a mixed gas of a prescribed nitrogen partial pressure or nitrogen gas, and the resulting melt is thereafter cast or solidified in an atmosphere controlled to have a nitrogen partial pressure of not less than 1.0 bar and a total pressure of not less than 4.0 bar, with the relationship between the partial pressure p and the total pressure P being
10.sup.p <P.sup.0.37 +log.sub.10.sup.6
thereby obtaining good quality ingot free of blowholes.
Based on the results of tests for determining the creep rupture strength of the steel taught by Japanese Patent Application No. Hei 2-37895 up to 50 thousand hours, the inventors discovered that the creep rupture strength of the steel at 150 thousand hours, as estimated by linear extrapolation, is no more than 176 MPa and, in particular, that the steel experiences a marked decrease in creep rupture strength between 30 and 50 thousand hours. Further studies showed that the reason for the decrease in creep rupture strength was that during the creep test large Fe 2 W grains measuring 1 μm or more in diameter precipitated in large amounts, principally at the grain boundaries, leading to large-scale loss of W as a solid solution element from the steel.
Moreover, they further discovered that by limiting the W content to not more than 1.5% so as to prevent precipitation of W as Fe 2 W and by adding Nb in excess of 0.12% so that NbN and (Nb, V)N, the most stable of all nitrides, become the principal precipitation hardening factors, it is possible to obtain a ferritic heat-resisting steel exhibiting a creep rupture strength at 650° C., 355 bar and 150 thousand hours of not less than 200 MPa, as estimated by linear extrapolation.
In addition they discovered that owing to the increase in the N solution limit resulting from the addition of a large amount of Nb the pressurized atmosphere conditions required for casting of sound ingot become a total pressure of not less than 2.5 bar and a nitrogen partial pressure of not less than 1.0 bar, with the relationship between the total pressure P and the nitrogen partial pressure p being
P>2.5p.
There have been few papers published on research into high-nitrogen ferritic heat-resisting steels and the only known published report in this field in Ergebnisse der Werkstoff-Forschung, Band I, Varlag Schweizerische Akademie der Werkstoffwissenschaften "Thubal-Kain", Zurich, 1987, 161-180.
However, the research described in this report is limited to that in connection with ordinary heat-resisting steel and there is no mention of materials which can be used under such severe conditions at 650° C., 355 bar and 150 thousand hours continuous operation.
SUMMARY OF THE INVENTION
An object of this invention is to provide a high-nitrogen ferritic heat-resisting steel which overcomes the shortcomings of the conventional heat-resisting steels, and particularly to provide such a steel exhibiting outstanding creep rupture strength and capable of being used under severe operating conditions, wherein the decrease in creep rupture strength following prolonged aging and the degradation of high-temperature oxidation resistance caused by precipitation of carbides are mitigated by adding nitrogen to supersaturation so as to precipitate fine nitrides and/or carbo-nitrides which suppress the formation of carbides such as the M 23 C 6 precipitates seen in conventional steels.
This invention was accomplished in the light of the aforesaid knowledge and, in one aspect, pertains substantially to a high-nitrogen ferritic heat-resisting steel with high niobium content comprising, in weight percent 0.01-0.30% C, 0.02-0.80% Si, 0.20-1.00% Mn, 8.00-13.00% Cr, 0.005-1.00% Mo, 0.20-1.50% W, 0.05-1.00% V, over 0.12 up to 2.00% Nb and 0.10-0.50% N and being controlled to include not more than 0.050% P, not more than 0.010% S and not more than 0.020% O, and optionally comprising (A) one or both of 0.01-1.00% Ta and 0.01-1.00% Hf and/or (B) one or both of 0.0005-0.10% Zr and 0.01-0.10% Ti, the balance being Fe and unavoidable impurities.
Another aspect of the invention pertains to a method of producing such a high-nitrogen ferritic heat-resisting steel with high niobium content wherein the steel components are melted and equilibrated in an atmosphere of a mixed gas of a prescribed nitrogen partial pressure or nitrogen gas, and the resulting melt is thereafter cast or solidified in an atmosphere controlled to have a total pressure of not less than 2.5 bar and a nitrogen partial pressure of not less than 1.0 bar, with the relationship between the nitrogen partial pressure p and the total pressure P being
P>2.5p.
The above and other features of the present invention will become apparent from the following description made with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an ingot and the manner in which it is to be cut.
FIG. 2 is a graph showing the relationship between the steel nitrogen content and the weight percentage of the total of M 23 C 6 +M 6 C+NbC+Cr 2 N+NbN among the precipitates in the steel accounted for by M 23 C 6 +M 6 C+NbC and the relationship between the steel nitrogen content and the weight percentage of the total of M 23 C 6 +M 6 C+NbC+Cr 2 N+NbN among the precipitates in the steel accounted for by Cr 2 N+NbN.
FIG. 3 is a graph showing conditions under which blowholes occur in the ingot in terms of the relationship between the total pressure and nitrogen partial pressure of the atmosphere during casting.
FIG. 4 is a schematic view showing the manner in which creep test pieces are taken from a pipe specimen and a rolled plate specimen.
FIG. 5 is a graph showing the relationship between steel nitrogen content and estimated creep rupture strength at 650° C., 150 thousand hours.
FIG. 6 is a graph showing the relationship between steel Nb content and estimated creep rupture strength at 650° C., 150 thousand hours.
FIG. 7 is a graph showing the relationship between steel W content and estimated creep rupture strength at 650° C., 150 thousand hours.
FIG. 8 is a graph showing an example of creep test results in terms of stress vs rupture time.
FIG. 9 is a graph showing the relationship between steel nitrogen content and Charpy impact absorption energy at 0° C. following aging at 700° C. for 10 thousand hours.
FIG. 10 is a graph showing the relationship between steel nitrogen content and the thickness of the oxidation scale formed on the surface of a test piece after oxidation at 650° C. for 10 thousand hours.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The reasons for the limits placed on the components of the high-nitrogen ferritic heat-resisting steel with high Nb content according to this invention will now be explained.
C is required for achieving strength. Adequate strength cannot be achieved at a C content of less than 0.01%, while at a C content exceeding 0.30% the steel is strongly affected by welding heat and undergoes hardening which becomes a cause for low-temperature cracking. The C content range is therefore set at 0.01-0.30%.
Si is important for achieving oxidation resistance and is also required as a deoxidizing agent. It is insufficient for these purposes at a content of less than 0.02%, whereas a content exceeding 0.80% reduces the creep rupture strength. The Si content range is therefore set at 0.02-0.80%.
Mn is required for deoxidation and also for achieving strength. It has to be added an amount of at least 0.20% for adequately exhibiting its effect. When it exceeds 1.00% it may in some cases reduce creep rupture strength. The Mn content range is therefore set at 0.20-1.00%.
Cr is indispensable to oxidation resistance. It also contributes to increasing creep resistance by combining with N and finely precipitating in the base metal matrix in the form of Cr 2 N, Cr 2 (C, N) and the like. Its lower limit is set at 8.00% from the viewpoint of oxidation resistance. Its upper limit is set at 13.00% for maintaining the Cr equivalent value at a low level so as to realize a martensite phase texture.
W produces a marked increase in creep rupture strength by solution hardening. Its effect toward increasing creep rupture strength over long periods at high temperatures of 550° C. and higher is particularly pronounced. Its upper limit is set at 1.50% because at contents higher than this level it precipitates in large quantities in the form of carbide and intermetallic compounds which sharply reduce the toughness of the base metal. The lower limit is set at 0.20% because it does not exhibit adequate solution hardening effect at lower levels.
Mo increases high-temperature strength through solution hardening. It does not exhibit adequate effect at a content of less than 0.005% and at a content higher than 1.00% it may, when added together with W, cause heavy precipitation of Mo 2 C type oxides which markedly reduce base metal toughness. The Mo content range is therefore set at 0.005-1.00%.
V produces a marked increase in the high-temperature strength of the steel regardless of whether it forms precipitates or, like W, enters solid solution in the matrix. When it precipitates, the resulting VN and (Nb, V)N serve as precipitation nuclei for Cr 2 N and Cr 2 (C, N), which has a pronounced effect toward promoting fine dispersion of the precipitates. It has no effect at below 0.05% and reduces toughness at higher than 1.00%. The V content range is therefore set at 0.05-1.00%.
Nb is an element which increases high-temperature strength by precipitating as NbN, (Nb, V)N, Nb(C, N) and (Nb, V) (C, N). Also, similarly to V, it promotes fine precipitate dispersion by forming precipitation nuclei for Cr 2 N, Cr 2 (C, N) and the like. For it to disperse in the steel as the primary precipitation hardening factor it has to be added in excess of 0.12%. However, its upper limit is set at 2.00% because when present at higher levels it reduces strength by causing precipitate coagulation and enlargement.
N dissolves in the matrix and also forms nitride and carbo-nitride precipitates. As the form of the precipitates is mainly Cr 2 N and Cr 2 (C, N), there is less precipitate-induced consumption of Cr and W than in the case of the M 23 C 6 , M 6 C and other such precipitates observed in conventional steels. N thus increases oxidation resistance and creep rupture strength. At least 0.10% is required for precipitation of nitrides and carbo-nitrides and suppressing precipitation of M 23 C 6 and M 6 C. The upper limit is set at 0.50% for preventing coagulation and enlargement of nitride and carbo-nitride precipitates by the presence of excessive nitrogen.
P, S and O are present in the steel according to this invention as impurities. P and S hinder the achievement of the purpose of the invention by lowering strength, while O has the adverse effect of forming oxides which reduce toughness. The upper limits on these elements is therefore set at 0.050%, 0.010% and 0.020%, respectively.
The basic components of the steel according to this invention (aside from Fe) are as set out above. Depending on the purpose to which the steel is to be put, however, it may additionally contain (A) one or both of 0.01-1.00% Ta and 0.01-1.00% Hf and/or (B) one or both of 0.0005-0.10% Zr and 0.01-0.10% Ti.
At low concentrations Ta and Hf act as deoxidizing agents. At high concentrations they form fine high melting point nitrides and carbo-nitrides and, as such, increase toughness by decreasing the austenite grain size. In addition, they also reduce the degree to which Cr and W dissolve in precipitates and by this effect enhance the effect of supersaturation with nitrogen. Neither element exhibits any effect at less than 0.01%. When either is present at greater than 1.00%, it reduces toughness by causing enlargement of nitride and carbo-nitride precipitates. The content range of each of these elements is therefore set at 0.01-1.00%.
Acting to govern the deoxidation equilibrium in the steel, Zr suppresses the formation of oxides by markedly reducing the amount of oxygen activity. In addition, its strong affinity for N promotes precipitation of fine nitrides and carbo-nitrides which increase creep rupture strength and high-temperature oxidation resistance. When present at less than 0.0005% it does not provide an adequate effect of governing the deoxidation equilibrium and when present at greater than 0.10% it results in heavy precipitation of coarse ZrN and ZrC which markedly reduce the toughness of the base metal. The Zr content range is therefore set at 0.0005-0.10%.
Ti raises the effect of excess nitrogen by precipitating in the form of nitrides and carbo-nitrides. At a content of less than 0.01% it has no effect while a Ti content of over 0.10% results in precipitation of coarse nitrides and carbo-nitrides which reduce toughness. The Ti content range is therefore set at 0.01-0.10%.
The aforesaid alloying components can be added individually or in combinations.
The object of this invention is to provide a ferritic heat-resisting steel that is superior in creep rupture strength and high-temperature oxidation resistance. Depending on the purpose of use it can be produced by various methods and be subjected to various types of heat treatment. These methods and treatments in no way diminish the effect of the invention.
However, in view of the need to supersaturate the steel with nitrogen, it is necessary during casting to raise the total pressure of the atmosphere to not less than 2.5 bar and to control the relationship between the total pressure P and the nitrogen partial pressure p to satisfy the inequation P>2.5 p. As an auxiliary gas to be mixed with the nitrogen gas it is appropriate to use an inert gas such as Ar, Ne, Xe or Kr. These casting conditions were determined by the following experiment.
Steel of a chemical composition, aside from nitrogen, as indicated in the present invention was melted in an induction heating furnace installed in a chamber that could be pressurized up to 150 bar. A mixed gas of argon and nitrogen having a nitrogen partial pressure adequate for achieving the target nitrogen content was introduced into the furnace and maintained at a pressure which was varied from test to test. After the nitrogen and molten metal had reached chemical equilibrium, the molten metal was cast into a mold that had been installed in the chamber beforehand, whereby there was obtained a 5-ton ingot.
The ingot was cut vertically as shown in FIG. 1 and the ingot 1 was visually examined for the presence of blowholes.
Following this examination, a part of the ingot was placed in a furnace and maintained at 1180° C. for 1 hour and then forged into a plate measuring 50 mm in thickness, 750 mm in width and 4,000 mm in length.
This plate was subjected to solution treatment at 1200° C. for 1 hour and to tempering at 800° C. for 3 hours. The steel was then chemically analyzed and the dispersion state and morphology of the nitrides and carbo-nitrides were investigated by observation with an optical microscope, an electron microscope, X-ray diffraction and electron beam diffraction, whereby the chemical structure was determined.
Among the precipitates present within the as-heat-treated steel, FIG. 2 shows how the proportion of the precipitates in the steel accounted for by M 23 C 6 type carbides and M 6 C or NbC type carbides and the proportion thereof accounted for by Cr 2 N type nitrides and NbN type nitrides vary with nitrogen concentration. At a nitrogen concentration of 0.10%, nitrides account for the majority of the precipitates in the steel of the invention, while at a nitrogen concentration of 0.15%, substantially 100% of the precipitates are nitrides with virtually no carbides present whatsoever. Thus for the effect of this invention to be adequately manifested it is necessary for the nitrogen concentration of the steel to be not less than 0.1%.
The graph of FIG. 3 shows how the state of blowhole occurrence varies depending on the relationship between the total and nitrogen partial pressures of the atmosphere. For achieving a nitrogen concentration of 0.10% or higher it is necessary to use a total pressure of not less than 2.5 bar. Equilibrium calculation based on Sievert's law shows that in this case the nitrogen partial pressure in the steel of this invention is not less than 1.0 bar.
Moreover, where for controlling the amount of nitride and carbo-nitride precipitation the nitrogen partial pressure is maintained at 1.0-6.0 bar (nitrogen concentration within the steel of approximately 0.5 mass %), it becomes necessary to vary the total pressure between 2.5 and about 15 bar, the actual value selected depending on the nitrogen partial pressure. Namely, it is necessary to use a total pressure falling above the broken line representing the boundary pressure in FIG. 3.
When the boundary line of FIG. 3 is determined experimentally it is found to lie at
P=2.5p
meaning that the steel according to this invention can be obtained by selecting an atmosphere of a pressure and composition meeting the condition of the inequality
P>2.5p
It is therefore necessary to use furnace equipment enabling pressure and atmosphere control. Without such equipment, it is difficult to produce the steel of the present invention.
There are no limitations whatever on the melting method. Based on the chemical composition of the steel and cost considerations, it suffices to select from among processes using a converter, an induction heating furnace, an arc melting furnace or an electric furnace.
The situation regarding refining is similar. Insofar as the atmosphere is controlled to a total pressure of not less than 2.5 bar and a nitrogen partial pressure of not less than 1.0 bar, it is both possible and effective to use a ladle furnace, an electro-slag remelting furnace or a zone melting furnace.
After casting under a pressurized atmosphere of a total pressure of not less than 2.5 bar and a nitrogen partial pressure of not less than 1.0 bar, it is possible to process the steel into billet, bloom or plate by forging or hot rolling. Since the steel of this invention includes finely dispersed nitrides and carbo-nitrides, it is superior to conventional ferritic heat-resisting steels in hot-workability. This is also one reason for employing nitrides and carbo-nitrides obtained by adding nitrogen to beyond the solution limit.
For processing the steel into products, it is possible to first process it into round or rectangular billet and then form it into seamless pipe or tube by hot extrusion or any of various seamless rolling methods. Otherwise it can be formed into sheet by hot and cold rolling and then made into welded tube by electric resistance welding. Alternatively, it can be processed into welded pipe or tube by use of TIG, MIG, SAW, LASER and EB welding, individually or in combination. Moreover, it is possible to expand the size range of products to which the present invention can be applied by following any of the aforesaid processes by hot or warm stretch reduction or sizing.
The steel according to the invention can also be provided in the form of plate or sheet. The plate or sheet can, in its hot-rolled state or after whatever heat treatment is found necessary, be provided as a heat-resisting material in various shapes, without any influence on the effects provided by the invention.
The pipe, tube, plate, sheet and variously shaped heat-resisting materials referred to above can, in accordance with their purpose and application, be subjected to various heat treatments, and it is important for them to be so treated for realizing the full effect of the invention.
While the production process ordinarily involves normalizing (solution heat treatment)+ tempering, it is also possible and useful additionally to carry out one or a combination of two or more of quenching, tempering and normalizing. It is also possible, without influencing the effects of the present invention in any way, to repeatedly carry out one or more of the aforesaid processes to whatever degree is necessary for adequately bringing out the steel properties.
The aforesaid processes can be appropriately selected and applied to the manufacture of the steel according to the invention.
WORKING EXAMPLES
The steels indicated in Tables 1-14, each having a composition according to the present invention, were separately melted in amounts of 5 tons each in an induction heating furnace provided with pressurizing equipment. The resulting melt was cleaned by ladle furnace processing (under bubbling with a gas of the same composition as the atmosphere) for reducing its impurity content, whereafter the atmosphere was regulated using a mixed gas of nitrogen and argon so as to satisfy the conditions of the inequality P>2.5 p. The melt was then cast into a mold and processed into a round billet, part of which was hot extruded to obtain a tube 60 mm in outside diameter and 10 mm in wall thickness and the remainder of which was subjected to seamless rolling to obtain a pipe 380 mm in outside diameter and 50 mm in wall thickness. The tube and pipe were subjected to a single normalization at 1200° C. for 1 hour and were then tempered at 800° C. for 3 hours.
In addition, a 5 ton ingot was cast and forged into a slab which was hot rolled into 25 mm and 50 mm thick plates.
As shown in FIG. 4, creep test pieces 6 measuring 6 mm in diameter were taken along the axial direction 4 of the pipe or tube 3 and along the rolling direction 5 of the plates and subjected to creep test measurement at 650° C. Based on the data obtained, a linear extrapolation was made for estimating the creep rupture strength at 150 thousand hours. A creep rupture strength of 150 MPa was used as the creep rupture strength evaluation reference value. The creep rupture strength at 650° C., 150 thousand hours is hereinafter defined as the linearly extrapolated value at 150 thousand hours on the creep rupture strength vs rupture time graph.
Toughness was evaluated through an accelerated evaluation test in which aging was carried out at 700° C. for 10 thousand hours. JIS No. 4 tension test pieces were cut from the aged steel and evaluated for impact absorption energy. Assuming a water pressure test at 0° C., the toughness evaluation reference value was set at 10 J.
High-temperature oxidation resistance was evaluated by suspending a 25 mm×25 mm×5 mm test piece cut from the steel in 650° C. atmospheric air in a furnace for 10 thousand hours and then cutting the test piece parallel to the direction of growth of the scale and measuring the oxidation scale thickness.
The 650° C., 150 thousand hour creep rupture strength, the Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours and the oxidation scale thickness after oxidation at 650° C. for 10 thousand hours are shown in Tables 2, 4, 6, 8, 10, 12, and 14.
For comparison, steels of compositions not falling within the present invention were melted, processed and tested in the same way as described above. Their chemical compositions and the evaluation results are shown in Tables 15 and 16.
FIG. 5 shows the relationship between the nitrogen content of the steels and the estimated creep rupture strength at 650° C., 150 thousand hours. It will be noted that the creep rupture strength attains high values exceeding 150 MPa at a steel nitrogen content of 0.1% or higher but falls below 150 MPa and fails to satisfy the evaluation reference value that was set at a steel nitrogen content of less than 0.1%.
FIG. 6 shows the relationship between the Nb content of the steels and the estimated creep rupture strength at 650° C., 150 thousand hours. It will be noted that the creep rupture strength attains values exceeding 150 MPa at a steel Nb content exceeding 0.12% but at a Nb content of 2.0% or higher the creep rupture strength is instead lowered owing to the precipitation of coarse NbN and Fe 2 Nb type Laves phase at the melting stage.
FIG. 7 shows the relationship between the W content of the steels and the estimated creep rupture strength at 650° C., 150 thousand hours. The creep rupture strength is below 150 MPa at a W content of less than 0.2% and is 150 MPa or higher in a content range of 0.2-1.5%. When the W is present in excess of 1.5%, the creep rupture strength falls below 150 MPa owing to coarse Fe 2 W precipitating at the grain boundaries.
FIG. 8 shows the results of the creep test in terms of stress vs rupture time. A good linear relationship can be noted between stress and rupture time at a steel nitrogen content of not less than 0.1%. Moreover, the creep rupture strength is high. On the other hand, when the steel nitrogen content falls below 0.1%, the relationship between stress and rupture time exhibits a pronounced decline in creep rupture strength with increasing time lapse. Either the linearity is not maintained, or the slope of the creep rupture curve is steep, with the short-term side creep rupture strength being high but the long-term creep rupture strength being low, or the creep rupture strength is low throughout. This is because W and the other solution hardening elements precipitate as carbides whose coagulation and enlargement degrades the creep rupture strength property of the base metal. In contrast, at a nitrogen content of 0.1% or higher, fine nitrides are preferentially precipitated so that the formation of carbides is greatly delayed. Therefore, since the dissolution of the solution hardening elements into carbides was suppressed and also because the finely precipitated nitrides remained present in a stable state without coagulating and enlarging during the long-term high-temperature creep test, a high creep rupture strength was maintained in the long-term creep test.
FIG. 9 shows the relationship between Charpy impact absorption energy at 0° C. following aging at 700° C. for 10 thousand hours and steel nitrogen content. When the steel nitrogen content falls within the range of 0.1-0.5%, the impact absorption energy exceeds 10 J. In contrast, when it falls below 0.1%, there is little or no suppression of grain growth by residual high melting point nitrides during solution treatment and, as a result, the impact absorption energy decreases, and when it exceeds 0.5%, the impact absorption energy is reduced by heavy nitride precipitation.
FIG. 10 shows the relationship between the thickness of the oxidation scale formed on the surface of a test piece after oxidation at 650° C. for 10 thousand hours and the steel nitrogen content. Although the oxidation scale thickness is between 400 and 900 μm when the steel nitrogen content falls below 0.1%, it decreases to 50 μm or less when the steel nitrogen content is 0.1% or higher.
Reference is now made to the comparison steels shown in Table 5. Nos. 161 and 162 are examples in which insufficient steel nitrogen content resulted in a low estimated creep rupture strength at 650° C., 150 thousand hours and also to poor high-temperature oxidation resistance. Nos. 163 and 164 are examples in which excessive steel nitrogen content caused heavy precipitation of coarse nitrides and carbo-nitrides, resulting in a Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours of not more than 10 J. No. 165 is an example in which a low W concentration resulted in a low creep rupture strength at 650° C., 150 thousand hours owing to insufficient solution hardening notwithstanding that the steel nitrogen content fell within the range of the invention. No. 166 is an example in which a high W concentration led to low rupture strength and toughness owing to precipitation of coarse Fe 2 W type Laves phase at the grain boundaries during creep. No. 167 is an example in which a low Nb content resulted in a low estimated creep rupture strength at 650° C., 150 thousand hours. No. 168 is an example in which a high Nb content caused profuse precipitation of coarse Fe 2 Nb type Laves phase during creep, which in turn lowered both the estimated creep rupture strength at 650° C., 150 thousand hours and the Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours. No. 169 is an example in which heavy precipitation of coarse ZrN caused by a Zr concentration in excess of 0.1% resulted in a Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours of less than 10 J. Nos. 170, 171 and 172 are examples similar to the case of No. 169 except that the elements present in excess were Ta, Hf and Ti, respectively. As a result, heavy precipitation of coarse TaN, HfN and TiN resulted in a Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours of less than 10 J. No. 173 is an example in which, notwithstanding that the steel composition satisfied the conditions of the present invention, since the nitrogen partial pressure was 2.2 bar and the total pressure was 2.5 bar, values not satisfying the inequality P>2.5 p, many large blowholes formed in the ingot, making it impossible to obtain either a sound ingot or a plate and leading to a reduction in both the estimated creep rupture strength at 650° C., 150 thousand hours and the Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours.
TABLE 1______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________ 1 0.195 0.251 0.801 0.048 0.008 0.666 0.094 9.52 0.586 2 0.070 0.475 0.632 0.013 0.005 0.132 0.370 10.38 0.038 3 0.192 0.709 0.261 0.042 0.009 1.185 0.174 8.70 0.707 4 0.032 0.316 0.231 0.022 0.008 0.418 0.487 12.80 0.767 5 0.219 0.220 0.299 0.018 0.004 1.064 0.496 11.18 0.427 6 0.096 0.190 0.620 0.022 0.003 0.608 0.066 9.82 0.865 7 0.288 0.762 0.546 0.038 0.008 1.308 0.402 9.66 0.283 8 0.270 0.515 0.216 0.014 0.001 0.680 0.462 9.07 0.843 9 0.098 0.369 0.583 0.039 0.003 0.927 0.105 11.51 0.74810 0.259 0.477 0.995 0.039 0.002 0.582 0.089 10.40 0.17911 0.083 0.594 0.404 0.021 0.007 1.824 0.050 11.70 0.82012 0.206 0.478 0.961 0.035 0.004 0.336 0.073 8.84 0.36613 0.100 0.663 0.812 0.026 0.003 1.163 0.469 12.74 0.50414 0.113 0.515 0.514 0.043 0.004 1.837 0.418 11.87 0.41615 0.152 0.577 0.217 0.033 0.007 0.823 0.237 12.21 0.80416 0.127 0.600 0.467 0.024 0.002 0.392 0.454 9.62 0.84317 0.092 0.722 0.203 0.022 0.006 1.747 0.246 12.49 0.70418 0.243 0.320 0.395 0.036 0.007 1.583 0.165 9.38 0.61319 0.060 0.713 0.388 0.013 0.001 0.194 0.285 11.20 0.73220 0.030 0.087 0.722 0.020 0.009 0.790 0.465 8.83 0.75121 0.210 0.544 0.354 0.026 0.004 1.791 0.341 10.73 0.36322 0.213 0.281 0.237 0.036 0.008 1.714 0.451 10.38 0.75623 0.101 0.227 0.520 0.041 0.008 0.897 0.200 8.70 0.11724 0.067 0.128 0.544 0.045 0.001 0.640 0.348 9.08 0.62525 0.172 0.142 0.473 0.038 0.002 0.340 0.307 12.53 0.482______________________________________
TABLE 2______________________________________ CS VE TONo. W Zr Ta Hf Ti N O MPa J μm______________________________________ 1 1.154 -- -- -- -- 0.375 0.002 231 19.4 46 2 0.716 -- -- -- -- 0.242 0.010 214 17.7 46 3 1.169 -- -- -- -- 0.422 0.019 230 55.3 38 4 1.439 -- -- -- -- 0.187 0.013 195 38.7 28 5 0.497 -- -- -- -- 0.210 0.007 183 54.3 47 6 1.187 -- -- -- -- 0.376 0.002 209 77.9 19 7 0.496 -- -- -- -- 0.153 0.012 243 18.8 13 8 0.608 -- -- -- -- 0.217 0.012 153 64.1 36 9 0.473 -- -- -- -- 0.440 0.006 157 16.9 3610 0.329 -- -- -- -- 0.301 0.017 226 31.2 2011 0.420 0.050 -- -- -- 0.270 0.009 226 14.1 1612 0.999 0.092 -- -- -- 0.427 0.006 178 49.6 1113 1.006 0.031 -- -- -- 0.445 0.019 201 45.7 3314 1.328 0.035 -- -- -- 0.197 0.016 161 15.1 5015 0.280 0.073 -- -- -- 0.164 0.010 179 41.0 2716 0.686 0.015 -- -- -- 0.218 0.012 175 32.4 3517 1.464 0.026 -- -- -- 0.228 0.017 213 35.1 3818 0.323 0.028 -- -- -- 0.276 0.002 166 64.9 4619 1.363 0.040 -- -- -- 0.438 0.005 202 28.6 2620 0.280 0.080 -- -- -- 0.183 0.013 240 45.7 2621 0.574 -- 0.291 -- -- 0.190 0.019 246 56.8 3222 1.196 -- 0.414 -- -- 0.134 0.018 242 42.0 1223 1.086 -- 0.275 -- -- 0.293 0.013 195 13.6 3424 0.480 -- 0.038 -- -- 0.132 0.017 226 55.8 2525 0.926 -- 0.039 -- -- 0.139 0.006 200 75.2 13______________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 3______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________26 0.027 0.796 0.445 0.045 0.005 1.306 0.157 12.42 0.85927 0.273 0.684 0.616 0.036 0.006 1.054 0.209 12.23 0.95428 0.093 0.727 0.740 0.018 0.007 1.824 0.100 10.41 0.45929 0.120 0.290 0.555 0.017 0.004 1.164 0.363 10.34 0.05530 0.118 0.298 0.215 0.023 0.006 0.328 0.177 10.47 0.91431 0.144 0.520 0.282 0.041 0.008 0.648 0.087 9.32 0.75632 0.248 0.694 0.487 0.019 0.007 0.572 0.391 10.20 0.24133 0.055 0.208 0.602 0.046 0.001 1.432 0.286 9.19 0.08034 0.198 0.752 0.361 0.048 0.002 1.631 0.296 12.13 0.93935 0.292 0.519 0.709 0.013 0.005 1.583 0.056 9.91 0.01136 0.106 0.449 0.217 0.049 0.003 1.617 0.334 11.12 0.49437 0.127 0.685 0.219 0.023 0.002 0.190 0.304 11.57 0.56338 0.118 0.576 0.459 0.022 0.006 0.492 0.278 9.73 0.40639 0.279 0.286 0.703 0.014 0.001 1.016 0.344 11.55 0.22040 0.237 0.746 0.301 0.027 0.003 1.137 0.138 8.01 0.69141 0.036 0.137 0.987 0.028 0.004 0.275 0.408 12.45 0.99342 0.024 0.558 0.524 0.023 0.001 1.619 0.351 10.85 0.82443 0.111 0.602 0.658 0.043 0.006 1.759 0.272 11.70 0.87844 0.063 0.416 0.740 0.013 0.007 1.035 0.252 10.85 0.33145 0.220 0.528 0.523 0.040 0.009 0.723 0.380 9.33 0.37946 0.203 0.303 0.544 0.013 0.010 0.266 0.060 10.46 0.19547 0.211 0.280 0.956 0.039 0.006 0.957 0.055 12.74 0.47048 0.158 0.227 0.728 0.025 0.005 0.334 0.227 9.64 0.40849 0.241 0.279 0.798 0.020 0.004 1.557 0.210 12.12 0.19550 0.078 0.197 0.915 0.030 0.008 0.262 0.310 8.54 0.524______________________________________
TABLE 4__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________26 1.374 -- 0.611 -- -- 0.377 0.001 238 15.8 4527 0.756 -- 0.221 -- -- 0.329 0.016 160 30.8 4928 1.272 -- 0.295 -- -- 0.468 0.007 232 63.1 1329 1.225 -- 0.134 -- -- 0.266 0.015 225 55.9 2330 0.834 -- 0.227 -- -- 0.199 0.007 156 21.9 2731 1.018 0.017 0.053 -- -- 0.149 0.013 194 79.6 3332 1.356 0.007 0.337 -- -- 0.379 0.019 159 32.3 2933 1.460 0.012 0.494 -- -- 0.378 0.019 221 68.5 2134 0.246 0.003 0.098 -- -- 0.411 0.016 194 59.9 3735 1.227 0.017 0.325 -- -- 0.353 0.005 200 21.0 2636 1.401 0.001 0.118 -- -- 0.284 0.017 158 69.4 1337 0.337 0.084 0.681 -- -- 0.476 0.009 186 77.7 4738 0.899 0.031 0.079 -- -- 0.399 0.002 152 24.2 1539 0.726 0.013 0.549 -- -- 0.135 0.019 176 28.7 2640 0.722 0.046 0.062 -- -- 0.163 0.009 227 32.3 4541 0.450 -- -- 0.844 -- 0.148 0.001 171 48.4 4142 1.484 -- -- 0.732 -- 0.168 0.010 180 55.9 4243 1.463 -- -- 0.509 -- 0.301 0.019 172 67.8 1444 1.266 -- -- 0.36 -- 0.423 0.014 165 26.7 4645 0.495 -- -- 0.954 -- 0.202 0.007 226 50.2 4346 0.695 -- -- 0.516 -- 0.116 0.002 227 47.5 3547 1.456 -- -- 0.215 -- 0.439 0.012 235 66.8 4948 0.429 -- -- 0.239 -- 0.254 0.013 221 16.1 3349 1.116 -- -- 0.775 -- 0.229 0.007 152 48.8 1350 1.143 -- -- 0.511 -- 0.241 0.008 195 71.6 18__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 5______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________51 0.013 0.514 0.430 0.043 0.001 0.562 0.385 9.86 0.02452 0.244 0.202 0.686 0.027 0.008 1.922 0.074 9.51 0.45153 0.251 0.594 0.652 0.029 0.003 0.881 0.135 10.99 0.96954 0.229 0.256 0.857 0.036 0.002 0.636 0.203 10.17 0.27455 0.091 0.135 0.271 0.016 0.001 0.590 0.138 8.04 0.04756 0.032 0.745 0.624 0.017 0.007 1.097 0.471 12.99 0.46657 0.252 0.293 0.474 0.026 0.007 1.554 0.160 8.45 0.22558 0.081 0.484 0.769 0.030 0.009 1.403 0.416 12.86 0.66159 0.011 0.299 0.870 0.018 0.008 0.988 0.430 12.23 0.01760 0.093 0.653 0.510 0.015 0.004 0.628 0.051 9.89 0.91461 0.236 0.532 0.650 0.031 0.006 1.657 0.267 11.83 0.40862 0.207 0.470 0.638 0.032 0.001 0.660 0.493 11.53 0.18763 0.060 0.620 0.630 0.026 0.007 1.736 0.134 9.91 0.92664 0.138 0.327 0.757 0.021 0.005 0.544 0.396 12.80 0.31865 0.061 0.155 0.791 0.024 0.004 1.198 0.245 11.28 0.05766 0.175 0.617 0.869 0.022 0.008 0.296 0.436 11.21 0.31767 0.095 0.311 0.345 0.023 0.005 1.922 0.377 11.03 0.78868 0.169 0.165 0.971 0.015 0.007 0.839 0.384 9.23 0.67369 0.018 0.714 0.898 0.045 0.002 0.192 0.314 9.23 0.15470 0.271 0.143 0.664 0.020 0.004 0.309 0.471 9.42 0.40271 0.119 0.553 0.823 0.029 0.003 0.583 0.261 8.20 0.60572 0.033 0.126 0.712 0.036 0.003 0.506 0.447 8.99 0.94473 0.240 0.227 0.929 0.013 0.003 0.416 0.228 10.50 0.65874 0.054 0.575 0.388 0.045 0.009 1.583 0.129 10.93 0.89875 0.116 0.159 0.450 0.041 0.009 1.533 0.233 8.81 0.361______________________________________
TABLE 6__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________51 0.750 0.065 -- 0.132 -- 0.363 0.010 171 28.4 1352 0.200 0.047 -- 0.829 -- 0.469 0.007 249 38.4 4953 0.378 0.073 -- 0.297 -- 0.243 0.011 247 78.5 3154 0.882 0.066 -- 0.709 -- 0.348 0.009 234 57.7 4855 1.307 0.043 -- 0.767 -- 0.271 0.002 178 23.3 2656 0.583 0.022 -- 0.647 -- 0.277 0.004 199 23.7 1457 0.908 0.072 -- 0.033 -- 0.242 0.010 213 36.2 1858 0.573 0.064 -- 0.619 -- 0.444 0.003 243 40.8 4759 1.144 0.064 -- 0.603 -- 0.359 0.016 205 14.2 2760 0.883 0.042 -- 0.150 -- 0.257 0.015 217 39.2 4661 0.699 -- 0.207 0.955 -- 0.218 0.012 200 25.1 3362 1.497 -- 0.536 0.229 -- 0.117 0.002 222 19.8 3363 0.258 -- 0.341 0.135 -- 0.227 0.007 201 35.9 1664 0.468 -- 0.360 0.355 -- 0.220 0.002 207 51.8 2765 0.441 -- 0.396 0.595 -- 0.377 0.009 157 10.9 1566 0.405 -- 0.897 0.534 -- 0.168 0.004 172 30.7 4867 1.254 -- 0.097 0.849 -- 0.272 0.010 167 54.5 1268 0.646 -- 0.016 0.264 -- 0.363 0.001 166 61.3 1669 1.421 -- 0.143 0.434 -- 0.318 0.019 184 28.0 2670 1.206 -- 0.178 0.542 -- 0.404 0.001 191 73.5 1171 0.881 0.045 0.012 0.273 -- 0.301 0.017 202 32.9 1572 1.365 0.019 0.047 0.337 -- 0.272 0.004 242 29.6 1173 0.980 0.015 0.162 0.924 -- 0.223 0.013 227 74.0 4374 0.592 0.051 0.010 0.719 -- 0.404 0.019 227 75.1 2075 1.100 0.046 0.178 0.898 -- 0.101 0.018 209 79.9 28__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 76______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________76 0.038 0.278 0.848 0.046 0.008 1.558 0.167 12.46 0.70877 0.168 0.707 0.952 0.030 0.009 1.092 0.253 10.45 0.16178 0.271 0.415 0.904 0.020 0.005 0.466 0.344 11.15 0.88679 0.253 0.712 0.448 0.022 0.010 0.980 0.296 12.97 0.57480 0.027 0.196 0.545 0.045 0.003 1.114 0.203 11.93 0.42381 0.228 0.180 0.543 0.036 0.006 1.228 0.370 11.44 0.61482 0.184 0.028 0.988 0.022 0.005 0.696 0.428 12.41 0.83483 0.092 0.657 0.819 0.012 0.006 1.776 0.235 8.22 0.75584 0.296 0.277 0.206 0.031 0.003 1.997 0.107 12.43 0.59185 0.275 0.590 0.894 0.049 0.006 1.727 0.127 10.93 0.52186 0.082 0.182 0.627 0.013 0.009 1.291 0.375 9.62 0.22387 0.201 0.362 0.750 0.049 0.006 1.062 0.487 9.47 0.88688 0.116 0.513 0.228 0.026 0.002 0.437 0.326 8.93 0.71089 0.161 0.761 0.800 0.011 0.002 0.717 0.195 11.38 0.86690 0.254 0.099 0.223 0.031 0.003 0.383 0.187 12.86 0.06691 0.299 0.227 0.243 0.015 0.002 0.718 0.155 11.73 0.96992 0.063 0.509 0.608 0.049 0.001 0.188 0.184 8.92 0.77793 0.179 0.315 0.673 0.020 0.006 1.041 0.360 10.41 0.68094 0.269 0.573 0.589 0.018 0.006 0.808 0.317 12.14 0.86395 0.239 0.643 0.497 0.048 0.006 0.746 0.137 12.49 0.50296 0.142 0.665 0.549 0.019 0.008 1.266 0.357 9.91 0.79697 0.182 0.791 0.892 0.018 0.005 1.684 0.152 12.81 0.41898 0.260 0.786 0.889 0.031 0.008 0.605 0.300 12.25 0.08399 0.298 0.405 0.687 0.049 0.009 0.167 0.197 11.60 0.461100 0.198 0.566 0.429 0.017 0.001 1.715 0.383 11.77 0.241______________________________________
TABLE 8__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________76 0.770 0.069 0.562 0.644 -- 0.178 0.011 242 32.0 3677 1.183 0.039 0.104 0.666 -- 0.321 0.002 195 14.8 3078 1.261 0.024 0.157 0.136 -- 0.200 0.014 187 40.8 1979 1.250 0.042 0.071 0.233 -- 0.487 0.013 235 53.2 4980 0.762 0.065 0.019 0.660 -- 0.464 0.003 212 31.2 2981 0.676 -- -- -- 0.082 0.204 0.014 183 57.2 2682 0.581 -- -- -- 0.081 0.380 0.013 167 38.9 4683 0.716 -- -- -- 0.090 0.264 0.004 184 59.2 3884 0.695 -- -- -- 0.083 0.134 0.018 202 62.3 1085 1.407 -- -- -- 0.076 0.268 0.001 241 61.1 2986 1.129 -- -- -- 0.084 0.137 0.007 218 67.7 2187 1.415 -- -- -- 0.082 0.415 0.017 152 61.7 1688 1.211 -- -- -- 0.040 0.183 0.008 213 20.0 1989 0.758 -- -- -- 0.065 0.309 0.012 168 26.2 4090 0.956 -- -- -- 0.039 0.473 0.004 238 58.4 2491 1.400 0.002 -- -- 0.069 0.349 0.006 190 60.0 4192 1.017 0.024 -- -- 0.037 0.210 0.002 243 79.0 1693 1.367 0.039 -- -- 0.050 0.133 0.016 217 58.3 3994 0.736 0.020 -- -- 0.080 0.195 0.014 179 46.5 3695 1.317 0.083 -- -- 0.052 0.466 0.016 198 55.2 3496 1.405 0.051 -- -- 0.075 0.218 0.010 194 64.5 4197 0.565 0.037 -- -- 0.073 0.132 0.015 232 49.8 4598 0.412 0.066 -- -- 0.023 0.482 0.009 237 28.1 1499 0.479 0.004 -- -- 0.027 0.347 0.003 223 45.0 34100 0.394 0.069 -- -- 0.016 0.396 0.001 162 79.7 14__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 9______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________101 0.019 0.256 0.274 0.023 0.004 0.876 0.266 11.27 0.616102 0.100 0.392 0.765 0.014 0.001 1.758 0.380 10.96 0.270103 0.061 0.732 0.450 0.038 0.008 1.892 0.357 11.79 0.383104 0.249 0.253 0.688 0.043 0.008 1.646 0.284 9.74 0.154105 0.282 0.275 0.824 0.036 0.007 1.357 0.470 10.74 0.763106 0.212 0.148 0.595 0.044 0.007 0.453 0.098 8.14 0.897107 0.099 0.043 0.977 0.015 0.006 0.226 0.380 8.02 0.757108 0.284 0.478 0.899 0.017 0.004 1.955 0.499 8.69 0.513109 0.237 0.048 0.922 0.017 0.004 1.291 0.312 11.17 0.856110 0.167 0.070 0.793 0.043 0.004 0.482 0.135 11.37 0.489111 0.123 0.680 0.262 0.021 0.003 1.753 0.495 12.72 0.084112 0.156 0.085 0.278 0.020 0.009 1.696 0.356 11.17 0.827113 0.038 0.770 0.994 0.047 0.002 0.663 0.475 10.15 0.416114 0.108 0.533 0.552 0.029 0.009 1.814 0.485 10.58 0.526115 0.274 0.302 0.304 0.014 0.005 1.769 0.473 8.42 0.851116 0.015 0.624 0.410 0.030 0.006 1.807 0.300 12.12 0.587117 0.255 0.467 0.614 0.024 0.003 0.392 0.272 10.10 0.910118 0.177 0.373 0.265 0.023 0.004 1.667 0.476 8.30 0.017119 0.272 0.483 0.721 0.036 0.002 1.254 0.323 10.19 0.590120 0.156 0.164 0.520 0.029 0.001 1.393 0.118 9.17 0.815121 0.030 0.730 0.614 0.030 0.005 1.490 0.395 11.15 0.877122 0.239 0.382 0.759 0.046 0.009 1.912 0.116 9.62 0.474123 0.111 0.044 0.701 0.026 0.007 1.124 0.489 10.50 0.281124 0.283 0.645 0.990 0.036 0.001 0.417 0.250 12.20 0.493125 0.226 0.762 0.575 0.024 0.005 0.131 0.157 10.70 0.298______________________________________
TABLE 10__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________101 0.381 -- 0.089 -- 0.094 0.310 0.017 170 39.6 40102 1.346 -- 0.057 -- 0.054 0.160 0.016 217 43.3 21103 0.263 -- 0.646 -- 0.046 0.218 0.012 221 68.1 43104 0.645 -- 0.097 -- 0.044 0.164 0.007 152 57.9 15105 1.425 -- 0.213 -- 0.019 0.273 0.005 227 25.4 23106 0.904 -- 0.941 -- 0.034 0.213 0.019 216 19.2 15107 1.275 -- 0.589 -- 0.060 0.268 0.006 189 17.4 20108 0.827 -- 0.257 -- 0.068 0.170 0.007 211 32.1 43109 1.104 -- 0.440 -- 0.031 0.210 0.015 155 77.8 34110 1.060 -- 0.545 -- 0.056 0.450 0.016 236 62.2 38111 0.271 0.039 0.030 -- 0.024 0.298 0.004 225 67.8 45112 0.296 0.052 0.119 -- 0.043 0.234 0.010 192 38.7 20113 0.729 0.085 0.011 -- 0.084 0.334 0.019 202 57.0 13114 1.148 0.009 0.066 -- 0.073 0.466 0.016 176 31.0 29115 1.156 0.041 0.174 -- 0.073 0.108 0.005 182 79.5 17116 0.997 0.052 0.030 -- 0.012 0.139 0.017 241 76.1 25117 0.921 0.007 0.023 -- 0.086 0.432 0.009 219 32.3 20118 1.171 0.032 0.149 -- 0.086 0.262 0.011 187 67.8 28119 1.341 0.089 0.057 -- 0.030 0.105 0.010 212 19.7 39120 0.364 0.049 0.199 -- 0.024 0.232 0.010 213 76.1 39121 1.085 -- -- 0.518 0.085 0.321 0.002 158 40.8 35122 0.507 -- -- 0.911 0.096 0.245 0.010 168 31.1 16123 0.813 -- -- 0.693 0.072 0.482 0.010 161 61.2 49124 0.958 -- -- 0.058 0.032 0.307 0.015 204 73.3 40125 1.176 -- -- 0.171 0.035 0.389 0.018 217 45.3 39__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 11______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________126 0.283 0.545 0.806 0.037 0.009 0.633 0.067 11.89 0.372127 0.079 0.145 0.236 0.044 0.003 0.416 0.070 11.77 0.918128 0.101 0.490 0.613 0.011 0.009 0.723 0.246 11.22 0.617129 0.112 0.546 0.487 0.046 0.001 1.964 0.230 11.21 0.157130 0.168 0.078 0.806 0.016 0.007 0.672 0.102 10.14 0.713131 0.176 0.388 0.916 0.029 0.008 1.932 0.406 11.45 0.488132 0.048 0.090 0.586 0.013 0.008 0.474 0.325 8.67 0.178133 0.274 0.484 0.754 0.035 0.005 1.318 0.165 12.68 0.954134 0.180 0.543 0.766 0.042 0.006 1.076 0.457 11.88 0.494135 0.258 0.024 0.373 0.023 0.007 1.989 0.391 9.73 0.029136 0.130 0.645 0.536 0.044 0.006 0.611 0.278 12.22 0.208137 0.277 0.191 0.985 0.033 0.009 0.139 0.415 10.17 0.214138 0.181 0.384 0.681 0.017 0.004 1.865 0.224 12.09 0.745139 0.181 0.587 0.978 0.044 0.006 1.433 0.235 8.94 0.500140 0.044 0.160 0.419 0.022 0.003 0.142 0.082 11.61 0.652141 0.116 0.041 0.761 0.018 0.003 1.168 0.072 11.08 0.397142 0.015 0.763 0.554 0.019 0.001 1.115 0.076 8.29 0.928143 0.231 0.128 0.741 0.033 0.004 1.269 0.393 9.13 0.422144 0.237 0.626 0.679 0.028 0.005 1.969 0.434 9.59 0.072145 0.236 0.452 0.514 0.011 0.001 1.700 0.059 8.08 0.062146 0.135 0.148 0.803 0.030 0.007 1.742 0.254 8.08 0.083147 0.129 0.624 0.481 0.031 0.002 0.580 0.425 10.43 0.812148 0.279 0.092 0.512 0.044 0.007 0.434 0.209 8.66 0.454149 0.200 0.253 0.237 0.034 0.009 0.723 0.138 11.16 0.182150 0.237 0.466 0.610 0.049 0.009 1.793 0.296 11.37 0.184______________________________________
TABLE 12__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________126 1.059 -- -- 0.733 0.010 0.207 0.004 219 60.8 11127 0.872 -- -- 0.945 0.019 0.237 0.014 229 63.5 46128 1.484 -- -- 0.472 0.033 0.156 0.015 214 30.4 49129 1.198 -- -- 0.523 0.070 0.432 0.018 246 10.9 50130 0.892 -- -- 0.752 0.055 0.346 0.001 190 51.7 34131 1.487 0.008 -- 0.873 0.050 0.167 0.003 166 61.5 11132 0.625 0.059 -- 0.091 0.075 0.180 0.018 245 19.4 47133 0.490 0.011 -- 0.559 0.099 0.453 0.013 193 77.2 49134 1.317 0.029 -- 0.965 0.049 0.263 0.011 230 73.7 26135 1.413 0.081 -- 0.038 0.034 0.482 0.005 175 57.5 24136 1.023 0.035 -- 0.412 0.068 0.392 0.007 195 75.0 32137 0.370 0.012 -- 0.798 0.080 0.257 0.012 211 70.9 16138 1.018 0.078 -- 0.887 0.040 0.360 0.015 240 22.6 25139 0.601 0.053 -- 0.365 0.056 0.174 0.010 202 13.2 25140 1.318 0.055 -- 0.912 0.010 0.373 0.018 214 55.7 24141 1.461 -- 0.893 0.227 0.099 0.433 0.005 197 59.3 30142 1.291 -- 0.389 0.493 0.025 0.233 0.005 219 36.6 31143 1.031 -- 0.277 0.404 0.029 0.442 0.010 199 70.7 14144 0.928 -- 0.128 0.139 0.039 0.339 0.013 155 69.5 45145 0.579 -- 0.089 0.880 0.072 0.199 0.003 206 11.7 34146 0.875 -- 0.348 0.329 0.098 0.297 0.017 221 49.5 27147 1.417 -- 0.113 0.662 0.045 0.100 0.013 168 21.4 11148 1.142 -- 0.247 0.075 0.020 0.494 0.004 217 10.9 15149 0.288 -- 0.022 0.243 0.040 0.149 0.013 185 64.9 25150 0.401 -- 0.372 0.357 0.076 0.337 0.005 242 58.3 10__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 13______________________________________(mass %) Invention steelsNo. C Si Mn P S Nb V Cr Mo______________________________________151 0.157 0.497 0.978 0.037 0.010 0.234 0.321 12.72 0.652152 0.154 0.087 0.687 0.026 0.008 1.123 0.289 8.62 0.764153 0.144 0.189 0.303 0.023 0.001 1.021 0.072 10.12 0.231154 0.176 0.143 0.360 0.015 0.009 0.282 0.193 8.02 0.213155 0.159 0.104 0.608 0.010 0.002 1.169 0.288 10.81 0.401156 0.010 0.619 0.814 0.016 0.008 1.219 0.230 9.53 0.516157 0.069 0.270 0.320 0.020 0.007 0.757 0.317 10.02 0.178158 0.246 0.373 0.476 0.049 0.010 0.142 0.186 10.76 0.205159 0.159 0.680 0.631 0.032 0.008 0.675 0.143 10.13 0.649160 0.152 0.556 0.529 0.035 0.004 1.745 0.275 9.10 0.748______________________________________
TABLE 14__________________________________________________________________________(mass %) Invention steels CS VE TONo. W Zr Ta Hf Ti N O MPa J μm__________________________________________________________________________151 0.429 0.091 0.090 0.113 0.055 0.338 0.002 206 37.3 16152 0.610 0.090 0.715 0.686 0.085 0.421 0.017 197 51.9 12153 0.554 0.012 0.131 0.772 0.091 0.269 0.017 183 43.9 24154 0.478 0.071 0.497 0.062 0.047 0.350 0.014 231 26.6 40155 1.283 0.091 0.492 0.726 0.013 0.340 0.003 212 13.8 29156 1.301 0.090 0.202 0.490 0.053 0.120 0.005 245 53.5 16157 0.741 0.085 0.361 0.510 0.048 0.164 0.015 199 19.2 31158 1.158 0.046 0.140 0.980 0.015 0.147 0.010 242 28.4 20159 0.833 0.091 0.089 0.591 0.015 0.339 0.009 192 24.2 31160 0.668 0.038 0.034 0.026 0.020 0.218 0.008 218 54.3 10__________________________________________________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
TABLE 15__________________________________________________________________________Comparison steels (mass %)No. C Si Mn P S Nb V Cr Mo W__________________________________________________________________________161 0.02 0.06 0.45 0.014 0.008 0.051 0.20 8.53 0.592 0.87162 0.07 0.07 0.57 0.012 0.004 0.066 0.22 8.99 0.424 0.88163 0.23 0.10 0.52 0.016 0.004 0.074 0.18 9.05 0.560 0.86164 0.15 0.13 0.45 0.011 0.002 0.033 0.19 9.23 0.550 0.77165 0.29 0.12 0.98 0.008 0.001 0.127 0.08 12.1 0.320 0.11166 0.15 0.09 0.24 0.009 0.001 0.290 0.45 12.7 0.007 1.80167 0.18 0.09 0.44 0.009 0.001 0.014 0.31 11.4 0.989 0.99168 0.11 0.12 0.74 0.004 0.001 2.880 0.22 11.8 0.679 0.67169 0.09 0.21 0.81 0.044 0.002 0.321 0.20 10.5 0.814 0.23170 0.10 0.23 0.99 0.024 0.001 0.545 0.19 10.0 0.333 0.77171 0.22 0.21 0.11 0.012 0.001 1.227 0.40 9.76 0.545 1.21172 0.07 0.27 0.07 0.013 0.009 1.621 0.49 9.00 0.512 1.09173 0.23 0.23 0.09 0.002 0.010 1.998 0.07 8.86 0.533 1.15__________________________________________________________________________
TABLE 16______________________________________Comparison steels (mass %) CS VE TONo. Zr Ta Hf Ti N O MPa J (μm)______________________________________161 0.007 0.65 -- 0.034 0.072 0.007 120 70 760162 0.008 0.77 -- 0.031 0.081 0.009 107 28 660163 0.002 0.78 -- 0.044 0.872 0.007 205 6 50164 0.012 0.71 0.66 0.100 0.525 0.002 185 3 35165 0.011 0.76 0.87 0.010 0.164 0.002 65 95 35166 -- -- 0.81 -- 0.128 0.002 90 2 20167 -- -- 0.59 -- 0.154 0.001 70 60 25168 -- -- -- 0.060 0.332 0.002 116 4 5169 0.145 0.89 -- 0.071 0.425 0.002 187 4 25170 -- 1.21 -- 0.032 0.202 0.002 153 7 40171 0.011 0.32 1.13 -- 0.191 0.008 220 7 45172 0.540 0.05 0.22 0.29 0.103 0.012 210 8 15173 0.880 -- 0.10 -- 0.200 0.006 24 2 30______________________________________ CS: Creep rupture strength at 650° C., 150 thousand hours; VE: Charpy impact absorption energy at 0° C. after aging at 700° C. for 10 thousand hours; TO: Oxidation scale thickness after 650° C., 10 thousand hour hightemperature oxidation
The present invention provides a high-nitrogen ferritic heat-resisting steel with high Nb content exhibiting a high rupture strength after prolonged creep and superior high-temperature oxidation resistance and, as such, can be expected to make a major contribution to industrial progress.
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A high-nitrogen ferritic heat-resisting steel with high niobium content comprises, in weight per cent, 0.01-0.30% C, 0.02-0.80% Si, 0.20-1.00% Mn, 8.00-13.00% Cr, 0.005-1.00% Mo, 0.20-1.50% W, 0.05-1.00% V, over 0.12 up to 2.00% Nb and 0.10-0.50%N, the balance being Fe and unavoidable impurities. A method of producing the steel comprises melting and equilibrating the steel components in an atmosphere of a mixed gas of a prescribed nitrogen partial pressure or nitrogen gas and thereafter casting or solidifying the resulting melt in an atmosphere controlled to have a total pressure of not less than 2.5 bar and a nitrogen partial pressure of not less than 1.0 bar, with the relationship between the nitrogen partial pressure p and the total pressure P being
P>2.5p.
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FIELD OF THE INVENTION
[0001] The present invention generally relates to techniques for monitoring and controlling continuous sheetmaking systems such as a papermaking machine and more, specifically to maintaining proper cross-directional alignment in sheetmaking systems by extracting alignment information from a closed-loop CD control system. BACKGROUND OF THE INVENTION
[0002] In the art of making paper with modern high-speed machines, sheet properties must be continually monitored and controlled to assure sheet quality and to minimize the amount of finished product that is rejected when there is an upset in the manufacturing process. The sheet variables that are most often measured include basis weight, moisture content, and caliper (i.e., thickness) of the sheets at various stages in the manufacturing process. These process variables are typically controlled by, for example, adjusting the feedstock supply rate at the beginning of the process, regulating the amount of steam applied to the paper near the middle of the process, or varying the nip pressure between calendaring rollers at the end of the process. Papermaking devices are well known in the art and are described, for example, in “Handbook for Pulp & Paper Technologists” 2nd ed., G. A. Smook, 1992, Angus Wilde Publications, Inc., and “Pulp and Paper Manufacture” Vol III (Papermaking and Paperboard Making), R. MacDonald, ed. 1970, McGraw Hill. Sheetmaking systems are further described, for example, in U.S. Pat. No. 5,539,634 to He, U.S. Pat. No. 5,022,966 to Hu, U.S. Pat. No. 4,982,334 to Balakrishnan, U.S. Pat. No. 4,786,817 to Boissevain et al, and U.S. Pat. No. 4,767,935 to Anderson et al. Process control techniques for papermaking machines are further described, for instance, in U.S. Pat. No. 6,149,770 to Hu et al., U.S. Pat. No. 6,092,003 to Hagart-Alexander et. al, U.S. Pat. No. 6,080,278 to Heaven et al., U.S. Pat. No. 6,059,931 to Hu et al., U.S. Pat. No. 6,853,543 to Hu et al., and U.S. Pat. No. 5,892,679 to He.
[0003] On-line measurements of sheet properties can be made in both the machine direction and in the cross direction. In the sheetmaking art, the term machine direction (MD) refers to the direction that the sheet material travels during the manufacturing process, while the term cross direction (CD) refers to the direction across the width of the sheet which is perpendicular to the machine direction.
[0004] Papermaking machines typically have several control stages with numerous, independently-controllable actuators that extend across the width of the sheet at each control stage. For example, a papermaking machine will typically include a headbox having a plurality of slice lip force actuators at the front which allow the stock in the headbox to flow out on the fabric of the web or wire. The papermaking machine might also include a steam box having numerous steam actuators that control the amount of heat applied to several zones across the sheet. Similarly, in a calendaring stage, a segmented calendaring roller can have several actuators for controlling the nip pressure applied between the rollers at various zones across the sheet.
[0005] All of the actuators in a stage are operated to maintain a uniform and high quality finished product. Such control might be performed, for instance, by an operator who periodically monitors sensor readings and then manually adjusts each of the actuators until the desired output readings are produced. Papermaking machines can further include computer control systems for automatically adjusting cross-directional actuators using signals sent from scanning sensors.
[0006] In making paper, virtually all MD variations can be traced back to high-frequency or low-frequency pulsations in the headbox approach system. CD variations are more complex. Preferably, the cross-directional dry weight profile of the final paper product is flat, that is, the product exhibits no CD variation, however, this is seldom the case. Various factors contribute to the non-uniform CD profiles such as non-uniformities in pulp stock distribution, drainage, drying and mechanical forces on the sheet. The causes of these factors include, for example, (i) non-uniform headbox delivery, (ii) clogging of the plastic mesh fabric of the wire, (iii) varying amounts of tension on the wire, (iv) uneven vacuum distribution, (v) uneven press or calendar nip pressures, and (vi) uneven temperatures and airflows across the CD that lead to moisture non-uniformities.
[0007] Cross-directional measurements are typically made with a scanning sensor that periodically traverses back and forth across the width of the sheet material. The objective of scanning across the sheet is to measure the variability of the sheet in both CD and MD. Based on the measurements, corrections to the process are commanded by the control computer and executed by the actuators to make the sheet more uniform.
[0008] In practice, control devices that are associated with sheetmaking machines normally include a series of actuator systems arranged in the cross direction. For example, in a typical headbox, the control device is a flexible member or slice lip that extends laterally across a small gap at the bottom discharge port of the headbox. The slice lip is movable for adjusting the area of the gap and, hence, for adjusting the rate at which feedstock is discharged from the headbox. A typical slice lip is operated by a number of actuator systems, or cells, that operate to cause localized bending of the slice lip at spaced apart locations in the cross-direction. The localized bending of the slice lip member, in turn, determines the width of the feed gap at the various slice locations across the web.
[0009] It is standard practice that sheetmaking machines be controlled by adjusting actuators using measurement signals provided by scanning sensors. In the case of cross-directional control, for example, a commonly suggested control scheme is to measure values at selected cross direction locations on a sheet and then to compare those measured values to target or set point values. The difference for each pair of measured and set point values, i.e., the error, can be used for algorithmically generating appropriate outputs to cross direction control actuators to minimize the error. In such systems, a measurement zone is defined as the cross direction portion of sheet which is measured and used as feedback control for a cross direction actuator zone, and a control zone is defined as the portion of the sheet affected by a cross direction actuator zone.
[0010] In practice, it is difficult to control sheetmaking machines by adjusting actuators using measurement signals provided by scanning sensors. The difficulties particularly arise because the scanning sensors are separated from the control actuators by substantial distances in the machine direction. Because of such separations, it is difficult to determine which measurements zones are associated with which actuator zones. Such difficulties are referred to as alignment problems in the papermaking art. Alignment problems are exacerbated when, as is typical, there is uneven paper shrinkage of a paper web as it progresses through a papermaking process. Another difficulty is that the effect of each actuator is not always limited within the corresponding control zone but spans over a few control zones. Alignment is an important process model parameter for keeping the CD control system stable and operating. The alignment can change over time and subsequently degrade the controller performance and thus paper quality.
[0011] One conventional method for aligning actuator zones with measurement zones involves the use of dye tests. In a dye test, narrow streams of colored liquid are applied to feedstock as it flows beneath a slice lip. The dye streams initially form parallel lines that extend in the machine direction, but those lines may deviate from parallel if there is web shrinkage during the papermaking process. The dye marks passing through the measurement devices reveal the distribution of control zones and therefore specify the alignment of measurement zones.
[0012] Conventional dye tests, however, have numerous drawbacks. The most serious drawback is that the tests destroy finished product and, therefore, it is seldom feasible to perform dye tests at an intermediate point in a sheetmaking production run, even though sheetmaking processes are likely to drift out of control during such times. Further, because of the limited thickness and high absorption characteristics of tissue grades of paper, dye tests are typically limited to paper products that have relatively high weight grades.
[0013] More recently, systems that automatically and non-destructively map and align actuator zones to measurements zones in sheetmaking systems have been developed. Some of these systems perform so-called “bump tests” by disturbing selected actuators and detecting their responses, typically with the CD control system in open-loop. The term “bump test” refers to a procedure whereby an operating parameter on the sheetmaking system, such as a papermaking machine, is altered and changes of certain dependent variables resulting therefrom are measured. Prior to initiating any bump test, the papermaking machine is first operated at predetermined baseline conditions. By “baseline conditions” is meant those operating conditions whereby the machine produces paper of acceptable quality. Typically, the baseline conditions will correspond to standard or optimized parameters for papermaking. Given the expense involved in operating the machine, extreme conditions that may produce defective, non-useable paper are to be avoided. In a similar vein, when an operating parameter in the system is modified for the bump test, the change should not be so drastic as to damage the machine or produce defective paper. After the machine has reached steady state or stable operations, the certain operating parameters are measured and recorded. Sufficient number of measurements over a length of time is taken to provide representative data of the responses to the bump test.
[0014] The standard bump test for CD model identification includes the following steps: (1) placing a control system in open-loop; (2) bumping a subset of the actuators at the headbox to follow a step or series of steps in time; (3) collecting the output data as measured by sensor(s) in the scanner; and (4) running a model identification algorithm to identify the model parameters including alignment.
[0015] For example, U.S. Pat. No. 5,400,258 to He discloses a standard alignment bump test for a papermaking system in which an actuator is moved and its response is read by a scanning sensor and the alignment is identified by the software. U.S. Pat. No. 6,086,237 to Gorinevsky and Heaven discloses a similar technique but with more sophisticated data processing. Specifically, in their bump test the actuators are moved and technique identifies the response as seen by the scanner.
[0016] With current bump test alignment methods, the operator can identify the alignment at the time of the bump test experiment. To track alignment changes over time there is a need to re-identify alignment over the course of days and weeks. Moreover, model identification for a system in closed-loop control is well known to be challenging. This is due in part to the fundamental reason that a closed-loop control system works to eliminate any perturbations, so prior art techniques have endeavored to “sneak” a perturbation into the actuator profile that works against the rest of the system and attaining sufficient excitation of the system is difficult to achieve.
SUMMARY OF THE INVENTION
[0017] The present invention provides a novel method for identifying the alignment of a sheetmaking system while the system remains in closed-loop control. In contrast to the standard model identification techniques that are employed in conjunction with an open or closed-loop control system, the invention exploits the closed-loop control to its advantage. The technique can include the following steps: (1) leaving the control system in closed-loop, (2) artificially inserting a step signal on top of the measurement profile from the scanner (equivalently, inserting a step signal on top of a setpoint target profile), (3) recording the data as the control system moves the actuators to remove the perceived disturbance, and (4) refining or developing a model from the artificial measurement disturbance to the actuator profile.
[0018] The invention is based in part on the recognition that steady-state response of the actuator profile contains information from which the sheetmaking system alignment can be extracted.
[0019] In one embodiment, the invention is directed to a method for alignment of a sheetmaking system having a plurality of actuators arranged in the cross-direction wherein the system includes a control loop for adjusting output from the plurality of actuators in response to sheet profile measurements that are made downstream from the plurality of actuators, the method including the steps of:
(a) determining alignment information from at least two cross-directional positions by: (i) operating the system and measuring a profile of the sheet along the cross-direction of the sheet downstream from the plurality of actuators and generating a profile signal that is proportional to a measurement profile; (ii) adding a perturbative signal to the measurement profile (equivalently, adding a perturbative signal to a setpoint target profile) to generate a modified profile signal that simulates a disturbance (equivalently, a setpoint change) at a position along the measurement profile; (iii) determining alignment shift information based on the closed-loop response of the actuator profile to the modified profile signal (or setpoint change); and (iv) repeating steps (i) through (iii) wherein step (ii) comprises adding a perturbative signal to the measurement profile (equivalently, adding a perturbative signal to a setpoint profile) to generate a modified profile signal that simulates a disturbance (equivalently, a setpoint change) at a different position along the measurement profile thereby obtaining alignment shift information from at least two cross-directional positions;
[0025] (b) identify the changes in alignment of the sheetmaking system, if any, from the alignment shift information from at least two cross-directional positions.
[0026] In another embodiment, the invention is directed to method for extracting cross-directional information from a sheetmaking system having a plurality of actuators arranged in the cross-direction wherein the system includes a control loop for adjusting output from the plurality of actuators in response to sheet profile measurements that are made downstream from the plurality of actuators, the method including the steps of:
(a) operating the system and measuring a profile of the sheet along the cross-direction of the sheet downstream from the plurality of actuators and generating a profile signal that is proportional to a measurement profile; (b) adding a perturbative signal to the measurement profile (equivalently, adding a perturbative signal to a setpoint target profile) to generate a modified profile signal that simulates a disturbance (equivalently, a setpoint change) of at least one position along the measurement profile; and (c) determining cross-directional alignment information based on actuator responses to the modified profile signal.
[0030] In a further embodiment, the invention is directed to a system for alignment of a sheetmaking system having a plurality of actuators arranged in the cross-direction wherein the system includes a control loop for adjusting output from the plurality of actuators in response to sheet profile measurements that are made downstream from the plurality of actuators, the system comprising:
(a) means for determining alignment information from at least two cross-directional positions that includes: (i) means for measuring a profile of the sheet along the cross-direction of the sheet downstream from the plurality of actuators; (ii) generating a profile signal that is proportional to a measurement profile; (iii) means for adding a perturbative signal to the measurement profile (equivalently, adding a perturbative signal to a setpoint target profile) to generate a modified profile signal that simulates a disturbance (equivalently, a setpoint change) at a position along the measurement profile; and (iv) means for determining alignment shift information based on the closed-loop response of the actuator profile to the modified profile signal; and (b) means for identifying the changes in alignment of the sheetmaking system, if any, from the alignment shift information from at least two cross-directional positions.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] FIGS. 1, 2 , and 3 are schematic illustrations of a papermaking system;
[0038] FIG. 4 is a block diagram of a sheetmaking system with the inventive reverse closed-loop bump test;
[0039] FIGS. 5A, 5B , and 5 C are the setpoint target, actuator and measurement profiles vs. CD position, respectively, in a normal steady-state closed-loop operation;
[0040] FIG. 6A shows the setpoint target that is modified with “bumps” at ¼ (low side) and ¾ (high side) across the paper, and FIGS. 6B and 6C show the actuator and measurement profiles vs. CD positions, respectively, in a closed loop steady-state operation with setpoint target bumps;
[0041] FIGS. 7A, 7B , and 7 C show the difference between the closed-loop profiles representing normal steady-state closed loop operation in FIGS. 5A, 5B , and 5 C and the closed-loop steady-state profile with setpoint target bumps of FIGS. 6A, 6B , and 6 C;
[0042] FIGS. 8A and 8C are the graphs of gain vs. frequency of the low side and high side actuator responses to reverse bump tests, respectively;
[0043] FIGS. 8B and 8D are the graph of low-frequency phase vs. frequency of the low side and high side actuator responses; and
[0044] For FIG. 9 , the asterisks plot the slopes of the zero frequency phases illustrated in FIGS. 8B and 8D vs. CD positions of the induced setpoint target bumps that are positioned approximately ¼ and ¾ of the way across the paper; the straight line in FIG. 9 is a straight line fit between these two data appoints.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0045] As shown in FIG. 1 , a system for producing continuous sheet material includes various processing stages such as headbox 10 , steambox 12 , a calendaring stack 14 and reel 16 . The array of actuators 18 in headbox 10 controls the discharge of wet stock (or feedstock) material through a plurality of slices onto supporting web or wire 30 which rotates between rollers 22 and 24 . Similarly, actuators 20 on steambox 12 can control the amount of steam that is injected at points across the moving sheet. Sheet material exiting the wire 30 passes through a dryer 34 which includes actuators 36 that can vary the cross directional temperature of the dryer. A scanning sensor 38 , which is supported on supporting frame 40 , continuously traverses and measures properties of the finished sheet in the cross direction. Scanning sensors are known in the art and are described, for example, in U.S. Pat. No. 5,094,535 to Dalquist, U.S. Pat. No. 4,879,471 to Dalquist, et al, U.S. Pat. No. 5,315,124 to Goss, et al, and U.S. Pat. No. 5,432,353 to Goss et al, which are incorporated herein. The finished sheet product 42 is then collected on reel 16 . As used herein, the “wet end” portion of the system includes the headbox, the web, and those sections just before the dryer, and the “dry end” comprises the sections that are downstream from the dryer. Typically, the two edges of the wire in the cross direction are designated “front” and “back” (alternatively, referred as the “high” and ‘low”) with the back side being adjacent to other machinery and less accessible than the front side.
[0046] The system further includes a profile analyzer 44 that is connected, for example, to scanning sensor 38 and actuators 18 , 20 , 32 and 36 on the headbox 10 , steam box 12 , vacuum boxes 28 , and dryer 34 , respectively. The profile analyzer is a computer which includes a control system that operates in response to the cross-directional measurements from scanner sensor 38 . In operation, scanning sensor 38 provides the analyzer 44 with signals that are indicative of the magnitude of a measured sheet property, e.g., caliper, dry basis weight, gloss or moisture, at various cross-directional measurement points. The analyzer 44 also includes software for controlling the operation of various components of the sheetmaking system, including, for example, the above described actuators.
[0047] FIG. 2 depicts a slice lip control system which is mounted on a headbox 10 for controlling the extent to which a flexible slice lip member 46 extends across the discharge gap 48 at the base of the headbox 10 . The slice lip member 46 extends along the headbox 10 across the entire width of the web in the cross-direction. The actuator 18 controls of the slice lip member 46 , but it should be understood that the individual actuators 18 are independently operable. The spacing between the individual actuators in the actuator array may or may not be uniform. Wetstock 50 is supported on wire 30 which rotates by the action of rollers 22 and 24 .
[0048] As an example shown in FIG. 3 , the amount of feedstock that is discharged through the gap between the slice lip member and the surface of the web 30 of any given actuator is adjustable by controlling the individual actuator 18 . The feed flow rates through the gaps ultimately affect the properties of the finished sheet material, i.e., the paper 42 . Specifically, as illustrated, a plurality of actuators 18 extend in the cross direction over web 30 that is moving in the machine direction indicated by arrow 6 . Actuators 18 can be manipulated to control sheet parameters in the cross direction. A scanning device 38 is located downstream from the actuators and it measures one or more the properties of the sheet. In this example, several actuators 18 are displaced as indicated by arrows 4 and the resulting changes in sheet property is detected by scanner 38 as indicated by the scanner profile 54 . By averaging many scans of the sheet, the peaks of profile 54 indicated by arrows 56 can be determined. This type of operation is typically used in traditional open and closed-loop bump tests. In contrast, the inventive reverse bump test does not directly send perturbations to the actuator profile. It should be noted that besides being positioned in the headbox, actuators can be placed at one or more strategic locations in the papermaking machine including, for example, in the steamboxes, dryers, and vacuum boxes. The actuators are preferably positioned along the CD at each location.
[0049] FIG. 4 illustrates an embodiment the closed-loop reverse bump test for a sheetmaking system such as that shown in FIG. 1 . The term “reverse bump test” denotes that in contrast to standard model identification techniques that perturb one or more actuators and then extract information from the response, e.g., measurement profile from the scanner, the inventive technique artificially inserts a step signal d y on top of the measurement profile y (equivalently, a step signal d r on top of the setpoint target profile r) and then analyzes the actuator response while the system is under closed-loop control.
[0050] Referring to FIG. 4 , the process employs a controller denoted by K for use with a profile analyzer for the sheetmaking system denoted G. Signals associated with this process include r, u, and y. The r signal represents a selected target or selected setpoint level, signal u represents the actuator signal, and signal y represents the measurement profile, e.g., scanner measurements. When controlling and measuring sheetmaking parameters in the cross direction, it is understood that the signals will be arrays or vectors, so that, for instance, y can be described as a vector whose ith component is the weight level or moisture level or thickness of a sheet at the ith position along a scanner. The signal d y represents an unmeasured disturbance or a perturbation or offset signal that is inserted in the measurement profile. The signal d r represents a perturbation or offset signal that is inserted on the target profile. The controller K can be any suitable closed-loop controller and may contain many signal processing components, for example, spatial and/or temporal filters, a proportional integral derivative (PID) controller, Dahlin controller, proportional plus integral (PI) controller, or proportional plus derivative (PD) controller, or a model predictive controller (MPC). An MPC is described in U.S. Pat. No. 6,807,510 to Backstrom and He, which is incorporated herein by reference. During normal production, a y signal profile is continuously generated by scanning the finished paper product and this signal is compared to the r signal for any error defined by e=r−y when d r =0.
[0051] The inventive closed-loop reverse bump test can be implemented to generate alignment data for any of the actuators that control cross direction operations of the various components for the sheetmaking system shown in FIG. 1 provided that the actuators are connected to the perturbed profile measurement y, setpoint r, or error e in the closed-loop through controller K. Therefore, while the invention will be illustrated by monitoring the actuators at the headbox which control that feedstock discharge through the individual slices, the invention can also be implemented to ascertain alignment data for any of the actuators that control cross directional unit operations in the sheetmaking machine including, for example, the steambox, dryer, and vacuum box.
[0052] In implementing the reverse bump test, a sheetmaking system G, such as a papermaking machine, is initially operated with actuators that are set by the feedback controller K to cause y to match a target signal profile r as closely as possible. During paper production, a y signal profile is generated by scanning the finished paper product. Thereafter, with the papermaking machine still in closed-loop control, the target profile is modified by inserting a pertubative signal d r to create a setpoint target profile at summer 64 of r+d r . The measurement profile y signal profile from the scanner will be subtracted from the setpoint target profile at summer 62 . Controller K will convert the error signal e from the comparator into an actuator signal profile u that is received by the papermaking machine. The effect will be that the papermaking machine feedstock discharge through the slice lip opening at the headbox that will be adjusted to have the measurement profile y follow the perceived change in setpoint target.
[0053] The following describes a preferred technique of implementing the inventive reverse bump test for closed-loop identification of CD controller alignment. In operation, the control system of the papermaking machine, for instance, is left in the closed-loop and a step signal is artificially inserted on top of the measurement profile from the scanner which measures the finished paper product. Data is recorded as the control system responds by adjusting the actuators at the headbox to remove the perceived perturbation. Finally, a model, which contains alignment information, is identified from the data comprising the artificial measurement disturbance and the resulting actuator profile. In actual implementation of the reverse bump test, the “bump” should not be so drastic as to cause the final product, e.g., paper, to be unfit for sale.
[0054] Reverse Bump Test Design And Data Collection Procedure
[0055] (1) Design a bump test by designing the setpoint target bumps (δr).
[0056] a. Using a papermaking machine for illustrative purposes, preferably at least two well-separated “bump” are positioned in the cross-direction. For example, they can be located at ¼ and ¾ across the sheet width.
[0057] b. In the time domain, operate the machine at a baseline and then operate the machine in a plurality of steps up and down. The simplest technique is to execute a single step that lasts long enough for the closed-loop controller to reach its new steady state with the setpoint bumps.
[0058] (2) Run the reverse bump test. With the CD in closed-loop control, modify the setpoint target profile with (r+δr) as designed above. While logging the data for:
[0059] a. Two dimensional setpoint target array (r).
[0060] b. Two dimensional setpoint target bumps (δr).
[0061] c. Two dimensional scanner profile measurements (y).
[0062] d. Two dimensional actuator profile array (u).
[0063] To illustrate the utility of the inventive technique, computer simulations implementing the reverse bump test for closed-loop identification were conducted using Matlab R12 software from Mathworks. The simulations modeled a papermaking machine as depicted in FIG. 4 with a headbox having 45 actuators that controlled pulp stock discharge through the corresponding slice lip opening. The weight of the finished paper was measured by a scanner at 250 points or bins across the width of the paper from the front to back side of the machine; each bin represents a distance of about 5 mm. The weight of the finished paper had a mean value of about 191 lb per 1000 units of sheet. The model also simulated closed-loop control of the actuators in response to signals from the scanner.
[0064] FIGS. 5A and 5C show the setpoint target and measurement profiles for paper vs. CD position in a normal steady-state closed loop operation. As is apparent, the setpoint target and measurement profiles for the finished paper are essentially the same and are represented by horizontal profiles depicting paper that has a weight of slightly more than 191 lb per 1000 units of sheet. Note that an actual papermaking machine would typically not have such a flat measurement profile y as there are typically uncontrollable high spatial frequency components that are not removed by the controller and do not affect this analysis. FIG. 5B is the headbox actuator profile and shows how the flow of pulp through the slices in the headbox varies across the headbox. The change in actuator response is relative to a baseline of zero. These profiles illustrate the appearance of the cross-directional control system prior to performing the “reverse bump test” experiment.
[0065] FIGS. 6A and 6C show the setpoint target and measurement profiles for paper vs. CD position in a steady-state closed loop operation after the setpoint target has been modified with ‘bumps’ at ¼ and ¾ across the paper sheet. As is apparent, the modifying setpoint target causes a corresponding change in the measurement profile for the finished paper. FIG. 6B is the headbox actuator profile and shows the slice jack actuator positions across the headbox. These profiles illustrate the appearance of the cross-directional control system during the “reverse bump test” experiment once the closed-loop has reached the steady-state.
[0066] Alignment Identification Algorithm
[0067] a. Using standard techniques, the response of the actuator profile to the setpoint target bumps is computed. In one preferred method, the actuator profile can be computed as the difference between the baseline actuator profile (prior to bumps) and the steady-state actuator profile (after bumps are inserted). As an illustration, FIGS. 7A, 7B , and 7 C are the difference between the closed-loop target setpoint, actuator and measurement profiles. The actuator array illustrated is denoted as u resp . Specifically, the actuator profile plotted in FIG. 7B was computed by subtracting the normal operation closed-loop actuator profile in FIG. 5B from the closed-loop actuator profile resulting from the setpoint target bumps in FIG. 6B ,
u resp =u bump −u normal
[0068] The 1-dimensional array profiles u normal and u bump are the best estimates of the actuator profile during the baseline collection and the actuator profile for the system having reached steady-state after the bumps.
[0069] b. Next the actuator response profile and the setpoint target bump profile (as illustrated in the graphs in FIGS. 7B and 7A ) are partitioned. in the middle to make two arrays of approximately equal length:
u resp = [ u low u high ]
δ r = [ δ r low δ r high ]
[0070] c. Compute the Fourier transforms of each of the component arrays:
U low ƒ =ƒƒt ( u low ) δ R low ƒ =ƒƒt (δƒ low )
U high ƒ =ƒƒt ( u high ) δ R high ƒ =ƒƒt (δƒ high )
[0071] d. Now the closed-loop spatial frequency response of the low end of the sheet and the high end of the sheet may be given by:
T low ƒ =U low ƒ ./δR low ƒ
T high ƒ =U high ƒ ./δR high ƒ
where “./” denotes element-by-element division.
[0072] e. For CD control systems, the low-frequency components of the arrays T low ƒ , and T high ƒ will be equal to the inverse of the frequency response of the process itself, as practical cross-directional control will eliminate all low spatial frequency components of the steady-state error profile e=r−y, thus meaning that the actuator profile u contains exactly the correct alignment at low spatial frequencies. Thus the low frequency phase information in the arrays T low ƒ and T high ƒ will contain the true alignment information of the system.
[0073] e. The phase information of phase(T low ƒ ) and phase(T high ƒ ) could potentially be used directly. Alternatively, as illustrated here, the possibility of using the reverse bump test to compute the alignment change between two reverse bump tests that are performed perhaps days/weeks/months apart was considered. In this case, the alignment change between the alignment at the time of an “old” reverse relative to the alignment at the time of a “new” reverse bump test is computed, as follows:
H low ƒ =U low ƒ (new)./ U low ƒ (old)
H high ƒ =U high ƒ (new)./ U high ƒ (old)
then the phase information phase(H low ƒ ) and phase(H high ƒ ) are plotted with respect to the spatial frequency v as shown in FIGS. 8B and 8D , respectively.
[0074] g. A straight line through the low frequency components of phase(H low ƒ ) and phase(H high ƒ ) is fitted through the low frequency components of the two plots of FIGS. 8B and 8D , respectively. For the example illustrated in FIG. 8 , the low side phase ( FIG. 8B ) has a slope of 29.5 engineering units at zero frequency. Since the simulation used millimeters, the slope is 29.5 mm). The high side phase ( FIG. 8D ) has a slope of 50.9 mm at zero frequency. The y-axis intercepts of these straight lines should naturally be zero (and this can be constrained during the curve fit). The slope of this straight line is equal to the change in the alignment of the paper sheet at the CD positions of the low bump and the high bump, respectively.
[0075] h. Since it was assumed the change in alignment to be linear, the fact that at least two well-spaced bumps were employed allowed the two slopes to determine the two degrees of freedom assumed for the linear change in alignment. A straight line is drawn between the two measured points in FIG. 9 to model the change in alignment for the overall sheet as a function of the cross-directional position. Specifically, in FIG. 9 , the slopes of the zero frequency phases illustrated in FIG. 8 , i.e., 29.5 mm and 50.9 mm, were plotted against the CD position of the induced setpoint target bumps (δr) which are positioned approximately ¼ and ¾ of the way across the sheet as described above. It was assumed that the change in alignment was linear across the sheet width. The line in the graph is an alignment update computed from a linear fit between the two data points computed from the data obtained during the reversed bump test. A linear alignment shift is the most common experienced on actual papermaking machines. As is evident, other models of alignment can be accommodated and would simply involve a different distribution of the induced setpoint target bumps (δr).
[0076] If a more complicated nonlinear shrinkage pattern is assumed, then the above procedure could be modified to identify the nonlinear alignment change. This can be accomplished by designing more than two well-spaced bumps. This could potentially require the bumps to be staggered in time. For example, the bumps can be implemented sequentially. Finally, the change in cross-directional controller alignment as a function of cross-directional position on the sheet has been computed. e.g., as illustrated in FIG. 9 . This function can then be used to update the alignment of the online cross-directional controller. A CD control system will perform at its best when the controller alignment matches the true alignment of the paper sheet and the actuators.
[0077] The foregoing has described the principles, preferred embodiment and modes of operation of the present invention. However, the invention should not be construed as limited to the particular embodiments discussed. Instead, the above-described embodiments should be regarded as illustrative rather than restrictive, and it should be appreciated that variations may be made in those embodiments by workers skilled in the art without departing from the scope of present invention as defined by the following claims.
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A reverse bump test, for identifying the alignment of a sheetmaking system while the system remains in closed-loop control, includes the following steps: (a) leaving the control system in closed-loop, (b) artificially inserting a step signal on top of the measurement (or setpoint) profile from the scanner, (c) recording the data as the control system moves the actuators to remove the perceived disturbance (or setpoint change), and (d) refining or developing a model from the artificial measurement disturbance (or setpoint change) to the actuator profile. The technique supplies the probing/perturbation signal to the scanner measurement, which is equivalent to supplying the probing/perturbation signal to the setpoint target) rather than inserting bumps via the actuator set points as has been practiced traditionally.
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BACKGROUND OF THE INVENTION
The present invention relates to a synthesizer using a PLL (phase-locked loop) circuit, which is hereinafter called a PLL synthesizer. More specifically, the invention relates to a PLL synthesizer which can provide oscillation frequencies at small step intervals and which responds in a sufficiently short time.
FIG. 1 shows a well known PLL oscillation circuit. This PLL oscillation circuit has a voltage-controlled oscillator (VCO) 41 with an oscillation frequency that can be operated by a control voltage. It also has a frequency divider (DIV) 42 for dividing the frequency of a signal supplied from the voltage-controlled oscillator 41 at a dividing ratio set by an input set value. Finally, the circuit has a phase comparator (PC) 43 to perform a phase comparison between an output signal of the frequency divider 42 and a reference frequency signal. It also supplies the voltage-controlled oscillator 41 with a phase error signal as the control voltage. The phase comparator 43 has a filter which can interrupt pulse-like signal components occurring in every phase comparison.
In this PLL oscillation circuit, an oscillation frequency fo is given by fo=k×fr where k is the dividing ratio of the frequency divider 42 and fr is a frequency of the reference frequency signal. Since the dividing ratio k is a positive integer, this PLL oscillation circuit provides oscillation frequencies at a step interval of fr.
Oscillation frequencies with smaller step intervals can be obtained with this PLL oscillation circuit by reducing the reference frequency fr. However, if the reference frequency fr is reduced, the cutoff frequency of the filter of the phase comparator 43 can also be lowered. If the cutoff frequency of the filter of the phase comparator 43 is reduced, the time constant of the filter is increased, which elongates the response time until stabilization of the output. That is, this PLL oscillation circuit has a problem that if it is attempted to obtain oscillation frequencies with smaller step intervals, the response time until stabilization of the output in response to switching of the oscillation frequency becomes longer.
FIG. 2 shows a conventional PLL oscillation circuit that has solved the above problem. This PLL oscillation circuit has the following components. Reference numeral 51 denotes a voltage-controlled oscillator (VCO). A first frequency divider (DIV1) 52 divides an oscillation frequency fo of an output signal of the voltage-controlled oscillator 51 at a ratio of k (positive integer). A second frequency divider (DIV2) 53 further divides the frequency of an output signal of the first frequency divider 52. A phase comparator (PC) 54 compares the phase of the output signal of the first divider 52 with that of a reference frequency signal. A triangular wave oscillator (TRI OSC) 55 generates a triangular wave based on a frequency-divided signal as output from the second frequency divider 53. An adder (SUM) 56 adds the output signals of the phase comparator 54 and the triangular oscillator 55.
In this PLL oscillation circuit, the frequency of the signal input to the first frequency divider 52 is usually divided at a ratio of k or k+j (j is an integer other than 0). The frequency-divided signal is input to the phase comparator 54, where it is subjected to phase comparison with the reference frequency (fr) signal. On the other hand, the frequency-divided signal output from the first frequency divider 52 is input to the second frequency divider 53, where it is subjected to frequency division at a ratio s. The frequency-divided signal as output from the second frequency divider 53 is input to the triangular wave oscillator 55. Further, the second frequency divider 53 supplies a switching signal to the first frequency divider 52 at a predetermined timing to effect switching between the frequency division of k and that of k+j.
The triangular wave oscillator 55 generates a triangular wave with a period T based on the frequency-divided signal supplied from the second frequency divider 53. The output signal from the phase comparator 54 and the triangular wave from the triangular wave oscillator 55 are subjected to addition (or subtraction) in the adder 56. As a result, a varying signal, having the period T, is removed from the output signal of the phase comparator 54. An output signal from the adder 56 is supplied, as a frequency control signal, to the voltage-controlled oscillator 51.
In the case with frequency division of k+j where j=1 and the first frequency divider 52 performs m times of frequency division of k+1 and s-m times of frequency division of k. Then, the output frequency fo is expressed as ##EQU1## It is understood that oscillation frequencies can be obtained with the step interval fr/s. That is, it is possible to obtain oscillation frequencies with small step intervals without reducing the frequency fr of the reference frequency signal. This type of PLL oscillation circuit is, for example, disclosed in Japanese Unexamined Patent Publication No. Sho. 63-28131 (1988).
However, the above method for decreasing the step intervals of oscillation frequencies by using a triangular wave has the following problem. Since the frequency division number of the period T depends on the oscillation frequency, an error in the oscillation frequency of the triangular wave directly deteriorates the stability of the oscillation frequency of the voltage-controlled oscillator 51.
SUMMARY OF THE INVENTION
An object of the present invention is to provide, by solving the above-described problems, a PLL circuit which can stably oscillate to provide oscillation frequencies having small step intervals even with a high reference frequency.
To attain the above object, according to the invention, a PLL circuit comprises variable frequency oscillation means for outputting an oscillation frequency signal, pulse train generating means for generating a plurality of non-uniform pulse trains that vary periodically on a time series by using the oscillation frequency signal as a clock signal, phase comparing means for outputting a phase error signal by determining a phase error between an input reference frequency signal and the oscillation frequency signal based on the reference frequency signal and the plurality of sequential pulse trains, and filtering meads for filtering the phase error signal to produce a frequency control signal, and supplying the frequency control signal to the variable frequency oscillation means.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention will be described below in further detail with reference to the accompanying drawings, in which:
FIG. 1 is a block diagram showing an example of prior art PLL synthesizers;
FIG. 2 is a block diagram showing another example of prior art PLL synthesizers;
FIG. 3 is a block diagram showing a first embodiment of the present invention;
FIG. 4 shows a temporal variation of the clock number in the output of a flip-flop 12 of the first embodiment shown in FIG. 3;
FIG. 5 shows waveforms appearing at respective parts in the first embodiment,
FIG. 6 shows current waveforms appearing at respective positions in a synthesizing section 26 of the first embodiment;
FIG. 7 is a block diagram showing a second embodiment of the present invention; and
FIG. 8 is a block diagram showing a third embodiment of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A first embodiment of a PLL circuit according to the present invention will be described. FIG. 3 shows the first embodiment of the invention. A PLL oscillation circuit of FIG. 3 has a voltage-controlled oscillator (VCO) 11, a flip-flop (F/F) 12, an adder 13, a subtracter 14, a selector 15, numerical comparators 16 through 19, flip-flops (F/F's) 20 through 24, a gate section 25, a combining section 26, and a filtering section 27.
The operation of the PLL oscillation circuit of this embodiment will be described below with reference to FIGS. 3 through 6. In FIG. 3, each flip-flop 12, adder 13, subtracter 14, selector 15, and the numerical comparators 16 through 19 can deal with numerical values of, for instance, 13 bits (the maximum number of bits necessary to operate this embodiment). The adder 13 adds a predetermined value m (in this embodiment, m=4, which is equal to the number of the numerical comparators 16 through 19) to a numerical value output from the flip-flop 12, and outputs an additional result. The output m of the adder 13 is input to the subtracter 14 and the selector 15. The subtracter 14 subtracts a preset value n (n is a positive integer between 520 and 8188 in the configuration of FIG. 3) from the numerical value output of the adder 13, and supplies a subtraction result to the selector 15. The number 520 is the maximum of preset values 516, 515, 514 and 513 (described later) of the respective numerical comparators 16 through 19 plus m=4. The number 8188 is the maximum number 8192 expressed by 13 bits (the maximum number of bits that can be dealt with in this embodiment) minus m=4. The selector 15 is controlled by an output k of the subtracter 14 to select the output m of the adder 13 when the output of the subtracter 14 is negative, and selects the output ι of the subtracter 14 when the output of the subtracter 14 is zero or positive. The flip-flop 12 receives the numerical value as selected by the selector 15 with an output of the voltage-controlled oscillator 11 used as a clock signal, and outputs the received value at a timing of the next clock.
For example, if the initial output of the flip-flop 12 is 0 and the preset value n is 6001, the output m of the adder 13 increases to take, in order, the values 4, 8, . . . , 6000, 6004, . . . . On the other hand, the output 1 of the subtracter 14 increases to take, in order, the values -5997, -5993, . . . , -1, 3, . . . . The selector 15 selects the output m of the adder 13 when the output 1 of the subtracter 14 is negative. It selects the output 1 of the subtracter 14 when the output 1 of the subtracter 14 is zero or positive. Therefore, in this case, the output of the selector 15 takes, in order, the values 4, 8, . . . , 6000, 3, 7, . . . . That is, the output of the selector 15 is expressed as
X.sub.i =X.sub.i-1 +4 (mod n)
where X i is a current output value, X x-1 is an output value at a one-clock preceding timing and mod n is abbreviation of modulo-n. The flip-flop 12 outputs the output of the selector 15 at a prescribed timing as described in FIG. 4. With the above operation, the flip-flop 12 produces an output as shown in part (a) of FIG. 5.
The numerical value output from the flip-flop 12 is input to a plurality of (4 in this embodiment) numerical comparators 16 through 19. Four different detection thresholds (which increase or decrease in order one by one) are set in the respective numerical comparators 16 through 19. Each of the numerical comparators 16 through 19 outputs a high-level (H) signal when the numerical value received from the flip-flop 12 is equal to or larger than the detection threshold.
For example, assume here that the flip-flop 12 produces the output as shown in part (a) of FIG. 5 and detection thresholds of 516, 515, 514 and 513 are set in the respective numerical comparators 16 through 19. In this case, the numerical comparators 16 through 19 have output waveforms as shown in parts (b) to (e) of FIG. 5, respectively. As is apparent from these figures, the output waveform of each of the numerical comparators 16 through 19 is a non-uniform, sequential pulse train in which pulses having a repetition period of 1500 clocks and a pulse having a repetition period of 1501 clocks are periodically repeated. Further, the pulses having the period of 1501 clocks of the numerical comparators 16 through 19 appear at different timings.
Numerical comparators 16 through 19 are connected to the flip-flops 20 through 23, respectively, and the sequential pulse signals from the numerical comparators 16 through 19 render the flip-flops 20 through 23 in set states at their rise timings. On the other hand, receiving a reference frequency signal, the flip-flop 24 is rendered in a set state at its rise timings.
Each flip-flops 20 through 24 outputs a high-level (H) signal when it is in the set state. The outputs of the flip-flops 20 through 24 are input to the gate section 25. The gate section 25 outputs a reset signal when all of the outputs of the flip-flops 20 through 24 are at the high level. The flip-flops 20 through 24 are rendered in reset states by this reset signal.
Assume here that the PLL oscillation circuit of this embodiment is in a steady-state operation with an oscillation frequency that is, for instance, 1500.25 times the reference frequency fr. The number 1500.25 is equal to n/m when n=6001 and m=4. The reference frequency signal is shown in part (ref) of FIG. 5. In this case, the flip-flops 20 through 24 produce outputs as shown in part (f) to (j) of FIG. 5, respectively.
The outputs of the flip-flops 20 through 24 are also input to the combining section 26. The combining section 26 consists of resistors R 1 to R 5 and semiconductor switches S 1 to S 5 that are connected to the respective flip-flops 20 through 25 and are closed when the corresponding flip-flop is in a set state. The semiconductor switches S 1 to S 4 are connected to power supplies and the semiconductor switch S 5 is connected to ground. A current flowing through the semiconductor switches S 1 to S 4 and a current flowing through the semiconductor switch S 5 is in an opposite direction. The same resistance R of the resistors R 1 to R 4 and a resistance r of the resistor R 5 has a relationship R=4r. Therefore, the sum of the currents flowing through the resistors R 1 to R 5 becomes zero.
For example, at a timing t1 shown in FIG. 5, currents shown in parts (o) to (s) of FIG. 6 flow through the resistors R 1 to R 5 , respectively. The combining section 26 outputs the sum of the currents shown in parts (o) to (s) of FIG. 6 as a phase error signal. The phase error signal has a waveform shown in part (u) of FIG. 6. In this embodiment, when the PLL oscillation circuit is in the steady state, an electricity amount (a current value multiplied by its continuation time) flowing through all of the resistors R 1 to R 4 and that flowing through the resistor R 5 cancel out each other, so that an electricity amount of the phase error signal is zero. Similarly, at each of timings t2, t3 and t4, the electricity amount flowing through all of the resistors R 1 to R 4 and that flowing through the resistor R 5 cancel out each other, so that the phase error signal output from the combining section 26 has an electricity amount of zero. When the PLL oscillation circuit is not in the steady state, the electricity amount is a positive or negative value. The phase error signal obtained in the above manner does not have the components having non-uniform repetition periods of the sequential pulse trains that are the outputs of the flip-flops 20 through 23.
The phase error signal as output from the combining section 26 is input to the filtering section 27. Having an operational amplifier OP1, resistors R 6 and R 7 , and capacitors C 1 and C 2 , the filtering section 27 so set as to sufficiently smooth variation components of the phase error signal and to give a proper time constant to the PLL oscillation circuit. Since the phase error signal output from the combining section 26 does not include the components of the non-uniform repetition periods of the sequential pulse trains that are the outputs of the flip-flops 20 through 23, the time constant of this PLL oscillation circuit may be set so as to sufficiently suppress the component of the reference frequency fr, which is constant. There does not exist a problem that the time constant is so large that it takes long time for the oscillation frequency to become stable. As a result, a deviation of the oscillation frequency of the voltage-controlled oscillator 11 appears as phase shifts of the sequential pulse trains. A PLL loop is formed by negatively feeding back, to the voltage-controlled oscillator 11, the phase error signal obtained by comparing those pulse trains with the reference frequency signal.
The oscillation frequency fo of this PLL oscillation circuit is given by fo=n×(fr/m) where m is a positive integer representing the addition value of the adder 13, n is the setting value of the subtracter 14, and fr is the reference frequency. That is, the step interval of oscillation frequencies of this PLL oscillation circuit is fr/m. In this embodiment, in which m=4 and n=6001, fo is calculated as
fo=n×(fr/m)=6001×(20×10.sup.3 /4)=30.005 (MHz)
where fr is assumed to be 20 kHz. In this case, the step interval of oscillation frequencies is 20/4=5 kHz.
Although the step interval of oscillation frequencies is reduced to 5 kHz, it suffices that the time constant of the filtering section 27 is selected to be such a value as can suppress the component of the reference frequency fr. This enables formation of a synthesizer without elongating the response time. As a result, arbitrary oscillation frequencies can be obtained by changing the setting value n and the addition value m.
In the embodiment described above, the adder 13 adds 4 to the output of the flip-flop 12, and the setting value n is subtracted from the addition output. Alternatively, 4 may be subtracted from the output of the flip-flop 12 by a subtracter, the output of the subtracter being summed with the setting value n.
FIG. 7 shows a second embodiment of the present invention, which is the same as the first embodiment of FIG. 3 except that a subtracter 28 and an adder 29 are used instead of the adder 13 and the subtracter 14.
If it is assumed that the initial output of the flip-flop 12 is 6000, and the setting value n is 6001, the output of the subtracter 28 decreases to take, in order, the values 5996, 5992, . . . , 0, -4, -8 . . . . On the other hand, the output of the adder 29 decreases to take, in order, the values 11997, 11993, . . . , 6001, 5997, . . . . The selector 15 selects the output of the subtracter 28 if the output of the adder 29 is larger than, or equal to 6001 setting value n, and selects the output of the adder 29 if it is smaller than 6001. As a result, the output of the selector 15 takes, in order, the values 5996, 5992, . . . , 0, 5997, 5993, . . . . That is, the output of the selector 15 is expressed as
X.sub.i =X.sub.i-1 -4 (mod n)
where X i is a current output value and X i-1 is an output value at a one-clock preceding timing.
Although in the above-described embodiments the addition value m of the adder 13 is set at 4, the invention is not limited to this case.
For example, FIG. 8 shows a generalized configuration in which numerical comparators 30-1 through 30-m, flip-flops 31-1 through 31-m, switches 32-1 through 32-m, and resistors 33-1 through 33-m are provided by the same number as the addition value m. In this case, a relationship
R.sub.33-1 =R.sub.33-2 = . . . =R.sub.33-3 m=m×R.sub.5
is established in consideration of the current balance.
In the above embodiments, the thresholds of the numerical comparators 16 through 19 are set at 516, 515, 514 and 513, respectively, with the result that the output waveform of each numerical comparator has pulses having the repetition period of 1500 clocks and pulses having the repetition period of 1501 clocks. The above consecutive thresholds are selected to facilitate the detection of the phase error signal. However, the invention is not limited to this case, but other numbers smaller than the setting value n may be selected in which case the resistances R 1 to R 5 are selected so that the phase error signal detected by the combining section 26 does not include the components of non-uniform repetition periods.
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To provide stable oscillation frequencies at small step intervals even with a high reference frequency, a PLL circuit of the present invention includes variable frequency oscillation means for outputting an oscillation frequency signal, pulse train generating means receiving the oscillation frequency signal as a clock signal, for converting a train of n clocks to m pulses where n and m are positive integers, generating sequential pulses produced by arranging part of the m pulses so that they have non-uniform numbers of clocks, and outputting m periodical, sequential pulse trains so that the pulses having the non-uniform numbers of clocks are arranged differently, phase comparing means for outputting a phase error signal by determining a phase error between the reference frequency signal and the oscillation frequency signal based on the reference frequency signal and the m sequential pulse trains, and filtering means for filtering the phase error signal to produce a frequency control signal, and supplying the frequency control signal to the variable frequency oscillation means.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from German Patent Application No. 102 31 829.8, which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The invention relates to a device on a spinning preparatory machine, especially a carding machine, cleaning machine or the like for cotton having at least one separating blade for impurities, which is associated with a clothed roller, for example a licker-in or the like.
[0003] In a known arrangement the separating blade is arranged on a support which is displaceable parallel to (concentrically with) the periphery of the roller and wherein the distance between the separating blade and a fixed-position counter-element bordering the separation opening is variable.
[0004] In the known device of European Patent Specification No. 0 618 318, the impurities separated by the separating blade fall downwards into the space below the roller and have to be removed from there. Removal is complicated and can result in the machine becoming blocked. A further disadvantage is that the impurities fall diffusely and therefore the entire lower machine space has to be cleaned. As a result, the impurities and the air currents are swirled about.
SUMMARY OF THE INVENTION
[0005] It is an aim of the invention to provide a device of the kind mentioned at the beginning which avoids or mitigates the mentioned disadvantages and which allows uniform removal of impurities and uniform supplying of air into the extraction chamber, especially when the position of the separating blade is varied.
[0006] The invention provides a device on a spinning preparatory machine having at least one separating blade which is associated with a roller and co-operates with a fixed position counter element to define a separation opening for impurities, wherein the separating blade is arranged on a support which is displaceable substantially parallel to the periphery of the roller for adjusting the distance between the separating blade and the fixed-position counter-element, the device further comprises an extraction chamber which is mounted on the support, and the extraction chamber co-operates with a guide element, the guide element being arranged to be in a fixed position during operation of the machine and being able to guide separated impurities and/or air into the opening of the extraction chamber.
[0007] The movable extraction hood cooperates with a fixed-position guide element and, as a result, the separated impurities and/or the intake air can be guided uniformly into the extraction hood. In this way, when the positions of the blade and the extraction hood are changed, advantageously a substantially constant amount of air is sucked into the extraction hood and the impurities (waste) are prevented from falling past the extraction hood. The provision of constant amounts of air and constant flow speeds for supplying the extraction hood with air is in particular possible where, as is preferred, the fixed-position guide element cooperates with the movable extraction hood in the manner of a nested arrangement.
[0008] Advantageously, the distance between the guide element and a fixed position counter-element is substantially constant. Advantageously, the distance between the guide element and the fixed position counter-element has a free end, which may decrease in thickness. Advantageously, the free end is oriented in the direction of the intake opening (intake slot). The guide element may have at least one rounded edge over its width. The guide sheet may have a free end. The guide sheet may have a curved guide surface. Advantageously, the distance of the guide element from the roller is less than the distance of the guide sheet. Advantageously, the guide element co-operates with the guide sheet. The guide sheet may be arranged substantially underneath the guide element with respect to the roller. The guide sheet may be displaced with respect to the fixed-position guide element. Advantageously, the displacement is effected in a parallel direction. Advantageously, the radii of curvature of the rear side surface of the guide element and of the guide surface of the guide sheet are the same. The guide element and the guide sheet are advantageously nested with one another. The extraction chamber may be mounted separately on the support. The extraction chamber may be mounted releasably on the support. Advantageously, the width of the intake opening is approximately 15 to 25 mm. Advantageously, the end face of the extraction chamber is adjoined by an extraction line, which may be connected to at least one suction source. Advantageously, the position of the support can be adjusted by means of an adjusting device. The adjusting device may be manually operable. The adjusting device may be motor-operable. The support may be associated with a mechanical adjusting device, for example, a rack having a curved tooth bar which co-operate with a pinion. The adjusting device may have a driven reversing gear. Advantageously, the fixed position guide element is associated with an adjusting and fixing device. Advantageously, there is a continuous opening between the guide element of air. Advantageously, supplied air can be taken in through the opening. Advantageously, the supplied air assists the transport of impurities.
[0009] The invention also provides a device on a carding machine, cleaning machine or the like for cotton having at least one separating blade for impurities, which is associated with a clothed roller, for example a licker-in or the like, wherein the separating blade is arranged on a support which is displaceable parallel to (concentrically with) the periphery of the roller and wherein the distance between the separating blade and a fixed-position counter-element bordering the separation opening is variable, in which the separating blade is associated with an extraction chamber which is mounted on the support, and the extraction chamber co-operates with a fixed-position guide element which is able to guide the separated impurities and/or air into the opening of the extraction chamber.
[0010] Furthermore, the invention provides a method of removing impurities from textile fibre material at a roller, comprising withdrawing the impurities from the vicinity of the roller through a separation opening having a separation blade, adjusting the position of the separation blade to adjust the size of the separation opening and guiding the impurities into an extraction chamber by means of a guide element.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] [0011]FIG. 1 is a diagrammatic side view of a carding machine having a device according to the invention;
[0012] [0012]FIG. 2 is a diagrammatic side view of a cleaner having a device according to the invention; and
[0013] [0013]FIGS. 3 a , 3 b show the device according to the invention in positions with a narrow cleaning gap (FIG. 3 a ) and with a wide cleaning gap (FIG. 3 c ).
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0014] With reference to FIG. 1, a carding machine, for example a high performance carding machine DK 903 (trade mark) made by Trützschler GmbH & Co. KG, having a feed roller 1 , feed table 2, lickers-in 3 a , 3 b , 3 c , cylinder 4 , doffer 5 , stripper roller 6 , nip rollers 7 , 8 , web guide element 9 , sliver funnel 10 , delivery rollers 11 , 12 , revolving card top 13 with clothed card top bars 14 , can 15 and coiler 16 . The directions of rotation of the rollers are indicated by curved arrows. Reference letter A denotes the operating direction. The lickers-in 3 a , 3 b and 3 c are each associated with a separating blade 17 a , 17 b and 17 c , respectively, having extraction hoods 18 a , 18 b , 18 c . In the region of the extraction chambers 18 a , 18 b , 18 c there are arranged as described below with reference to FIGS. 3 a , 3 b , guide elements 19 a , 19 b and 19 c , respectively. The separating blades 17 a , 17 b and 17 c and the extraction hoods 18 a , 18 b and 18 c are each arranged on a respective displaceable support 20 a , 20 b and 20 c , (see FIGS. 3 a , 3 b showing blade 17 a and hood 18 a arranged on support 20 a ).
[0015] Referring to FIG. 2, a cleaning device, which is arranged in a closed housing, is supplied with the fibre material to be cleaned (arrow H), which is especially cotton, in flock form. This is effected, for example, by a filling chute (not shown), by a conveyor belt or the like. The lap is supplied by means of two feed rollers 32 , 33 under the clamping action of a pinned roller 23 , having pins 23 a , which is rotatably mounted in the housing and rotates anticlockwise. Downstream of the pinned roller 23 there is arranged a clothed roller 24 which is covered with sawtooth clothing 24 a . The roller 23 has a circumferential speed of about from 10 to 21 m/sec. The roller 24 has a circumferential speed of about from 15 to 25 m/sec. The direction of rotation of each of rollers 23 , 24 is indicated by arrows I, II, respectively. Downstream of the rollers 23 and 24 there are arranged one after the other two further sawtooth rollers 25 and 26 , the directions of rotation of which are indicated by III and IV, respectively. The rollers 25 , 26 , have sawtooth surfaces 25 a , 26 a . The rollers 23 to 26 have a diameter of about from 150 to 300 mm. The pinned roller 23 is enclosed by the housing. The pinned roller 23 is associated with a separation opening 27 for discharging fibre impurities, the size of which is matched or is matchable to the degree of contamination of the cotton. The separation opening 27 is associated with a separating edge 17 a , for example a blade. In the direction of arrow I there are present at the roller 23 a further separation opening 28 and a separating edge 17 b . The sawtooth roller 24 is associated with a separation opening 29 and a separating edge 17 c ; the sawtooth roller 25 is associated with a separation opening 30 and a separating edge 17 d ; and the sawtooth roller 26 is associated with a separation opening 31 and a separating edge 17 e . Each separating blade 17 a to 17 e is associated with an extraction hood 18 a to 18 e . Reference letter B denotes the operating direction of the cleaner. Each extraction hood 18 a to 18 e is associated with a guide element 19 a to 19 e . Reference letter I denotes the air current containing impurities F, which enters the extraction hood 18 b . Reference numeral 28 A denotes a portion of the housing. Downstream of roller 26 is a conduit 22 for taking away fibre material ejected from roller 26 .
[0016] With reference to FIGS. 3 a , 3 b , the licker-in 3 a of the carding machine of FIG. 1 is associated with the separating blade 17 a for impurities F, which blade is arranged on a support 20 a . The edge 17 ′ of the separating blade 17 a is opposed to the direction of rotation 3 ′ of the licker-in 3 a . The support 20 a , for example an extruded aluminium profile, is displaceable in the direction of arrows C and D parallel to the outer surface of the licker-in 3 a , i.e. concentric with the centre point M of the licker-in 3 a . Reference numeral 21 denotes the separation opening which is located between the separating blade 17 a and the feed roller 1 . The feed roller 1 is in a fixed position in that, at least during operation, the roller axis is in a fixed position. Because the support 20 a is displaceable in directions C, D, the distance between the separating blade 17 a and the slow-speed feed roller 1 bordering the separation opening 21 can be varied. The separating blade 17 a is mounted on the support 20 a by means of a screw connection 34 or the like so as to be displaceable in the direction of the licker-in 3 a . The separating blade 17 a is associated with the extraction hood 18 a , which is mounted in a pivot bearing 35 on the support 20 a . Reference numeral 18 ′ denotes the inlet opening into the extraction hood 18 a , which opening extends in slot-like manner across the width of the machine or the extraction hood 18 a . On the extraction hood 18 a there is mounted opposite the support 20 a -in the region of the intake slot 18 ′ a guiding member 18 ″ in the form of a guide sheet 18 ″. The free end of the guide sheet is directed towards the intake slot 18 ′. The guiding element 18 ″, which together with the extraction hood 18 a forms an integrally extruded component, has a slightly curved shape. The extraction chamber 18 a is associated with a guide element 19 a , which is in a fixed position during operation, and is located in the region underneath the separation opening 21 . The guide element 19 a is somewhat angular in shape and has a slightly curved arm 19 ′, the free end of which points towards the intake opening 18 ′. The other end of the arm 19 ′ is rounded and merges into a holding and securing element 19 ″ for the guide element 19 a . The distance a between the rounded portion and the feed roller 1 , which denotes an air-inlet opening 38 for an air current E, is constant during operation. The guiding member 18 ″ is arranged on the side of the arm 19 ′ remote from the licker-in 3 a . The displacement of the support 20 a is effected by a rack 36 with a pinion 37 . Whilst it is in a fixed position during operation, the position of the guide element 19 a and thus the distance a can be adjusted by means of an adjusting device (not shown) when the carding machine is not operating.
[0017] When the support 20 a is displaced in the direction of arrow C, the separating blade 17 a and the extraction hood 18 a are displaced from the position according to FIG. 3 a into the position according to FIG. 3 b . At the same time, the guiding member 18 ″ is also displaced in direction C. As a result of the displacement of the separating blade 17 a , the separation opening 21 is enlarged so that more impurities F are separated from the fibre material. The guiding member 18 ″ is displaced concentrically with respect to the arm 19 ′. The width of the air-inlet opening 38 and of the intake slot 18 remain constant even when the support 20 a is displaced, so that when the separation opening 21 is altered the size of the incoming air current E and the size of the extracted air current G remain the same. A further advantage is that for any size of the separation opening 21 the separated impurities F always fall onto the arm 19 ′ and/or onto the guiding member 18 ′ and are reliably guided through the extraction slot 18 ′ into the extraction chamber 18 a.
[0018] The fixed-position guide element 19 a cooperates with the guiding element 18 ′ on the lines of a nested arrangement. The guiding member 18 ″ may cooperate in sliding fashion with arm 19 ′ of guide element 19 a . Displacement of the support 20 a in the direction of arrows C and D results in a narrow cleaning gap (FIG. 3 a ) and a wide cleaning gap (FIG. 3 b ), respectively.
[0019] In FIGS. 3 a , 3 b the invention has been described using the example of a device underneath a high-speed roller, e.g. licker-in 3 a . The device according to the invention can be arranged in accordance with FIG. 2 also above or below a high-speed roller of a cleaner, e.g. the rollers 24 and 26 . The extraction hoods 18 b , 18 c of FIG. 1 may be of similar construction to that described in FIGS. 3 a , 3 b , with reference to extraction hood 19 a of FIG. 1. In that case, however, the guide elements 19 b , 19 c , will cooperate with a counter-surface other than feed roller 1 .
[0020] Reference letter K denotes an air current which according to FIG. 2 detaches fibre flocks from the last roller 26 of the cleaner, the fibre flocks being extracted in accordance with arrow L.
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In a device on a spinning preparatory machines, especially a carding machine, cleaning machine or the like for cotton having at least one separating blade for impurities, which is associated with a clothed roller, for example a licker-in or the like, wherein the separating blade is arranged on a support which is displaceable parallel to (concentrically with) the periphery of the roller, the distance between the separating blade and a fixed-position counter-element bordering the separation opening is variable.
In the event of a change in the position of the separating blade, in order to provide uniform removal of impurities and uniform supply of air into an extraction chamber, the separating blade is associated with an extraction chamber which is mounted on the support, and the extraction chamber cooperates with a fixed-position guide element which is able to guide the separated impurities and/or air into the opening of the extraction chamber.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a division of U.S. patent application Ser. No. 11/430,179, filed on May 9, 2006, now U.S. Pat. No. 7,597,853, the entire contents of which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention generally relates to diagnostic test strips for testing biological fluids. More specifically, the present invention relates to an apparatus and method for storing and dispensing diagnostic test strips.
2. Background of the Invention
Diagnostic test strips are used to measure analyte concentrations in biological fluids. For example, diagnostic test strips are often used by diabetic patients to monitor blood glucose levels.
To preserve their integrity, diagnostic test strips must be maintained in appropriate environmental conditions. That is, the test strips should be maintained at appropriate humidity levels, and should remain free of foreign substances. Furthermore, to avoid contamination by skin oils or foreign substances, test strips should not be handled prior to use.
Thus, to preserve test strips, they are typically maintained in a storage vial or the like. In order to use a test strip, a user must reach into the vial, and retrieve a single test strip. However, many users, such as diabetic patients, have impaired vision or physical dexterity. Such users may find it difficult to retrieve a single test strip from a storage vial. Further, users may accidentally touch multiple test strips while reaching into the storage vial to withdraw a test strip, and potentially contaminate the unused test strips.
Accordingly, there is a need for an apparatus for storing diagnostic test strips in appropriate environmental conditions, and for conveniently dispensing the test strips one at a time.
SUMMARY OF THE INVENTION
An object of the present invention is to address at least the above problems and/or disadvantages and to provide at least the advantages described below. Accordingly, an object of the present invention is to provide an apparatus for storing a plurality of test strips and dispensing the test strips one at a time.
According to one embodiment of the present invention, the above and other objects are achieved by an apparatus for storing and dispensing a test strip which comprises a container including an outer wall and a plurality of radially extending slots formed by a plurality of dividing walls. Each slot is sized to receive a single test strip, and a rotatably positionable cover is carried by the container for covering the plurality of radially extending slots. The cover includes an opening so that when the cover rotates, the cover opening aligns with one of the slots at a time to allow removal of a single test strip located within the respective slot.
According to another embodiment of the present invention, an apparatus for storing and dispensing a test strip comprises a vial with a plurality of radially extending slots, each slot adapted to store a test strip, means for exposing one of the plurality of radially extending slots to dispense a test strip stored in the exposed slot, and means for actuating the exposing means.
According to still another embodiment of the present invention, a method for storing and dispensing test strips comprises the steps of storing a plurality of test strips in a radially arranged manner in a container, and covering the plurality of test strips in such a manner as to allow only one test strip at a time to be dispensed from the container.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other objects, features, and advantages of certain exemplary embodiments of the present invention will be more apparent from the following description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a perspective view of a storage vial for storing and dispensing test strips, according to a first exemplary embodiment of the present invention;
FIG. 2 is a top view of the container of the storage vial of FIG. 1 , with the lid and rotatable cover both removed to expose the radial slots within the vial;
FIG. 3 is a top view of the container of FIG. 1 , with only the lid removed to expose the rotatable cover;
FIG. 4 is a bottom perspective view of the rotatable cover of the storage vial of FIG. 1 ;
FIG. 5 is an exploded perspective view of a storage vial for storing and dispensing test strips, according to a second exemplary embodiment of the present invention;
FIG. 6 is a perspective view of the spinner of the storage vial of FIG. 5 ;
FIG. 7 is a cut-away perspective view of the sleeve of the storage vial of FIG. 5 ;
FIG. 8 is a perspective view of the cam sleeve and the spinner of the storage vial of FIG. 5 ;
FIG. 9 is a top view showing the interaction between the cam sleeve and the spinner of the storage vial of FIG. 5 ;
FIG. 10 is an enlarged view of the circled area in FIG. 9 ;
FIG. 11 is another top view showing the interaction between the cam sleeve and the spinner of the storage vial of FIG. 5 ;
FIG. 12 is an enlarged view of the circled area in FIG. 11 ; and
FIGS. 13-16 are diagrams showing the operation of the storage vial of FIG. 5 .
Throughout the drawings, the same reference numerals will be understood to refer to the same elements, features, and structures.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
The matters defined in the description such as a detailed construction and elements are provided to assist in a comprehensive understanding of the embodiments of the invention. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope and spirit of the invention. Also, descriptions of well-known functions and constructions are omitted for clarity and conciseness.
First Exemplary Embodiment
Referring to FIGS. 1-4 , a storage vial 100 for storing and dispensing test strips according to a first exemplary embodiment of the present invention includes a container 102 with a plurality of radial slots 104 formed by a plurality of dividing walls 106 . Each slot 104 is sized to receive one test strip 108 . A rotatable cover 110 is positioned on top of the slots 104 to at least partially cover the plurality of slots 104 and prevent test strips received within the slots 104 from being removed from the slots 104 . The rotatable cover 110 has a cover opening 112 which is sized to allow one test strip 108 to pass through the cover opening 112 . The cover 110 may be rotated to align the cover opening 112 with one of the plurality of slots 104 to allow a test strip 108 located within the slot 104 to be dispensed.
As seen in FIG. 1 , the container 102 may be provided with a lid 114 to prevent humidity and other environmental contaminants from entering the container 102 . The lid 114 may be a separate detachable component, but preferably the lid 114 is connected to the container 102 by a hinge 116 . In the illustrated embodiment, the lid 114 is formed integrally with the container 102 so that it is connected to the container 102 by a living hinge 116 . The lid 114 preferably forms a substantially hermetic seal with the container 102 . Such seals are known to those skilled in the art, and therefore, a detailed description of the seal will be omitted for conciseness. The lid 114 has an extended portion 118 which serves as a handle for a user to conveniently open the lid 114 . For convenience of explanation, the lid 114 is only shown in FIG. 1 .
FIG. 2 is a top view of the container 102 after the lid 114 has been opened, with the rotatable cover 110 removed. The container 102 has a plurality of dividing walls 106 which form a plurality of slots 104 . Each slot 104 is sized to receive one test strip. A boss 120 is located at the center of the container 102 . The boss 120 has a recess 122 . The recess 122 has an undercut portion (not illustrated) to cooperate with an elongated shaft 124 located on the rotatable cover 110 , as will be described in further detail below.
Each of the dividing walls 106 extends radially inwardly from the outer wall 126 of the container 102 . In an exemplary embodiment, the dividing walls 106 extend inwardly for approximately one-half (½) the width of a test strip. This allows a larger number of strips to be contained within the container 102 because each test strip does not need to be enclosed on all sides. It also allows each of the dividing walls 106 to have a substantially even wall thickness, thereby improving moldability. In the illustrated embodiment, the dividing walls 106 are formed integrally with the container 102 . The dividing walls may, however, be formed separately as a sleeve to be inserted into the container 102 , as will be described in further detail in connection with the second exemplary embodiment.
The dividing walls 106 may be formed of a desiccant entrained polymer to regulate the specific relative humidity within the container 102 (to prevent damage to humidity-sensitive test strips). U.S. Pat. No. 5,911,937, which is hereby incorporated by reference in its entirety, discloses one suitable desiccant entrained polymer. Forming the dividing walls 106 of a desiccant entrained polymer increases the exposed surface area of the desiccant entrained polymer, thereby improving humidity regulation within the container 102 . Alternatively, the container 102 may be formed of a polymer with an insert-molded desiccant, or a desiccant may be placed in the bottom of the container 102 , in the lid 114 of the container 102 , or in one or more of the slots 104 .
FIG. 3 is a top view of the container 102 after the lid 114 has been opened, with the rotatable cover 110 shown in place. The cover 110 has a cover opening 112 which is sized to allow one test strip 108 to pass through the cover opening 112 . The cover 110 has a handle to allow a user to grasp the cover 110 to rotate the cover 110 . The outer diameter of the cover 110 is smaller than the inner diameter of the outer wall 126 of the container 102 . This provides a gap between the outer wall 126 and the cover 110 so that a user may peer into the slots 104 in the container 102 and visually determine how many test strips are remaining in the container 102 , and the placement of those test strips.
FIG. 4 is a bottom perspective view of the rotatable cover 110 . The cover 110 has an upper surface 130 and a lower surface 132 . The lower surface 132 of the cover 110 has an elongated shaft 124 . The elongated shaft 124 is configured so that it is positionable within the recess 122 located in the boss 120 in the container 102 . Preferably, the elongated shaft 124 has an undercut portion 134 which cooperates with a mating portion (not illustrated) in the recess 122 of the boss 120 . In this way, the elongated shaft 124 can be snap-fit into the boss 120 .
The lower surface 132 of the cover 110 has detents 136 that engage the dividing walls 106 to control the rotation of the cover 110 . In the illustrated embodiment, the detents 136 are formed by a plurality of extended protrusions. Preferably, the detents 136 are sized and positioned so that they align the cover opening 112 with one of the slots 104 . The detents 136 also provide tactile feedback to a user indicating when the cover 110 has been rotated to the next slot 104 .
The method of using the storage vial 100 for storing and dispensing test strips according to the first exemplary embodiment of the invention will now be described. Initially, test strips are loaded into the radially extending slots 104 formed in the container 102 so that one test strip is located in each slot 104 . The rotatable cover 110 is then assembled to the container 102 by placing the elongated shaft 124 into the recess 122 in the boss 120 . The elongated shaft 124 is retained in the recess by a snap-fit or the like. The lid 114 is then placed on the container 102 to form a substantially hermetic seal. The storage vial 100 may now be stored, and the test strips will be protected from environmental hazards, such as moisture. Typically, the foregoing steps will be performed by a manufacturer, rather than an end user of the storage vial 100 .
To dispense a test strip, a user opens the lid 114 to expose the rotatable cover 110 and the cover opening 112 . The user rotates the cover 110 by manipulating the cover handle 128 , with the user's fingers or the like, so that the cover opening 112 is aligned with one of the slots 104 . The detents located on the cover 110 provide assistance in aligning the cover opening 112 with one of the slots 104 . When the cover opening 112 is aligned with a desired slot 104 , a user then inverts the container 102 . A test strip located within the slot 104 is dispensed through the cover opening 112 with the aid of gravity. The user may then grasp the dispensed test strip to withdraw the test strip from the container 102 and use the test strip. To dispense another test strip, the user rotates the cover 110 again to the next slot with an unused test strip. After dispensing the desired number of test strips, the user may then replace the lid 114 on the container 102 to store the remaining test strips for future use.
After all of the test strips stored in the container 102 have been dispensed, the storage vial 100 may be discarded, or may be returned to the manufacturer for recycling. Reusable embodiments of the container 102 are also within the scope of the present invention.
Second Exemplary Embodiment
Referring to FIGS. 5-16 , a storage vial 200 for storing and dispensing test strips according to a second exemplary embodiment of the present invention includes a container 200 with a plurality of radial slots 204 formed by a plurality of dividing walls 206 . Each slot 204 is sized to receive one test strip 208 . A rotatable spinner 210 forms a cover which is positioned on top of the slots 204 to at least partially cover the plurality of slots 204 and prevent test strips received within the slots 204 from being removed from the slots 204 . The spinner 210 has a cover opening 212 which is sized to allow one test strip to pass through the cover opening 212 . The spinner 210 is rotated by a pushbutton 214 . Each time the pushbutton 214 is pressed, the spinner 210 rotates so that the cover opening 212 is aligned with a new radial slot 204 . Once the spinner 210 is aligned with a slot 204 containing a test strip, a user may invert the container 200 to dispense the test strip.
Referring to FIG. 5 , the storage vial 200 includes a container 200 , a sleeve 216 , a biasing element 218 , a spinner 210 , and a cam sleeve 220 .
The container 200 is preferably formed of a substantially vapor impermeable material. The container 200 has a lid (not shown) which is substantially similar to the lid described with respect to the first embodiment.
Referring to FIG. 7 , the sleeve 216 has a plurality of dividing walls 206 which form a plurality of slots 204 . Each slot 204 is sized to receive one test strip. A boss 222 is located at the center of the sleeve 216 . The boss 222 has a recess 224 . The recess 224 receives an elongated shaft 226 located on the spinner 210 , as will be described in further detail below.
Each of the dividing walls 206 extends radially inwardly from the outer wall 228 of the sleeve 216 . In an exemplary embodiment, the dividing walls 206 extend inwardly for approximately two-thirds (⅔) the width of a test strip, for the reasons discussed above with respect to the first embodiment. A plurality of guiding ribs 230 may be formed on the outer surface of the boss 222 . The guiding ribs 230 help align test strips in the slots 204 to prevent the test strips from becoming misaligned. The outer diameter of the sleeve 216 is sized so that it fits snugly within the container 200 .
Preferably, the sleeve 216 is formed of a desiccant entrained polymer to regulate the specific relative humidity within the container 200 . As discussed above, forming the dividing walls 206 of a desiccant entrained polymer increases the exposed surface area of the desiccant entrained polymer, thereby improving humidity regulation within the container 200 . Alternatively, the sleeve 216 is formed of a standard polymer and a desiccant is placed within the container 200 .
The biasing element 218 is located between the spinner 210 and the sleeve 216 . The biasing element 218 may be, for example, a coil spring which fits around the elongated shaft 226 of the spinner 210 . The biasing element 218 applies a biasing force to press the spinner 210 in an upward direction (with reference to FIG. 5 ).
As seen most clearly in FIG. 6 , the spinner 210 has an upper surface 232 and a lower surface 234 , and a cover opening 212 which extends through the spinner 210 . The cover opening 212 is sized to allow one test strip to pass through the cover opening 212 . A plurality of first cams 236 are located around the outer periphery of the spinner 210 . The first cams 236 have first, angled cam surfaces 238 .
The spinner 210 has at least one flexing beam 240 located on the upper surface 232 of the spinner 210 . In the illustrated embodiment, four flexing beams 240 are provided. A pushbutton 214 is also provided on the upper surface 232 of the spinner 210 .
A portion 264 of the spinner 210 may be formed of an optically transparent material so that a user may determine how many test strips are in the storage vial 200 . The optically transparent portion 264 of the spinner 210 may be configured so that it magnifies the image being viewed, thus magnifying the edge of a strip.
An elongated shaft 226 is located on the lower surface 234 of the spinner 210 . The elongated shaft 226 preferably has a first portion 242 with a first, smaller diameter, and a second portion 244 with a larger diameter. The transition area between the first and second portions 242 , 244 forms a stop 246 . The first portion 242 of the elongated shaft 226 is sized to fit within the recess 224 in the boss 222 . The stop 246 prevents the spinner 210 from being pressed too far downward, as will be discussed in detail further below.
Referring to FIG. 8 , the cam sleeve 220 is a generally circular ring 248 which is sized to fit into the interior of the container 200 . On its interior surface, the cam sleeve 220 has a plurality of cam teeth 250 , and a plurality of second cams 252 . The second cams 252 have second, angled cam surfaces 254 which cooperate with the first, angled cam surfaces 238 , as will be discussed in detail below.
The spinner 210 and the cam sleeve 220 may be formed of a polymer or any other suitable material. They may also be formed of a desiccant entrained polymer, so long as the addition of the desiccant does not reduce the mechanical characteristics of the polymer enough to result in premature failure.
The method of using the storage vial 200 for storing and dispensing test strips according to the second exemplary embodiment of the invention will now be described. Initially, test strips are loaded into the radially extending slots 204 formed in the sleeve 216 so that one test strip is located in each slot 204 . The sleeve 216 is then placed in the container 200 . The biasing element 218 is placed around the elongated shaft 226 of the spinner 210 , and the elongated shaft 226 is inserted into the boss 222 in the sleeve 216 . The cam sleeve 220 is then placed into the container 200 . Rotational alignment between the cam sleeve 220 and the slots 204 can be maintained during assembly by using keyways, visual alignment or other conventional methods. The teeth on the cam sleeve 220 overhang the spinner 210 , so that the cam sleeve 220 retains all of the components within the container 200 . The cam sleeve 220 , in turn, is retained in the container 200 by an undercut in the container 200 , or by affixing the cam sleeve 220 to the container 200 with adhesives, ultrasonic welding, or other conventional fixation methods. A replaceable lid (not shown but similar to the lid 114 of the previous embodiment) is then placed on the container 200 to form a substantially hermetic seal. The storage vial 200 may now be stored, and test strips will be protected from environmental hazards, such as moisture. Typically, these steps will be performed by a manufacturer, rather than an end user of the storage vial 200 .
To dispense a test strip, a user opens the lid and pushes the pushbutton 214 to rotate the spinner 210 to the next slot 204 . FIGS. 9-16 illustrate the operation of the spinner 210 in detail. Initially, as seen in FIG. 13 , before a user presses the pushbutton 214 , the first cams 236 on the spinner 210 are disposed above the second cams 252 on the cam sleeve 220 due to the biasing force of the biasing element 218 . And, as seen in FIGS. 9 , 10 , and 13 , the flexing beams 240 are seated within the cam teeth 250 . The flexing beams 240 prevent the spinner 210 from freely rotating, and align the cover opening 212 with one of the plurality of slots 204 .
When a user begins to press the pushbutton 214 on the spinner 210 and overcomes the biasing force of the biasing element 218 , the spinner 210 is pressed lower into the container 200 . Thus, as seen in FIG. 14 , the first cam surfaces 238 begin to engage the second cam surfaces 254 . Since the second cam surfaces 254 are fixed with respect to the container 200 , the contact between the first cam surfaces 238 and the second cam surfaces 254 causes the first cam surfaces 238 to move towards the right (with reference to the illustrations), thereby causing the spinner 210 to begin to rotate in a forward direction. At this time, the flexing beams 240 also begin to flex to pass by the cam teeth 250 located on the cam sleeve 220 . If the pushbutton is released at this point, the interaction of the flexing beams 240 with the cam teeth 250 will restore the spinner 210 to the original position shown in FIG. 13 . This is because the surfaces 256 of the flexing beams 240 that contact the cam teeth 250 are rounded and have an ascending portion 258 , a top 260 , and a descending portion 262 . At this initial stage, the cam teeth 250 have not passed the tops 260 of the rounded surfaces 256 , and the ascending portions 258 of the rounded surfaces 256 of the flexing beams 240 engages the cam teeth 250 and generate a force in a reverse direction (i.e., a leftward direction).
If a user continues to press the pushbutton, however, the spinner 210 continues to rotate, and the tops 260 of the rounded surfaces 256 of the flexing beams 240 pass by the cam teeth 250 , as illustrated in FIGS. 11 , 12 , and 15 . At this position, the descending portions 262 of the rounded surfaces 256 of the flexing beams 240 generate a force in a forward direction (i.e. a rightward direction). Thus, as shown in FIG. 15 , the first cams 236 contact the second cams 252 , so that the rotation of the spinner 210 is restricted. At this point, the stop 246 on the spinner 210 engages the boss 222 to prevent the spinner 210 from being pressed further into the housing.
Finally, when the user releases the pushbutton 214 , the biasing element 218 urges the spinner 210 upward. The first cams 236 are disengaged from the second cams 254 , and the descending portions 262 of the rounded surfaces 256 of the flexing beams 240 interact with the cam teeth 250 to generate a force which rotates the spinner 210 in a forward direction so that the cover opening 212 is aligned with the next slot 204 , as shown in FIG. 16 . Thus, the flexing beams 240 ensure that the spinner 210 is completely rotated to the next slot 204 so that the cover opening 212 is aligned with the next slot 204 .
After the cover opening 212 is aligned with a slot 204 containing a test strip, the user inverts the container 202 . A test strip located within the slot 204 is dispensed through the cover opening 212 with the aid of gravity. The user may then grasp the exposed test strip to withdraw the test strip from the container 200 and use the test strip. To dispense another test strip, the user rotates the cover 210 again by pressing the pushbutton 214 on the spinner 210 . After dispensing the desired number of test strips, the user may then replace the lid on the container 200 to store the remaining test strips for future use.
After all of the stored test strips stored in the container 202 have been dispensed, the storage vial 200 may be discarded, or may be returned to the manufacturer for recycling. Reusable embodiments of the container 102 are also within the scope of the present invention.
While various embodiments have been chosen to illustrate the invention, it will be understood by those skilled in the art that various changes and modifications can be made therein without departing from the scope of the invention as defined in the appended claims.
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An apparatus for storing and dispensing a test strip includes a container configured to store a radial array of test strips. The container maintains appropriate environmental conditions, such as humidity, for storing the test strips. The container has a plurality of radially extending slots formed by a plurality of dividing walls, and each slot is sized to receive a single test strip. A rotatably positionable cover is carried by the container for covering the plurality of radially extending slots. The cover includes an opening, which, when the cover rotates, aligns with one of the slots at a time to allow removal of a single test strip located within the respective slot. Accordingly, the unused test strips remain free of contaminants such as naturally occurring skin oils on a user's hand.
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FIELD OF THE INVENTION
The invention relates to an occupant protection device for a driver's side of a motor vehicle.
BACKGROUND OF THE INVENTION
DE 195 01 859 A1 discloses a protection arrangement for a motor vehicle, in which a support element which is detached from a splashboard is rigidly connected to elements of the vehicle body whose position is virtually unchanged even in the event of an accident. The steering spindle of the motor vehicle is likewise connected to the support element, via a bearing. The steering spindle is furthermore mounted on a steering framework, the mounting being designed to be flexible in a specifically predetermined way. As a result, in the event of a crash, the steering spindle is pivoted downwards, so that an airbag installed in the steering wheel is brought into an improved position with respect to an occupant.
The steering spindle is designed to be telescoping and is designed with an integrated force limiter. Furthermore, in the event of a crash a foot pedal is moved away from the occupant by means of an actuating rod.
The disadvantage of this arrangement is the fact that in the event of a crash the force which is necessary for displacement of the steering spindle and which is introduced by the occupant is not adjusted to the severity of the accident.
SUMMARY OF THE INVENTION
The invention is based on the object of configuring the deformation performance of a steering system in the event of a vehicle crash in such a manner that said performance automatically sets itself to an occupant's mass and vehicle deceleration.
According to the invention, in the case of an occupant protection device for a driver's side of a motor vehicle, in which a steering spindle is guided in a steering-column tube, and a steering wheel is preferably provided with an airbag. The steering spindle is arranged such that it can move in the direction of its longitudinal axis, and said steering spindle is assigned at least one energy-absorbing element.
The advantage of the displaceable steering spindle resides in the fact that the entire steering gear, also including additional subassemblies secured on it, is moved away from the occupant in the event of a crash. As this happens, more or less energy is absorbed depending on the intensity of the impact on the occupant.
It is expedient for an energy-absorbing element to be arranged to adapt automatically to the mass and relative speed of the occupant colliding with the steering wheel or the airbag. This makes it possible to further reduce the risk of injury to the occupant.
This arrangement according to the invention can be realized in a number of embodiments.
Thus, in a first embodiment, provision is made for the steering-column tube to be guided displaceably on at least one holding part which is connected to a vehicle crossmember, which is very largely non-displaceable in the event of a crash. Provision is also made for the energy-absorbing element to be arranged between the steering-column tube and the holding part, the steering spindle being non-displaceable in the steering-column tube. The arrangement of a holding part, which is very largely non-displaceable in the direction of the occupant in the event of a crash, ensures that the steering-column tube, which is mounted displaceably in said holding part, and therefore the steering spindle is displaced away from the occupant. Even if the splashboard, which separates the passenger compartment from the engine compartment, is displaced by the impact in the direction of the occupant the tube and steering spindle are displaced away from the occupant.
It is expedient for the holding part, which is connected to the vehicle crossmember, to have at least one slot in which a guide pin, which is connected to the steering-column tube, engages. It is also expedient for a hydraulic arrangement with a piston and a cylinder to be provided as the energy-absorbing element, the piston being connected to the steering-column tube or to the holding part, and the cylinder being connected to the other part in each case. The holding part preferably has two slots which essentially extend in the direction of the longitudinal axis of the steering-column tube and which are each assigned a guide pin. Each guide pin is secured on a connecting part which is connected to the steering-column tube.
In a further refinement, provision is made for the steering-column tube to have, at its end which faces the occupant, at least one support for a switch unit. This support additionally serves as an element which impedes the deformation of the steering wheel in the event of a crash and therefore prevents the airbag from being deployed in the direction of the vehicle roof instead of in the direction of the occupant.
In a further refinement, a pedal-assembly auxiliary support is provided which is secured pivotably on the holding part at one end, is furthermore secured pivotably on the steering-column tube, and on whose other end is secured to at least one of the clutch, brake and gas pedals. The arrangement of the pedals in this manner achieves the effect that said pedals are pivoted away from the occupant in the event of a crash. The pedal-assembly auxiliary support is expediently connected to the steering-column tube via a clamping device. Releasing this clamping device enables the pedal assembly to be adjusted to the occupant before thejourney is begun. Once the clamping arrangement is fixed in position, the pedal-assembly auxiliary support is connected fixedly to the steering-column tube, so that in this embodiment too, the described advantageous action occurs in the event of a crash.
In a second embodiment, the steering-column tube is connected fixedly to the very largely non-displaceable vehicle crossmember, and the steering spindle can be displaced in the steering-column tube, in the direction of its longitudinal axis. In the case of this embodiment, the steering spindle can therefore be displaced directly.
In a further refinement of this embodiment, a guide bush (or bushing) for the steering spindle is provided in the steering-column tube. The guide bush is rotatable, but is axially non-displaceable, in the steering-column tube. The steering spindle can only be displaced axially in the guide bush. The steering spindle is expediently provided with a serration which is assigned a corresponding serration in the guide bush.
In this embodiment, the steering spindle and the guide bush expediently form a piston-cylinder arrangement, in which the cylinder space is divided by the piston into two chambers which can be connected to each other via at least one valve. Preferably, a plurality of valves which are connected in parallel are provided. A number of valves which differs as a function of the occupant's mass and relative speed of the occupant is brought into a working position. This is brought about by means of sensors which are known per se and by means of an associated control system.
Instead of valves which are connected in parallel, at least one valve having a variable cross section may also be provided.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be explained in exemplary embodiments with reference to drawings, in which:
FIG. 1 shows a side view of a section of a steering spindle with a steering-column tube which can move in a direction of its longitudinal axis;
FIG. 2 shows the steering spindle of FIG. 1 after a crash;
FIG. 3 shows a side view, partially cut away, of a steering spindle which is movable in the direction of its longitudinal axis in an immovable steering-column tube.
DETAILED DESCRIPTION
In the exemplary embodiment of FIG. 1, a steering spindle 1 is mounted rotatably in a steering-column tube 2 , but such that it cannot move in the axial direction. The steering-column tube 2 is guided such that it can move in the direction of its longitudinal axis on a holding part 3 . For this purpose, there are secured, for example welded, on the steering-column tube 2 two connecting parts 4 , 5 which each have a guide pin 6 , 7 . Each guide pin reaches into a respective slot 8 , 9 in the holding part 3 . The holding part 3 is secured on a crossmember 10 of the motor vehicle, which crossmember very largely retains its position in the event of a crash and so the holding part 3 is positionally stable too. This means that it is unnecessary to mount the steering spindle in a splashboard 14 , so the crash performance of the steering system is largely independent of the deformation of the splashboard.
An energy-absorbing element in the form of a piston-cylinder arrangement is provided between the holding part 3 and the steering-column tube 2 . In this arrangement, a cylinder 11 is connected to the holding part 3 , and a piston 12 is connected to the guide pin 6 . Apart from absorbing energy in the event of a crash, this piston-cylinder arrangement can also be used to set the steering spindle. In order to adjust the steering spindle longitudinally and therefore to set it to the particular size of the driver, a lever 13 is provided which can be pivoted about the guide pin 6 . In order to make the longitudinal adjustment, a valve 16 a is actuated by means of the upper part 15 of the lever 13 . Opening of the valve 16 a enables hydraulic fluid to flow via a line 16 into a vessel (not shown), so that the piston can easily be displaced in the cylinder. After the valve 16 a is closed, the function of the piston-cylinder arrangement as an energy-absorbing element is restored. During the displacement of the steering-column tube in order to adjust the steering spindle longitudinally, the guide pins 6 , 7 are only displaced in the slots 8 , 9 by an amount which is substantially smaller than the overall length of the slots. Therefore, a sufficient displacement path is still available in the slots for the displacement of the guide pins in the event of a crash.
An entire pedal assembly of the motor vehicle is likewise connected to the holding part 3 via an auxiliary support 17 by an upper end 18 being secured pivotably on the holding part 3 . The pedals, of which only one pedal 20 can be seen, are arranged pivotably at a lower end 19 of the auxiliary support. In its middle section, the auxiliary support 17 is connected to the steering-column tube 2 via a lever 21 and a clamping means 22 . Release of the clamping means 22 enables the entire pedal assembly to be pivoted and set in accordance with the driver's wishes. When the clamping means is fixed in place, the auxiliary support 17 is connected fixedly to the steering-column tube 2 .
A support 23 for a switch unit is secured on an upper end of the steering-column tube 2 . This support is additionally intended to impede deformation of a steering wheel 40 in an upper steering-wheel rim region in order thereby to obtain a crash-optimized deformation performance of the steering wheel over the entire steering-wheel angle range.
While FIG. 1 shows the normal position of the steering spindle and the pedal assembly, in FIG. 2 the position thereof after a crash is illustrated. In this figure, the steering-column tube 2 is displaced in the direction of the splashboard 14 , i.e. to the left in. the figure, and the guide pins 6 , 7 bear against the left end of the slots 8 , 9 . This displacement of the steering-column tube 2 together with the steering spindle 1 is caused by the impact of the occupant on the steering wheel or on the airbag. This impact causes pressure to be exerted via the steering-column tube on the piston 12 . After a certain level of force at least one valve is opened, so that energy is degraded. A further valve arrangement is explained further on with reference to FIG. 3 .
As a consequence of the displacement of the steering-column tube 2 , the lower end 19 of the pedal-assembly auxiliary support 17 , which is connected non-displaceably to said steering-column tube, is also displaced together with the entire pedal assembly away from the driver in the direction of the splashboard 14 , as can likewise be seen in FIG. 2 .
In the exemplary embodiment of FIG. 3, a steering-column tube 24 is provided which is connected fixedly to the crossmember 10 via connecting parts 25 , 26 . Mounted in the steering-column tube 24 is a steering column consisting of two parts, said parts forming a piston-cylinder arrangement. One part is thus designed as a bushing 27 which is mounted rotatably in the steering-column tube 24 . A steering spindle 28 , which is mounted in an axially displaceable manner in the bushing 27 , runs through this bushing 27 . The torque applied to the steering wheel is transmitted to the bushing by a serration 29 around the circumference of the steering spindle 28 and by a corresponding serration 30 in the bushing 27 .
In its central region, an internal diameter of the bushing 27 is larger than a diameter of the steering spindle 28 . This clearance is divided by a piston 31 , which is provided on the steering spindle, into two chambers 32 , 33 which are sealed off to the outside by sealing elements 34 . The two chambers are connected to each other via valves 35 , 36 , 37 which are connected in parallel.
A closed volume of a suitable medium, preferably a fluid, is situated in the chambers 32 , 33 and in the lines connecting them. In the basic position which is illustrated, the connection between the chambers 32 , 33 is interrupted, i.e. the axial displaceability of the steering spindle 28 and therefore of the steering wheel (not illustrated) is blocked. In order to adjust the steering column, all of the valves are brought into their working position in which they have a predetermined through-flow cross section. Axial displacement using little effort is therefore possible by the medium being pressed out of the chamber 32 into the chamber 33 and vice versa.
In the event of a crash, as the energy-absorbing element, the piston-cylinder arrangement of the steering column ensures that the energy caused by an occupant colliding with the steering wheel directly, or indirectly via a deployed gas bag, is degraded. In this arrangement, the valve system enables the damping performance to adjust automatically to the severity of the accident. For this purpose, a number of valves 35 , 36 , 37 which differs as a function of the mass and the relative speed of the occupant, is brought into their working position and the through-flow cross section therefore varies. Displacement of the medium from chamber 32 to chamber 33 is therefore possible at a different level of force. The necessary number of valves is set by means of sensors (not illustrated) and an assigned control switch system, which is known per se.
The valve arrangement described with respect to FIG. 3 can also be used for controlling the piston-cylinder arrangement of FIG. 1 .
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In an occupant protection device for a driver's seat of a motor vehicle, a steering spindle is arranged in a jacket tube and a steering wheel is preferably provided with an airbag. The steering spindle is movable in the direction of its longitudinal axis and at least one energy-absorbing element is associated with the steering spindle. The advantage of the sliding steering spindle is that the whole steering system, including additional subassemblies secured thereto, is moved away from the occupant in the event of a crash. Depending on the intensity of the impact on the occupant, more or less energy is absorbed.
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PRIORITY
[0001] This application claims the benefit of priority to U.S. Non-Provisional patent application Ser. No. 13/414,473, filed on Mar. 7, 2012 which claims priority to U.S. Provisional Patent Application No. 61/450,019, filed on Mar. 7, 2011, both of which are hereby incorporated by reference in their entirety.
TECHNICAL FIELD
[0002] This disclosure relates to piston and cylinder liner configurations for internal combustion engines.
BACKGROUND
[0003] Internal combustion engines are subject to government regulations and customer expectations. Government regulations include reducing emissions and improving engine efficiency to reduce fuel consumption. Customer expectations include improved engine reliability and longer engine life. While great strides have been made in addressing government regulations and improving the life of internal combustion engines, internal combustion engines are highly complex mechanisms and innovative approaches to engine components may yield life, reliability, and efficiency improvements.
SUMMARY
[0004] This disclosure provides an internal combustion engine comprising an engine body, a cylinder bore, a cylinder liner, and a piston. The cylinder bore is formed within the engine body and has at least one coolant passage located radially outward from the cylinder bore. The cylinder liner is positioned within the cylinder bore and has an internal diameter D. The piston is positioned within the cylinder liner to reciprocate along an axis. The piston includes a top surface, an outside wall having an outer peripheral surface, and a groove positioned an axial distance B from the top surface. A ratio of distance B to internal diameter D is less than 0.090.
[0005] Advantages and features of the embodiments of this disclosure will become more apparent from the following detailed description of exemplary embodiments when viewed in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 is a sectional view through a portion of an internal combustion engine in accordance with an exemplary embodiment of the present disclosure.
DETAILED DESCRIPTION
[0007] FIG. 1 shows an internal combustion engine 10 in accordance with an exemplary embodiment of the present disclosure. Engine 10 includes an engine body 12 , only a small portion of which is illustrated, a cylinder head 14 mounted on engine body 12 , at least one cylinder liner 16 positioned in engine body 12 , and at least one piston 18 positioned for reciprocal movement along an axis in cylinder liner 16 . Of course, engine 10 may contain a plurality of cylinder liners 16 and pistons 18 , for example four to eight of each, which may be arranged in a line or in a “V” configuration. As discussed hereinbelow, engine 10 includes various precise configuration parameters that yield certain benefits, such as improved cooling of pistons 18 and cylinder liners 16 , achieving improved life and reliability of engine 10 , and reducing emissions and achieving improved fuel economy and efficiency from engine 10 .
[0008] Engine body 12 includes at least one cylinder bore 20 . Cylinder liner 16 is positioned within cylinder bore 20 . Cylinder liner 16 includes an internal bore 17 , having an internal diameter D, to locate piston 18 . Piston 18 may be any type of piston so long as it contains the features identified hereinbelow necessary for accomplishing the present invention. For example, piston 18 may be an articulated piston. Liner 16 separates a lubricated portion 22 located at an interior portion of cylinder liner 16 and a combustion chamber 23 positioned at one end of an internal bore 17 between piston 18 and cylinder head 14 from a plurality of coolant passages 26 (e.g., 26 a, 26 b, 26 c ) formed in engine body 12 . A combustion bowl 24 positioned in a proximate, top or upper portion of piston 18 is part of combustion chamber 23 .
[0009] Combustion bowl 24 may have a plurality of features formed therein. For example, combustion bowl 24 may have a central portion 24 a that is axially closer to cylinder head 14 than an annular portion 24 b that extends around central portion 24 a. These features may be related to the characteristics of combustion chamber 23 , which may include fuel flow and how the fuel flow combusts or ignites (not shown). Combustion chamber 23 may have the characteristics of the combustion chamber described in U.S. Pat. No. 6,732,703, issued May 11, 2004, the entire content of which is incorporated by reference in its entirety.
[0010] Coolant passages 26 may be configured to provide optimal cooling for piston 18 . For example, coolant passage 26 a may be a high velocity coolant flow and coolant passage 26 b may be a low velocity coolant flow. Coolant passage 26 c may be a port that connects one part of fluid passages 26 with another part of fluid passage 26 , such as coolant passage 26 a with coolant passage 26 b.
[0011] Cylinder liner 16 includes a top flange portion 28 having an axial or longitudinal thickness A. Cylinder liner 16 also includes an annular wall portion 32 having a radial thickness C that extends axially or longitudinally from top flange portion 28 . Positioned axially further from wall portion 32 may be a protrusion 33 that cooperates with cylinder bore 20 to separate coolant passage 26 a from coolant passage 26 b. Included on cylinder liner 16 axially further from protrusion 33 may be a stop or step 34 . A wall portion 37 is located on cylinder liner 16 and extends from protrusion 33 to stop 34 . Top flange portion 28 includes an outer annular surface 30 that opposes annular cylinder bore 20 . Coolant passage 26 a is positioned radially outward from wall portion 32 on one side of cylinder liner 16 and coolant passage 26 c is positioned radially outward from wall portion 32 on the opposite side of cylinder liner 16 from coolant passage 26 a. Coolant passage 26 a, coolant passage 26 b, and coolant passage 26 c may be part of a single coolant passage that extends angularly about cylinder liner 16 .
[0012] Stop 34 located on cylinder liner 16 engages an annular land or stop 35 located on engine body 12 . Stop 34 provides a location that sets the depth or offset of a proximate, near or upper surface 40 of cylinder liner 16 with respect to a top surface 38 of engine body 12 . Stop 34 sets the axial length of the gap between top surface 40 of cylinder liner 16 and cylinder head 14 or a cylinder head gasket 41 . A stop having similarity to stop 34 is described in U.S. Pat. No. 4,294,203, issued Oct. 12, 1981, the entire content of which is hereby incorporated by reference. One or more grooves 42 may also be positioned on an outer wall 36 of cylinder liner 14 . One or more seals 44 may be positioned in each groove 42 . Seals 44 separate lubricated portion 22 from coolant passages 26 .
[0013] Cylinder liner 16 is inserted into engine body 12 from the top or proximate end of cylinder bore 20 . The outer periphery of cylinder liner 16 is a slip fit with cylinder bore 20 in the area of cylinder liner 16 that includes grooves 42 . As previously noted, seals 44 positioned within grooves 42 prevent lubricant from lubricated portion 22 from contaminating the coolant located in coolant passages 26 and prevent coolant from passages 26 from contaminating the lubricant in lubricated portion 22 . Annular surface 30 of flange portion 28 is a press fit with an inner surface 94 of cylinder bore 20 . The press fit may provide a seal between fluid passages 26 and combustion chamber 23 and secures cylinder liner 16 within engine body 12 . A seal (not shown) may also be located between flange portion 28 and inner surface 94 of cylinder bore 20 .
[0014] As previously noted, piston 18 is located within internal bore 17 , which has internal diameter D, of cylinder liner 16 . Piston 18 is shown in a top dead center (TDC) position in FIG. 1 . Piston 18 drives a conventional connecting rod 46 attached to a pin, rod or shaft 48 secured to piston 18 . Connecting rod 18 drives a crankshaft (not shown) of engine 10 . Connecting rod 18 and the crankshaft cause piston 18 to reciprocate along a rectilinear path within cylinder liner 16 . The TDC position is attained when the crankshaft is positioned to move piston 18 to the furthest position away from the rotational axis of the crankshaft. In the conventional manner, piston 18 moves from the TDC position to a bottom dead center (BDC) position when advancing through intake and power strokes. Piston 18 includes a plurality of grooves for piston rings and seals located on a periphery, outside diameter, or outside surface 49 of an outside wall 43 of piston 18 . The plurality of grooves includes a top, upper, proximate, or first groove 50 , a second, center or middle groove 52 and a third, bottom, lower, or distal groove 54 . Top groove 50 includes a first conventional compression ring 56 that assists to prevent combustion gas from combustion chamber 23 from travelling between piston 18 and cylinder liner 16 . An upper side 62 of top groove 50 is positioned a distance B from a top, upper, or proximate surface 64 of piston 18 . Middle groove 52 includes a second conventional compression ring 58 . Third groove 54 includes a conventional oil control ring 60 that limits the amount of oil that moves along internal bore 17 toward the upper or proximate end of piston 18 where combustion bowl 24 is located.
[0015] Distance B of top groove 50 is important from an emissions perspective. There is a radial gap between exterior or peripheral surface 49 of outside wall 43 of piston 18 and internal bore 17 of cylinder liner 16 . Fuel that is trapped in the region between peripheral surface 49 and internal bore 17 in the region above top ring 56 , which may be called a dead zone, is not combusted. This fuel becomes exposed as piston 18 moves away from the TDC position and the fuel enters an exhaust (not shown) of engine 10 . Unburned fuel contributes to increased emissions and leads to less efficiency of engine 10 . Thus, the ability to decrease distance B decreases emissions and improves fuel efficiency.
[0016] A scraper ring 39 may be positioned in cylinder liner 16 at an interior portion of top flange portion 28 . Scraper ring 39 has an inner diameter that is smaller than the diameter of internal bore 17 . Scraper ring 39 reduces the volume of the dead zone described hereinabove as well as helping to remove deposits on surface 49 of piston wall 43 above top groove 50 . Thus, scraper ring 39 helps remove deposits above top or first compression ring 56 .
[0017] Piston 18 is fabricated from two separate portions. An upper, proximate, or top portion 66 is joined to a lower, distal, or bottom portion 68 along a first joint 70 and a second joint 72 . First joint 70 includes a surface 74 located on lower portion 68 and a matching surface 76 located on upper portion 66 . First joint 70 is positioned between top groove 50 and second groove 52 . Second joint 72 includes a surface 78 located on upper portion 66 and a surface 80 located on lower portion 68 . Second joint 72 is axially displaced from first joint 70 in a direction that is further from combustion chamber 23 than first joint 70 . By having second joint 72 in this position, a wall or rib 88 , which is described in more detail hereinbelow, is readily accessible from a radial direction to form features therein, such as fluid passages (not shown). Top portion 66 and bottom portion 68 are affixed to each other through a conventional spin welding process. By fabricating piston 18 as two separate pieces, a gallery 82 may be extended, or positioned closer to top surface 64 during the fabrication of upper portion 66 since the interior of upper portion 66 is accessible prior to attaching or welding upper portion 66 to lower portion 68 .
[0018] Gallery 82 has a lower portion 82 a having a radial extent and an upper portion 82 b having a radial extent that is less than the radial extent of lower portion 82 a. Lower portion 82 a extends radially from a radial distance from the central axis of piston 18 , and upper portion 82 b extends radially from a radial distance that is further from the central axis of piston 18 than lower portion 82 a because upper portion 82 b follows the contour of combustion bowl 24 . Because upper portion 82 b follows the contour of combustion bowl 24 , the uppermost portion of portion 82 b of gallery 82 may be located at a distance equal to the wall thickness of combustion bowl 24 from top surface 64 of combustion bowl 24 . The position of the uppermost portion of portion 82 b enables top groove 50 to be in a closer position at distance B from top surface 64 than is possible in conventional piston designs, as will be explained in more detail hereinbelow. Positioning top groove 50 at distance B provides an advantage in that heat travels a shorter distance in piston 18 before reaching a cooling fluid than in a conventional piston design. The faster access to a cooling fluid reduces heat buildup in piston 18 , decreasing the stress on piston 18 , which therefore increases the life of piston 18 . Oil splash from connecting rod 46 goes through a plurality of piston passages 84 into gallery 82 and then back out piston passages 84 into lubricated portion 22 .
[0019] Hollowing out the interior of a conventional piston to form a gallery similar to gallery 82 is not possible because the top surface of a conventional piston would be unable to withstand the stresses in an associated combustion chamber. The reason a conventional piston is unable to withstand these stresses is because there would be insufficient support within a conventional piston to withstand the combustion pressure exerted on the top surface of a convention piston. Piston 18 overcomes this difficulty by fabricating upper piece or portion 66 and lower portion 68 , forming gallery 82 into at least upper portion 66 , and then welding the two portions together via a spin welding process. The outer surface or diameter 49 of piston 18 may then be machined, ground and/or honed to a desired dimension, removing any unevenness left by the spin welding process.
[0020] Passages 84 may be located in lower or distal portion 68 during casting or may be machined into lower portion 68 after casting. Wall or rib 88 located in proximate portion 66 is contiguous with a wall or rib 86 located in distal portion 68 . Wall or rib 88 and wall or rib 86 , because of the spin welding process, form a contiguous or continuous wall or rib that extends from a combustion bowl wall 90 , which is part of combustion bowl 24 , to a sidewall portion 92 , which is axially below bottom groove 54 . Sidewall portion 92 is part of sidewall, exterior wall, or outside wall 43 of piston 18 . Thus, piston 18 has the ability to provide cooling to a peripheral portion of the top of piston 18 in a region between combustion bowl 24 and outside wall 43 of piston 18 while maintaining the strength of a conventional piston because of the two-piece piston design.
[0021] To obtain the maximum cooling, emissions and efficiency benefit from the aforementioned features, certain ratios are applicable. A first ratio is quantified in equation (1), which specifies a limit for the ratio of the top ring distance B from top surface 64 of piston 18 to piston bore diameter D. This ratio applies to piston bores having a diameter that meets the requirements of equation (2).
[0000] B/D< 0.090 (Equation 1)
[0000] 275 mm≧D≧165 mm (Equation 2)
[0022] Distance B and diameter D are sized and dimensioned to result in a aximum ratio of 0.090, as described by equation (1), and preferably a maximum ratio of 0.085. The range of diameter D that achieves these ratios is as listed in equation (2) with a preferable range provided in equation (3).
[0000] 275 mm≧D≧175 mm (Equation 3)
[0000] Meeting the requirements of equation (1) is critical to optimizing emission and reducing fuel consumption. It is apparent from equation (1) that distance B should be as close to top surface 64 of piston 18 as possible while maintaining the strength of piston 18 . However, gallery 82 needs to extend to a location closer to top surface 64 of piston 18 than top groove 50 . Otherwise, cooling of piston 18 in the area of top groove 50 will be inadequate, leading to excessive heating of compression ring 56 , which leads to wear and early failure of cylinder liner 16 . Thus, top groove 50 can be no closer to top surface 64 than gallery 82 , which can only be as close to top surface 64 as the required strength of combustion bowl wall 90 .
[0023] Improved cooling of piston 18 is achieved by two aspects of the present disclosure. First, distance B of top groove 50 with respect to thickness C of cylinder liner 16 in wall portion 32 determines, in part, the adequacy of cooling of piston 18 . The relationship between distance B and thickness C is defined in equation (4).
[0000] B/C< 1.30 (Equation 4)
[0000] Distance B and thickness C are sized and dimensioned to result in a maximum ratio of 1.30 and preferably a maximum ratio of 1.25. As in equation (1), equation (4) indicates that distance B should be relatively small, at least in comparison to thickness C of wall portion 32 of cylinder 16 . As previously noted, while distance B should be as small as possible, this distance is limited by the ability to cool top groove 50 , which is limited by the ability to extend gallery 82 as close to top surface 64 of piston 18 as possible. The second aspect of cooling is determined by a ratio of thickness A of top flange 28 to distance B, specified in equation (5).
[0000] A/B< 0.80 (Equation 5)
[0000] Thickness A and distance B are sized and dimensioned to result in a maximum ratio of 0.80 and preferably a maximum ratio of 0.80. Thickness A of top flange 28 determines how close coolant passage 26 a comes to top surface 40 of cylinder liner 16 , which also limits distance B since thickness A must be no more than 0 . 75 times distance B. By having thickness A meet this condition, coolant is able to provide optimal cooling for top groove 50 . However, thickness A has a minimum thickness determined by the ability to withstand the pressures from combustion chamber 23 and by the ability to press fit top flange 28 into cylinder bore 20 . Thus, distance B is limited by two factors, the minimum thickness of top flange 28 and by the ability to make gallery 82 extend close to surface 64 of piston 18 .
[0024] Considering now equations (1)-(5), it is apparent that optimal cooling of piston 18 is achieved by meeting the requirements of equations (4) and (5), and minimum emissions and best efficiency is achieved by meeting the conditions of equations (1)-(3). The key to cylinder liner, piston ring, and piston longevity is minimizing the top ring reversal temperature. The top ring reversal temperature is the temperature of top compression ring 56 when piston 18 is at TDC and about to change direction from an upward stroke to a downward stroke. If the top ring reversal temperature is too high, then excessive wear of cylinder liner 16 and piston ring 56 occurs, shortening the life of cylinder liner 16 and piston ring 56 . However, groove 50 , which holds ring 56 , can only be moved higher by enabling cooling of ring 56 . The present disclosure describes a configuration that enables a much higher position for groove 50 and ring 56 than in conventional designs when the conditions of equations (1)-(5) are met, which improves the life and reliability of piston 18 as well as decreasing emissions and improving engine 10 efficiency.
[0025] While various embodiments of the disclosure have been shown and described, it is understood that these embodiments are not limited thereto. The embodiments may be changed, modified and further applied by those skilled in the art. Therefore, these embodiments are not limited to the detail shown and described previously, but also include all such changes and modifications.
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A cylinder liner and piston configuration for an internal combustion engine includes features for improving the cooling of the piston. Specific ratios and dimensions are included to optimize the features of the cylinder liner and piston. Also included are unique piston features that assist in achieving some of the specified dimensions and ratios.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The present patent application is a continuation-in-part of U.S. patent application Ser. No. 11/813,374, entitled “A MOLDING EQUIPMENT AND METHOD TO MANUFACTURE STACKABLE INTER-ENGAGING BRICKS, BLOCKS, STONES AND THE LIKE WITH A SMOOTH OR EMBOSSED FACE”, and filed at the United State Patent and Trademark Office on Jan. 9, 2006, which claims the benefits of priority of Canadian Patent Application No. 2,492,250, entitled “A MOLDING EQUIPMENT AND METHOD TO MANUFACTURE STACKABLE INTER-ENGAGING BRICKS, BLOCKS, STONES AND THE LIKE WITH A SMOOTH OR EMBOSSED FACE”, and filed at the Canadian Patent Office on Jan. 11, 2005, the content of which is incorporated herein by reference.
FIELD OF THE INVENTION
The present invention relates to the field of stackable inter-engaging bricks, blocks, stones and the like for building mortarless walls. This invention relates more precisely to the process of manufacturing individual smooth or embossed face or attached splittable inter-engaging bricks, blocks, stones and the like. As used herein, the word “bricks” also refers to blocks, stones and the like.
BACKGROUND OF THE INVENTION
Stackable inter-engaging bricks are used to build mortarless walls and this is known in the art. Wall building blocks which may be stacked and interlocked without being held together by a binding agent such as mortar are known. One such block has a top face which comprise a tongue element and a bottom face which comprise a mortise element. Both elements are configured in such a way that when two blocks are stacked, the bottom face of a block engages with the top face of a like block disposed below while the top face of the block engages with the bottom face of an above-disposed block. An example of such a block is shown in U.S. Pat. No. 6,108,995 (Bouchard et al.).
In the process of manufacturing stackable inter-engaging bricks 101 ( FIG. 16 ), multiple attached splittable bricks made of brick material such as concrete are first cast in a metal mold. The molded attached brick units are then extracted from the mold 100 ( FIG. 1 ) and conveyed through the manufacturing plant on steel or wood plates. The molded attached brick units are then cured in kilns in order to cure the brick material. Once cured, each of the attached bricks are detached in the middle in two individual split face bricks by the mean of a known splitting equipment. In this embodiment, every molded attached brick unit can produce two split face bricks.
The reason for manufacturing two split face bricks from a single attached splittable brick unit is found in the fact that, prior the completion of the curing procedure, an uncured single brick would be too fragile to be conveyed in the manufacturing plant without being unacceptably damaged or deformed in the process. Conveying uncured individual prior art bricks would result in an increase of defective or rejected bricks.
Also, the process of cutting attached brick units into individual bricks causes the bricks to have split faces, which may not be always desired.
The Bouchard mold, as the present mold, molds bricks standing on their side. It is important to understand that molding bricks on their side is not a simple design choice. As a matter of fact, inter-engaging bricks such as the bricks molded by the Bouchard mold are not held together by mortar. Such inter-engaging bricks are stacked rows upon rows in an inter-engaging manner. In that sense, the bricks are shaped such that the bottom portion of one brick is configured to engage the top portion of a brick located underneath.
The advantages of inter-engaging bricks are many. For instance, since they do not need mortar, their installation is typically much faster then regular mortar-held bricks. Also, such bricks can typically be installed by less skilled workers.
However, to provide a proper wall structure made from such inter-engaging bricks, it is important that the height of the brick, as viewed in their normal installed orientation, be constant, with low tolerance. Indeed, since such inter-engaging bricks are not held by mortar, the installer cannot use mortar to compensate for height variations between bricks during installation. Should the bricks have large height variations, the resulting wall constructed with such bricks would be misaligned as the cumulative effect of large height variations would be compounded over several rows of bricks.
Hence, by molding the bricks on their side, the bricks have very limited height variation but some length variations. However, variations in length are much less critical since bricks installed on the same row are installed side-by-side and any variation in length is or can be compensated for.
However, depending on the shape of the side section, bricks molded on their side can be unstable when standing on their side during the manufacturing process. In that sense, the shape of the side section of the bricks shown in Bouchard has been found to be somewhat unstable. The solution proposed in Bouchard was to link two bricks together with a bridging element. Once bridged, the overall side section of the bridged bricks is much more stable. Consequently, the bridged bricks can be carried around in the manufacturing plant with less risk of falling apart or being deformed, particularly in uncured state. In addition, the bridged bricks cannot rub against each other, preventing damages during transportation.
Still, the bridged bricks of Bouchard must be manually separated prior to installation. The manual separation involves the manual splitting of the bricks by hand and then the manual removal of the remaining portions of the bridge with a hammer. All these steps increase the manual labor required by the installers.
There is thus a need to find a mean by which stackable bricks could be molded, conveyed and cured individually without being damaged or deformed unacceptably and in such a way that the resulting brick faces could be smooth or embossed.
SUMMARY OF THE INVENTION
To overcome such shortcomings, the bricks resulting from the presently claimed molding equipment are individual in that they are not connected nor bridged as in the prior art. However, to achieve such a result, the individual bricks must be able to stand on their side in uncured state and be carried around without being damaged or otherwise deformed.
One of the main goals of the presently claimed invention is to provide a molding equipment capable of molding pairs of individual bricks suitably sized and shaped to be able to stand on their side in uncured form without being damaged or otherwise deformed during the manufacturing process.
After being molded, bricks, still uncured, travel through the manufacturing plant on steel plates. As they travel, the bricks are subjected to some shocks and vibrations. If the uncured bricks are too fragile, they will be damaged or otherwise deformed as they travel from the molding equipment to the kiln, thereby resulting in defective bricks to be discarded.
Another goal of the presently claimed invention is to have the molding equipment also capable of molding pairs of attached bricks, if needed.
The present invention discloses that when the individual bricks have a certain ratio of the side-section to the length, uncured bricks will be able to stand on their side and be carried around with less risks of being damaged or otherwise deformed.
According to an aspect of the present invention, using the shape of bricks as disclosed herein, a satisfactory ratio of approximately 26.65:1 must be used.
As such, the presently claimed invention comprises a molding equipment comprising a mold having a plurality of cavities, and removable brick separating elements configured to separate the cavities into two fully separated sub-cavities, each sub-cavity being configured to mold an individual brick standing on one of its sides.
According to another aspect of the invention, there is provided a molding equipment for molding multiple pairs of individual stackable inter-engaging bricks with a smooth or embossed face and without being damaged or deformed during molding, the molding equipment comprising:
a main body comprising cavities, each of the cavities being adapted to cast an appropriate material to produce the bricks, and each of the cavities comprising first attachment points; and
brick separating elements distinct from the main body, each of the brick separating elements comprising an upper part configured to be secured to the main body, and comprising several brick separating plates extending downwardly from the upper part and being respectively attachable to the first attachment points of the cavities to create two fully separated sub-cavities in the cavities;
wherein the sub-cavities are configured to form bricks with an appropriate side-section area to brick length ratio of approximately 26.65:1 so as to prevent the bricks from being damaged or deformed during molding, and wherein each of the separated sub-cavities is adapted to mold individual smooth or embossed face bricks standing on one of their sides.
According to still another embodiment, there is provided a molding equipment for molding multiple pairs of individual stackable inter-engaging bricks with a smooth or embossed face and without being damaged or deformed during molding, the molding equipment comprising:
a main body comprising cavities, each of the cavities being adapted to cast an appropriate material to produce the bricks, and each of the cavities comprising first attachment points; and
brick separating elements distinct from the main body, each of the brick separating elements comprising an upper part configured to be secured to the main body, and extending downwardly from the upper to the lower portion of the main body;
wherein brick separating elements are secured to the main body using dogs, wherein the sub-cavities are configured to form bricks and wherein each of the separated sub-cavities is adapted to mold individual smooth or embossed face bricks standing on one of their sides.
To attain these and other objects which will become more apparent as the description proceeds. According to one aspect of the present invention, a method to manufacture both individual smooth or embossed face bricks and attached splittable bricks is provided. Each of the bricks has a tongue interlock element and a mortise interlock element configured in such a way that the bricks are in a mutual engagement when bricks, blocks or stones or the like are stacked one of top of the other.
Molding equipment in accordance with the present invention comprises a mold having at least one and preferably a plurality of cavities. Each cavity allows the formation of a pair of splittable bricks. A brick separating element may be installed in the middle of each cavity to allow the formation of two individual free standing bricks. The brick separating element is typically secured in place by mean of a fastening device such as screws or bolts. Once the brick separating element is installed, the attached splittable brick cavity is effectively separated in two individual mold cavities.
The brick separating element has an upper part which contains openings. The openings are provided to receive fasteners such as screws or bolts. The fasteners are generally used to secure the brick separating element to the molding equipment main body.
The brick separating element is made from a hard and resistant material such as steel or cast iron.
The brick separating element can have a smooth surface or a surface with projection and/or cavities.
A method for manufacturing individual smooth or embossed face bricks using the molding equipment and the cavity separating element is also provided.
The method comprises: a) selecting the individual molds in which individual smooth face or embossed face bricks are to be molded, b) installing the smooth face brick separating element in the selected molds, c) installing the embossed face brick separating element in the selected molds, d) fastening the smooth face brick separating element with fasteners, e) fastening the embossed face brick separating element with fasteners, f) installing the molding equipment in the molding machine.
The invention accordingly comprises the construction, combination of elements, and arrangement of parts which will be exemplified in the construction herein set forth. Although the above summary describes more precisely the manufacturing of stackable inter-engaging bricks blocks, stones and the like to build mortarless wall on a structure, the present invention could also be used for example, to manufacture stackable inter-engaging bricks, blocks, stones and the like to build landscaping walls.
Other and further aspects and advantages of the present invention will be obvious upon an understanding of the illustrative embodiments about to be described or will be indicated in the appended claims, and various advantages not referred to herein will occur to one skilled in the art upon employment of the invention in practice.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other aspects, features and advantages of the invention will become more readily apparent from the following description, reference being made to the accompanying drawings in which:
FIG. 1 is an isometric view of prior art molding equipment used to manufacture splittable stackable inter-engaging bricks;
FIG. 2 is an isometric view of an individual stackable inter-engaging brick;
FIG. 3 is a top view of molding equipment to be used in manufacturing splittable stackable inter-engaging bricks in accordance with the present invention;
FIG. 4 is a top view of the molding equipment to be used in manufacturing individual smooth (or embossed) face stackable inter-engaging bricks in accordance with the invention;
FIG. 5 is a top view of two individual smooth (or embossed) face stackable inter-engaging bricks as produced in the molding equipment shown in FIG. 4 ;
FIG. 6 is an isometric of a single smooth face stackable brick in accordance with the invention;
FIG. 7 is a top view of splittable bricks as produced in the molding equipment shown in FIG. 3 ;
FIG. 8 is a side view of stacked bricks in accordance with the invention;
FIG. 9 is an isometric view of a single split face stackable brick in accordance with the invention;
FIG. 10 is a top view of smooth (or embossed) face bricks as produced in the molding equipment shown in FIG. 4 ;
FIG. 11 is an isometric view of a single embossed face stackable brick in accordance with the invention;
FIG. 12 is an isometric view of the brick separating element to be used in manufacturing smooth face stackable inter-engaging bricks;
FIG. 13 is an isometric view of the brick separating element to be used in manufacturing embossed face stackable inter-engaging bricks;
FIG. 14 is a side view of one brick separating plate to be used in manufacturing embossed face stackable inter-engaging bricks;
FIG. 15 is a side view of a possible pattern created by using several embossed face stackable inter-engaging bricks.
FIG. 16 is a top view of a prior art splittable stackable inter-engaging bricks as produced by a prior art molding equipment.
FIG. 17 is an isometric view of a molding equipment to manufacture splittable stackable inter-engaging bricks according to the present invention;
FIG. 18 is an exploded view of the molding equipment shown in FIG. 17 ;
FIG. 19 is a front elevation view of the molding equipment shown in FIG. 17 ;
FIG. 20 is a rear elevation view of the molding equipment shown in FIG. 17 ;
FIG. 21 is a top plan view of the molding equipment shown in FIG. 17 ;
FIG. 22 is bottom plan view of the molding equipment shown in FIG. 17 ;
FIG. 23 is a top view of a plate holding element;
FIG. 24 is a cross sectional view of the molding cavity;
FIG. 25 is a cross sectional view of a splitting plate for an embossed brick;
FIG. 26 is a perspective view of the splitting plate for an embossed brick;
FIG. 27 is a rear view of the splitting plate of FIG. 26 ;
FIG. 28 is a side elevation view of the splitting plate of FIG. 26 ;
FIG. 29 is top plan view of the splitting plate of FIG. 26 ;
FIG. 30 is a front elevation view of the splitting plate of FIG. 26 ;
FIG. 31 is bottom plan view of the splitting plate of FIG. 26 .
FIG. 32 is a left side elevation view of the molding equipment shown in FIG. 17 .
FIG. 33 is a perspective view of the elongated “v” shaped inducing member with securing dogs, omitting the molding cavities.
FIG. 34 is a perspective view of separating plates and securing dogs omitting the molding cavities.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
A novel molding equipment for molding inter-engaging bricks and a method for using the same will be described hereinafter. Although the invention is described in terms of specific illustrative embodiments, it is to be understood that the embodiments described herein are by way of example only and that the scope of the invention is not intended to be limited thereby.
With reference to the annexed drawings, the preferred embodiments of the present invention will be herein described for indicative purposes and by no means as of limitation.
The drawings and the description attached to it are only intended to illustrate the idea of the invention. As to the details, the invention may vary within the scope of the claims. So, the size and shape of the individual stackable inter-engaging brick 1 ( FIG. 6 ) may be chosen as desired, as long the size and shape enable the individual brick to stand on its side uncured as shown in FIG. 6 without falling over, being damaged, buckling or being otherwise deformed during the manufacturing process.
Referring to FIG. 6 , for a single individual stackable inter-engaging brick 1 having the present side-section shape 3 shown will stand on its side uncured without falling over, being damaged, buckling or being otherwise deformed during the manufacturing process if the side-section area 3 to the brick length 2 ratio is 26.65:1. As such, for a brick of this shape, a ratio of approximately 26.65:1 is preferred to provide an optimal standing brick. However, given other brick characteristics such as brick material, brick shape, brick side-section inertia momentum and brick length according to FIG. 6 , the ratio would be different.
Referring to FIGS. 3 and 4 , the molding equipment main body 10 is illustrated. Several cavities 12 are created in the molding equipment main body 10 . The cavities 12 are used to cast the concrete or other appropriate material to produce bricks (not shown here).
FIG. 3 shows molding equipment for producing splittable brick units. However, in FIG. 4 , a brick separating element 11 has been attached to the mold 12 (see FIG. 3 ) at attachment points 20 and 21 . The brick separating element 11 attached at attachment points 20 and 21 thus creates two separated cavities 13 to mold individual smooth or embossed face bricks.
FIG. 12 shows the brick separating element used to manufacture individual smooth face bricks. The upper part 30 of the brick separating element has openings 31 at both ends of the upper part to secure the brick separating element to the molding equipment main body 10 (see FIGS. 3 and 4 ). The brick separating element may have several brick separating plates 32 .
FIG. 13 shows the brick separating element used to manufacture individual embossed face bricks. The upper part 30 of the brick separating element has openings 31 at both ends of the upper part to secure the brick separating element to the molding equipment main body 10 (see FIGS. 3 and 4 ). The brick separating element may have several brick separating plates 33 .
Referring to FIGS. 12 and 13 , smooth 32 and embossed 33 brick separating plates are illustrated. The smooth 32 and embossed 33 brick separating plates have “V” shaped grooves 34 on each side to secure each brick separating plate 32 / 33 in the molding equipment main body 10 (see FIGS. 3 and 4 ).
Notably, in the presently claimed invention, the brick separating elements 11 fully separate the cavities 21 into two fully separated sub-cavities. Moreover, the bricks resulting from the molding equipment are fully separated and do not need any additional splitting step.
Now referring to FIGS. 17-18 , according to another embodiment of the present invention if shown a novel molding equipment used to manufacture splittable stackable inter-engaging bricks 1 . The molding equipment used to manufacture splittable stackable inter-engaging bricks 1 comprises a main body 200 and a brick extraction module 220 .
The main body 200 further comprises at least one, preferably a plurality of molding blocks having a series of moulding cavities for the manufacture splittable stackable inter-engaging bricks 1 . According to the present invention, the moulding cavities may be used for the manufacture of splittable stackable inter-engaging bricks 1 or may additionally comprise a middle plate 111 used to mold the brick without any further splitting required. According to this latter embodiment, the mortarless inter stackable bricks 1 are typically manufacture using a similar molding cavity whereas the user employ a fixation system for securing the separating plates 111 , to the molding blocks.
The fixation system referred herein comprises dog elements designed to secure the separating elements, such as separating plates 111 , to the molding blocks. The separating elements are inserted in the molding cavities of the molding blocks. The separating elements are than secured using an upper and lower dog respectively located on top and below the separating elements. The dogs are generally fixated to the molding blocks using at least one, preferably two fasteners. Depending on the configuration of the molding blocks there may be various types of dogs. In the present embodiment, three different types of upper 130 , 132 , 134 and lower 140 , 142 , 144 dogs are used. The first upper dogs type 130 are located toward the lowed portion of the inter-engaging stackable brick 1 , the second upper dogs type 132 are overlapping two mold cavities and the third upper dogs types 134 are at the top of the upper portion of the decorative brick portion. Similarly, according to the present embodiment, the first lower dogs type 140 are located toward the lowed portion of the inter-engaging stackable brick 1 , the second lower dogs type 142 are overlapping two mold cavities and the third lower dogs types 144 are at the top of the upper portion of the decorative brick portion. Understandably, depending on the configuration of the molding blocks and the molding cavity one could according to another embodiment without departing with the principle of the present invention, envision a dog designed to be universal thus having the ability to fit in all dog securing positions.
According one aspect of the present embodiment, the same mold cavities may be utilised for the manufacture of both mortarless stackable inter-engaging bricks 1 and mortarless splittable stackable inter-engaging bricks 1 . In the former mortarless inter-engaging stackable bricks 1 the dogs 130 , 132 , 134 , 140 , 142 , 144 will be used in combination with separating plates 111 whereas in the later mortarless splittable inter-engaging stackable bricks 1 the dogs 130 , 132 , 134 , 140 , 142 , 144 will be used in combination with elongated “v” shaped inducing member 120 .
According to one embodiment, to account for the use of the present dogs 130 , 132 , 134 , 140 , 142 , 144 , the molding blocks and molding cavities 212 preferably have grooves for mating with the protruding portion 160 of the elongated “v” shaped inducing member 120 or the protruding portion 170 of the plate 111 . These protruding portions 160 , 170 are preferably used to respectively insure secure fixation of the elongated “v” shaped inducing member 120 and plate 111 to the mold during use of the molding equipment.
According to one aspect of the present embodiment, the groove inducing portion 120 and plates 111 generally have indentations 113 , 114 , 112 , 115 on their lower and upper portion as to mate with the groove or plate 111 securing portions of the dogs 130 , 132 , 134 , 140 , 142 , 144 .
The separating plates 111 may be of various kind to produce different patterns or textures. They optionally also may be flat. In addition, the separating plates 111 typically comprise a portion inducing part of the “v” groove shape the stackable inter-engaging bricks preferably have.
Now referring to FIGS. 17-22 is shown the brick extraction module 220 having a lower head portion 228 substantially corresponding to the shape of the stackable inter-engaging bricks. The lower head 228 could be used for both individual mortarless stackable inter-engaging bricks 1 and mortarless splittable stackable inter-engaging bricks 1 . However, for mortarless splittable stackable inter-engaging bricks 1 , a different head without any void 240 separating both portions of the head 228 a and 228 b would be preferred.
As such, the present invention typically allows one molding block and molding cavities to be used for various king of stackable inter-engaging bricks.
Referring to FIG. 23 , different types of dogs are shown securing a separating plate 111 . The dogs shown in this embodiment each comprise two dog securing element or fasteners 150 , 152 . The various type of dogs 130 , 132 , 134 , 140 , 142 , 144 also comprise at least one indentation 180 mating the plate 111 or elongated “v” shaped inducing member 120 .
Referring to FIGS. 25-31 , in the present embodiment, is shown an exemplary separating plate 111 having upper 112 , 115 and lower 113 , 114 indentation to mate with the securing dogs 130 , 132 , 134 , 140 , 142 , 144 . Also shown in the FIGS. 25 and 26 are texture elements of the plate 195 to mold various design in the bricks.
Understandably, one mold may use various or identical separating plates 111 . Using identical plates 111 will result in identical stackable inter-engaging brinks whereas using different plates 111 will result in bricks having different designs.
Now referring to FIG. 22 , according to one embodiment of the present invention, the separating plates 111 are tapered from top to bottom. In other words, the upper portion of the separating plates 111 is wider than the lower portion. Accordingly, the upper portion of the mold cavity 401 , the bricks are smaller than in the lower portion 402 , thus promoting easy removal of the uncured brick from the mold. The smooth, embossed or textured plates 111 may all be tapered to promote easy brick removal. For example, a taped from a ¼ inch at the upper portion to the plate to a 3/16 inches at the bottom was found to be suitable for adequate removal of the bricks form the mold. Understandably, the degree of tapering will vary with the size and material of the bricks. Referring to FIG. 25 , the upper portion 601 will preferably be wider than the lower portion 602 of the separating plates.
Although the molding equipment and method for molding stackable inter-engaging bricks with smooth or embossed face has been described with a certain degree of particularity, it is to be understood that the disclosure has been made by way of example only and that the present invention is not limited to the feature embodiment(s) described and illustrated herein, but includes all variations and modifications within the scope and spirit of the invention as hereinafter claimed.
While illustrative and presently preferred embodiments of the invention have been described in detail hereinabove, it is to be understood that the inventive concepts may be otherwise variously embodied and employed and that the appended claims are intended to be construed to include such variations except insofar as limited by the prior art.
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A molding equipment and method to mold stackable inter-engaging bricks, blocks, stones and the like and bricks, blocks, stones and the like produced therewith are disclosed. The molding equipment comprises a main structure which contains individual cavities. Each cavity preferably has a middle structure to which a brick separating element can be attached. Without the brick separating element, each cavity can form two attached splittable bricks whereas with the brick separating element attached, each cavity can hold two individual smooth or embossed face bricks. The size and shape of the stackable inter-engaging bricks is such that once out of the mold but still in an uncured form, the brick can stand on its side without falling down, being damaged, buckling or being otherwise deformed during the manufacturing process.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a National Stage entry of International Application No. PCT/JP2003/007113, filed Jun. 5, 2003, the entire specification claims and drawings of which are incorporated herewith by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a steel strip made of martensitic steel and to a production technique for a hoop for a continuously variable transmission of an automobile, which is obtained by using this steel strip, and specifically relates to a technology which produces the hoop for a continuously variable transmission with precise size and shape in a simple manner.
2. Description of the Related Art
A hoop for a continuously variable transmission of an automobile must have high-strength in use, and therefore the hoop is produced by using a high-strength material. In manufacturing the hoop, first, both ends of a steel strip, which is a flat material, are welded to each other to obtain an annular or cylindrical member. The member is then cut in a predetermined width. The member is subjected to ring rolling at a reduction of not less than 30% so as to remove irregularities of the welded portion and to provide a predetermined thickness.
As examples of a steel strip used for such a hoop for a continuously variable transmission, Japanese Patent Unexamined (KOKAI) Publication No. 59-80772 proposes to use a maraging steel. Japanese Patent Unexamined (KOKAI) Publication No. 2000-63998 proposes to use a high-strength metastable austenite stainless steel. Japanese Patent Unexamined (KOKAI) Publication No. 2001-172746 proposes to use a high-strength strain induced martensitic steel.
When the maraging steel is used, a high-strength hoop is obtained by rolling, performing a solution treatment for obtaining a uniform rolled structure, and aging. The solution treatment is performed at about 800° C. to 900° C. However, contraction and expansion with transformation in heating and cooling are repeated since the martensite reverse transformation point of the maraging steel is 600° C. to 800° C. Therefore, shape changes such as bending and swells in the width-direction may occur after the solution treatment even if the hoop is rolled in a precise size and shape.
Therefore, changes in size and shape cause by the solution treatment must be corrected in order to obtain precise size and shape as a hoop for a continuously variable transmission of automobile. As a method for obtaining a precise size and shape, for example, Japanese Patent Unexamined (KOKAI) Publication No. 11-173385 proposes to use a heat treatment, and Japanese Patent Unexamined (KOKAI) Publication No. 2001-105050 proposes to apply plastic deformation in cold working. However, considerable labor is required in the above-described method.
When the above described strong metastable austenite stainless steel is used, solution treatment after rolling is not required. Even if aging is required, it can be performed at a temperature of about 400° C. to 500° C., which is not more than the transformation temperature. Therefore, in this case, changes in the size and shape caused by the heat treatment are not significantly observed. Accordingly, a precise product can be obtained, if precise size and shape are obtained by rolling.
However, when conventional metastable austenite type steels described in Japanese Patent Unexamined (KOKAI) Publication No. 2000-63998 or Japanese Patent Unexamined (KOKAI) Publication No. 2001-172746 are used, work hardening in rolling is very large. Therefore, in this case, precise control of plate thickness or circumferential length are difficult, and precise size and shape when used as a hoop for a continuously variable transmission of automobile cannot be obtained.
SUMMARY OF THE INVENTION
Therefore, an object of the present invention is to provide a steel strip made of martensitic steel and a production technique for a hoop for a continuously variable transmission of an automobile obtained by using this steel strip, in which manufacturing is simply performed while yielding precise size and shape of the hoop.
The present invention provides a steel strip made of martensitic steel, the steel strip is characterized in that C+N is not more than 0.12 wt %, Si is not more than 1 wt %, Mn is not more than 7 wt %, Ni is 2 to 24 wt %, Cr is 2 to 16 wt %, Mo is not more than 2.5 wt %, and Ni-Bal value and Ms value defined by the following equations shown by weight percentage of each composition are respectively Ni-Bal≧1.2, Ms≧−28.
Ni-Bal=Ni+0.5Mn+30(C+N)−1.1(Cr+1.5Si)+8.2
Ms=502−810C−1230N−13Mn−30Ni−12Cr−54Cu−46Mo
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a relationship between Ni segregation ratio and Ni-Bal value in a welded portion.
FIG. 2 shows a relationship between change of Mn amount (wt %) and Mn content (wt %) before and after laser welding.
FIG. 3 shows a relationship between work hardening amount (ÄHv) in 30% rolling and martensite rate (%) after annealing steel strip.
FIG. 4 shows a relationship between martensite rate (%) after annealing the steel strip and Ms value (° C.).
FIG. 5 shows a relationship between hardness (Hv) and C+N content (wt %) of a steel strip in which martensite rate is not less than 30% in a condition of annealing.
FIG. 6 shows a relationship between surface hardness (Hv) after nitriding and Cr content (wt %).
FIG. 7 shows a relationship between age hardening amount (ΔHv) which is the hardness difference before and after aging at 450° C. and martensite rate (%) after 50% rolling.
FIG. 8 shows a relationship between martensite rate (%) after 30% rolling and Md 30 value (C).
FIG. 9 shows a series of manufacturing processes in which a product hoop is produced from a steel strip.
FIG. 10 is a sectional view showing a product hoop after aging.
FIG. 11 is a side elevation showing a fatigue strength test apparatus of a product hoop.
FIG. 12 shows a relationship between tensile strength (N) and fatigue life (times) relating to a fatigue strength test of a product hoop.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the following, reasons for limitations concerned with characteristics of the present invention are explained in detail.
1. Reasons for Limitations Concerned with Content of Basic Compositions
When a solidification structure of Ni—Cr system steel is examined, a Schaeffler diagram is generally used. In a solidification process for an alloy, an austenite crystallizes at an initial stage, and a ferrite may be formed according to composition designs. A ferrite former (for example, Mo) is concentrated in a ä ferrite portion and an austenite former (for example, Ni) is concentrated in an austenite portion. Therefore, segregation is undesirably produced in the composition. Specifically, in a fatigue strength member which is welded like the present invention, the segregation concerning the composition must be suppressed as much as possible so as to obtain a uniform structure.
Based on such knowledge, composition designs in which the ferrite forming area is avoided in a Schaeffler diagram are required. This condition is formulated in accordance with the Schaeffler diagram as follows.
Ni equivalent>1.125(Cr equivalent−8)
(Ni equivalent=Ni+30C+0.5Mn,
C equivalent=Cr+Mo+1.5Si+0.5Nb)
In the present invention, workability is remarkably improved by forming martensite with small work hardening in an annealing condition such as described hereinafter. Therefore, in order to form the initial martensite, setting the composition which corresponds to the martensite forming area in the Schaeffler diagram is required. This condition is formulated in accordance with the Schaeffler diagram as follows.
Ni equivalent<−0.749(Cr equivalent−31.5)
(Ni equivalent=Ni+30C+0.5Mn,
C equivalent=Cr+Mo+1.5Si+0.5Nb)
Then, Ni is a stabilizing element for austenite, and a condition for forming martensite is that Ni equivalent is not more than 24 in the Schaeffler diagram. Therefore, the upper limit of the Ni content is 24 wt %. Cr is a strengthening element and a ferrite forming element. A condition for forming martensite is that the Cr equivalent is not more than 16 in the Schaeffler diagram. Therefore, the upper limit of Cr content is 16 wt %. The above-mentioned effects concerned with Ni and Cr respectively decrease and ferrite is formed, when the contents of both elements are not more than 2 wt %. Therefore, lower limits of contents for both elements are 2 wt %. These composition ranges are necessary conditions. In order to set a composition range for forming a mainly martensitic structure with high workability, additional limits are required.
2. Reasons for Limitations of Si and Mo Contents.
Si is an inevitable element for steel making processes. However, Si inhibits rolling characteristic and promotes formation of oxides in welding. Therefore, Si content is not more than 1 wt %. Mo is a stabilizing element for ferrite, and can be added so as to adjust austenite amount or martensite amount. However, ferrite is formed by excessive addition of Mo. Therefore, Mo content is not more than 2.5 wt %.
3. Reason for Limitation of Ni-Bal Value
In the Schaeffler diagram, the necessary condition of composition in which ferrite are not formed is mentioned above. More detailed reasons for limitations concerning the composition range are explained hereinafter. As mentioned above, the segregation in composition is formed when a welded portion separates into two phases of the ä ferrite portion and the austenite portion in welding. When a segregation is formed in welding, it is very difficult to remove the segregation in subsequent processes. As a result, uniformity of the structure cannot be obtained, and the fatigue strength decreases. Therefore, it is required to limit the Ni-Bal value defined by the following equations shown by weight percentage of each composition. The Ni-Bal value shows appearance characteristics of the austenite structure in solidification. If the Ni-Bal value is not more than 0, the appearance rate of the ferrite is large, and if it is not less than 0, appearance rate of the austenite is large.
Ni-Bal=Ni+0.5Mn+30(C+N)−1.1(Cr+1.5Si)+8.2
FIG. 1 shows a relationship between the Ni segregation ratio of the weld portion (data in Table 2 described hereinafter) and the Ni-Bal value (data in Table 2 similarly described hereinafter). The segregation ratio is defined as follows.
segregation ratio= A max/ A min
Amax is the maximum count of Ni characteristic X-ray by EPMA line analysis, and Amin is the minimum count of Ni characteristic X-ray by the EPMA line analysis.
As shown in FIG. 1 , the Ni segregation ratio is rapidly increased when the Ni-Bal value is less than 1.2. This is because the solidification structure separates into two phases of austenite and ferrite, thereby causing the Ni segregation. However, when the Ni-Bal value is not less than 5, the segregation ratio is very near to 1. Therefore, the Ni-Bal value was set to be not less than 1.2 by the present inventor. It is more preferable that the Ni-Bal value be set to be not less than 5.
4. Reason for Limitation of Mn Content
A steel strip of the present invention contains Mn so as to adjust the austenite amount or martensite amount. Mn may evaporate in welding the steel strip when the Mn content is large, since the vapor pressure of Mn is high. FIG. 2 shows a relationship between change in Mn amount before and after laser welding (wt %) (data in Table 2 described hereinafter) and Mn content (wt %) (data in Table 1 described hereinafter). The above change in Mn amount was measured by EPMA. As shown in FIG. 2 , the Mn amount rapidly decreases when the Mn content is more than 7 wt %. In the steel strip used for the hoop for a continuously variable transmission of an automobile, characteristics including welded portion must be considered. Therefore, the inventors set the Mn content to be not more than 7 wt % in order to obtain a stabilized composition system even after the welding.
5. Reason for Limitation of Ms Value
When a hoop for a continuously variable transmission of an automobile is produced by using a steel strip of the present invention, work hardening occurs in rolling. The work hardening is caused by formation of strain induced martensite and work hardening of austenite. However, when the martensite structure exists from an initial stage, it is difficult to harden the martensite. FIG. 3 shows a relationship between work hardening amount (ÄHv) in 30% rolling (data in Table 2 described hereinafter) and martensite rate (%) after annealing steel strip (data in Table 2 similarly described hereinafter). The martensite rate is defined by peak intensity ratio of X-ray diffraction. As shown in FIG. 3 , the work hardening amount decreases as the martensite rate increases. The work hardening amount can be stably decreased if the martensite rate is not less than 30%. This fact means that the workability improves as the martensite rate increases.
The martensite rate (%) after annealing depends on the Ms value which is defined by the following equation shown by weight percentage of each composition.
Ms=502−810C−1230N−13Mn−30Ni−12Cr−54Cu−46Mo
The Ms value is an empirical formula which shows a temperature (° C.) in which 50% martensitic transformation by volume ratio is realized. FIG. 4 shows a relationship between martensite rate (%) after annealing the steel strip (data in Table 2 described hereinafter) and Ms value (° C.) (data in Table 2 similarly described hereinafter). As shown in FIG. 4 , the martensite rate can be not less than 60% when the Ms value is not less than −28° C., and the martensite rate can be reliably not less than 80% when the Ms value is not less than −7° C. Then, the present inventors set the Ms value not less than −28° C. so as to stably decrease the work hardening amount. It is more preferable that the Ms value be not less than −7° C.
6. Reason for Limitation of Composition Range of C+N
As mentioned above, work hardening decreases as the martensite rate increases. However, the workability is not excellent when the initial hardness is high. The initial hardness of martensite depends on the amounts of carbon and nitrogen which are included in the solid solution. FIG. 5 shows a relationship between hardness (Hv) of a steel strip in which the martensite rate is not less than 30% in a condition of annealing (data in Table 2 described hereinafter) and C+N content (wt %) (data in Table 2 similarly described hereinafter). As shown in FIG. 5 , the above mentioned hardness extremely increases when the C+N content is more than 0.12 wt %. Therefore, the C+N content must be not more than 0.12 wt % in order to obtain excellent workability based on the initial hardness. Therefore, the inventors set the C+N content to be not more than 0.12 wt % in order to obtain excellent workability based on the initial hardness.
Therefore, according to the present invention, it is provided with a steel strip made of the martensitic steel in which the hoop for continuously variable transmission can be easily produced and the precise size and shape of the hoop can be obtained based on the above-mentioned reason for limitation, without performing a heat treatment described in Japanese Patent Unexamined (KOKAI) Publication No. 11-173385 and the cold plastic deformation described in Japanese Patent Unexamined (KOKAI) Publication No. 13-105050. Preferred embodiments and production method of the present invention are explained hereinafter.
In the invention, the Cr content is preferably 2 to 10 wt %. Cr: 2 to 10 wt %
Nitriding is generally performed when wear resistance is improved by increasing surface hardness of a rolled hoop or when fatigue strength is improved. Specifically, concerning the hoop for a continuously variable transmission of an automobile, a nitride layer called a “white layer” on the surface is observed by an optical microscope. The surface is embrittled when the surface hardness is not less than 1000 in Hv. The hardened layer depth by the nitriding also decreases, and therefore, the fatigue strength decreases. In the Ni—Cr system steel, the surface hardness is extremely high and the white layer is easily formed. In order to avoid such failure, it is effective to decrease Cr which easily forms the nitride as much as possible. FIG. 6 shows a relationship between surface hardness (Hv) after nitriding (data in Table 2 described hereinafter) and Cr content (wt %) (data in Table 1 described hereinafter). When the Cr content is not more than 10 wt %, surface hardness can be decreased, and this is extremely effective for members such as a hoop for a continuously variable transmission of an automobile, which requires curvature fatigue characteristics. The hardened layer depth can be increased because the surface hardness can be relatively decreased, and this fact is also effective for improvement of the fatigue characteristics.
The Cr content is set to be 2 to 10 wt % by the present inventors, based on the above-mentioned knowledge.
Md30 value defined by following equations shown by weight percentage of each composition is set to be not less than 100.
Md30=497−462(C+N)−9.2Si−8.1Mn
−13.7Cr−20(Ni+Cu)−18.5Mo
Md30≧100
As mentioned above, ring rolling which enables precise working can be performed by using a material with good workability. However, when a hoop for continuously variable transmission of an automobile is produced, strengthening by using aging is generally performed in order to additionally improve strength. As examples of providing aging characteristics, an example in which Ti and Al are added (for example, Japanese Patent Unexamined (KOKAI) Publication No. 59-170244), an example in which N is added (for example, Japanese Patent Unexamined (KOKAI) Publication No. 56-139663), an example in which Cu is added (for example, Japanese Patent Unexamined (KOKAI) Publication No. 56-139663), an example in which Si is added (for example, Japanese Patent Unexamined (KOKAI) Publication No. 6-33195), and an example in which Ni and Mn are arranged (for example, “Concerning age hardening characteristics of Fe—Ni—Mn martensitic alloy”, Minoru Tanaka etc., a magazine published by The Japan Institute of Metals, Vol. 31 (1967), No. 9, P. 1075˜1081) may be mentioned. Ti, Al, and Si are effective as aging elements. However, these elements easily form non-metallic inclusions such as oxides and nitrides, and they are not preferable for producing products in which fatigue strength is required, as in the present invention. Therefore, addition of N and Cu as aging elements or adjustment of Ni and Mn is preferable.
Aging must be performed at a temperature of not more than the transformation temperature in order to age without decreasing the size precision. In steel mainly made of martensite as in the present invention, the aging must be performed at not more than 600° C. since the martensite inverse transformation temperature is 600 to 800° C. It is important to control a structure after the rolling in order to obtain excellent aging characteristics in such a temperature range. Because packing rate of martensite is lower than that of austenite since the crystal structure of the martensite is bct and the crystal structure of the austenite is fcc, and therefore, when the martensite amount is large, the diffusion amount of the aging elements is large, to improve the aging characteristics.
FIG. 7 shows a relationship between age hardening amount (ΔHv) which is the hardness difference before and after aging at 450° C. (data in Table 2 described hereinafter) and martensite rate (%) after 50% rolling (data in Table 2 similarly described hereinafter). As shown in FIG. 7 , a correlation between the age hardening amount and the martensite rate is observed, the age hardening can be performed when the martensite rate after the rolling is not less than 70%. In particular, remarkable age hardening amount is observed when the martensite rate is not less than 90%.
The martensite rate after the rolling depends on Md30 value defined by the following equation shown by weight percentage of each composition.
Md30=497−462(C+N)−9.2Si−8.1Mn
−13.7Cr−20(Ni+Cu)−18.5Mo
The Md30 value is an empirical formula which shows a temperature (C) in which 60% martensitic transformation at volume ratio is realized when 30% tensile deformation is given. FIG. 8 shows a relationship between martensite rate (%) after 30% rolling (data in Table 2 described hereinafter) and Md 30 value (° C.) (data in Table 2 similarly described hereinafter). When the rolling rate is 30%, the above mentioned martensite rate can be not less than 70% if the Md30 value is not less than 100° C., the martensite rate can be reliably not less than 90% if the Md30 value is not less than 140° C. Therefore, the Md30 value is suitably not less than 100° C., and it is more suitably not less than 140° C.
The steel strip of the present invention was explained above, and production methods for a hoop for a continuously variable transmission of an automobile of the present invention, obtained by using these steel strips, will be explained in detail hereinafter.
The present invention provides a production method for a hoop for a continuously variable transmission of an automobile in which cold rolling of not less than 30% is performed on a steel strip made of martensitic steel in which C+N is not more than 0.12 wt %, Si is not more than 1 wt %, Mn is not more than 7 wt %, Ni is 2 to 24 wt %, Cr is 2 to 16 wt %, Mo is not more than 2.5 wt %, and Ni-Bal≧1.2, Ms≧−28. According to the method, the hoop of precise size and shape can be produced by producing the hoop by performing general cold rolling on a steel strip produced under the above mentioned various reasons for limitations, and this manufacturing can be simply performed without separately performing a heat treatment and a plastic deformation in the cold as in a conventional technology.
The present invention also provides another production method for a hoop for a continuously variable transmission of an automobile in which cold rolling of not less than 30% is performed on a steel strip in which C+N is not more than 0.12 wt %, Si is not more than 1 wt %, Mn is not more than 7 wt %, Ni is 2 to 24 wt %, Cr is 2 to 16 wt %, Mo is not more than 2.5 wt %, and Ni-Bal≧1.2, Ms≧−28, Md30≧100, and afterwards, the steel strip is aged at a temperature of not more than a martensite inverse transformation temperature. According to the method, a hoop with excellent strength based on the aging can be produced without decreasing dimensional accuracy, specifically by setting the Md30 value of the steel strip to be not less than 100° C. and by aging at a temperature of not more than an martensite inverse transformation temperature.
Moreover, the present invention also provides another production method for a hoop for a continuously variable transmission of an automobile in which cold rolling of not less than 30% is performed on a steel strip in which C+N is not more than 0.12 wt %, Si is not more than 1 wt %, Mn is not more than 7 wt %, Ni is 2 to 24 wt %, Cr is 2 to 10 wt %, Mo is not more than 2.5 wt %, and Ni-Bal≧1.2, Ms≧−28, and afterwards, the steel strip is nitrified. According to the method, the surface hardness of the hoop can decrease specifically by setting the Cr content in the steel strip to be 2 to 10 wt % and by nitriding. This production method is extremely effective for members, which requires curvature fatigue characteristics, such as a hoop for a continuously variable transmission of an automobile.
Furthermore, the present invention also provides another production method for a hoop for a continuously variable transmission of an automobile in which cold rolling of not less than 30% is performed on a steel strip in which C+N is not more than 0.12 wt %, Si is not more than 1 wt %, Mn is not more than 7 wt %, Ni is 2 to 24 wt %, Cr is 2 to 16 wt %, Mo is not more than 2.5 wt %, and Ni-Bal≧1.2, Ms≧−28, Md30≧100, and afterwards, the steel strip is aged at a temperature of not more than the martensite inverse transformation temperature and is nitrified. According to the method, a hoop with excellent strength based on the aging can be produced without decreasing the dimensional accuracy, by setting Md30 value of the steel strip to be not less than 100° C. and by aging at the temperature of not more than the martensite inverse transformation temperature. At the same time, a hoop with excellent wear resistance and fatigue strength can be produced by nitriding.
EXAMPLES
Hereinafter, the present invention will be explained in further detail by examples.
Table 1 respectively shows practical examples 1 to 4 according to the present invention and comparative examples 1 to 15 according to the conventional technology, concerned with composition of steel strip as a material of a hoop for a continuously variable transmission of an automobile. After steel strips 250 mm wide and 0.4 mm thick, having each composition shown in the Table 1 were annealed, 30% rolling and 50% rolling were performed in order, and aging was performed on the 50% rolled products by the present inventor. After steel strips 250 mm wide and 0.4 mm thick, having each of the compositions shown in Table 1 were annealed, 30% rolling and 50% rolling were performed in order, and nitriding was performed on the 50% rolled products by the present inventor. Table 2 shows results concerned with hardness (Hv) after 50% rolling and aging each steel strip, hardening amount (ÄHv) after aging, and surface hardness (Hv) after nitriding each steel strip. The other data shown together in Table 2 are data with regard to parameters of vertical line or horizontal axis in graphs of the steel strips shown in FIG. 1 to FIG. 8 .
TABLE 1
(wt %: balance of substantially Fe)
C
Si
Mn
Cr
Ni
Mo
Cu
N
Nb
practical example 1
0.045
0.45
5.48
4.98
9.57
1.02
0.00
0.023
0.11
practical example 2
0.032
0.45
5.43
10.34
4.59
1.03
0.00
0.020
0.00
practical example 3
0.038
0.46
5.39
4.91
7.17
2.01
0.00
0.022
0.10
practical example 4
0.042
0.45
5.47
5.15
5.94
1.00
0.00
0.022
0.00
comparative example 1
0.058
1.12
0.35
15.26
3.59
0.22
1.58
0.089
0.06
comparative example 2
0.054
1.57
0.98
15.61
4.03
0.21
1.98
0.112
0.06
comparative example 3
0.069
0.89
7.23
15.58
4.22
0.19
0.00
0.130
0.06
comparative example 4
0.054
1.27
2.89
15.84
4.23
0.19
0.00
0.136
0.06
comparative example 5
0.054
1.85
1.55
15.07
4.01
0.21
0.00
0.153
0.06
comparative example 6
0.042
0.45
7.56
13.91
6.01
1.02
0.00
0.021
0.09
comparative example 7
0.054
2.54
1.91
15.62
4.01
1.05
0.00
0.099
0.07
comparative example 8
0.046
4.52
0.33
15.17
4.02
1.57
0.00
0.075
0.06
comparative example 9
0.075
0.57
6.91
14.11
3.44
2.10
0.00
0.090
0.09
comparative example 10
0.081
0.25
0.65
16.88
4.21
2.51
0.00
0.090
0.00
comparative example 11
0.020
0.51
1.53
17.30
5.35
0.00
0.00
0.167
0.06
comparative example 12
0.019
0.52
1.52
17.29
5.91
0.00
0.00
0.126
0.06
comparative example 13
0.021
0.51
1.55
17.21
6.23
0.00
0.00
0.171
0.07
comparative example 14
0.022
0.52
1.52
17.19
6.98
0.00
0.00
0.098
0.06
comparative example 15
0.021
0.51
1.53
17.09
8.12
0.00
0.00
0.044
0.07
TABLE 2
change of Mn
C + N
Ms
Md30
amount before
Ni segregation
martensite rate(%)
content
value
value
Ni-Bal
and after laser
ratio in welded
30%
50%
(wt %)
(° C.)
(° C.)
value
welding(wt %)
portion
annealing
rolling
rolling
practical
0.068
−28
139
16.3
−0.6
1.13
62
95
100
example 1
practical
0.052
72
172
5.0
−0.3
1.14
83
97
100
example 2
practical
0.060
8
174
13.7
0.1
1.14
90
97
100
example 3
practical
0.064
84
211
12.4
−0.2
1.15
100
100
100
example 4
comparative
0.147
−45
131
−2.3
0.0
1.86
50
76
88
example 1
comparative
0.166
−117
100
−2.1
0.0
1.81
35
74
84
example 2
comparative
0.199
−130
37
3.4
−1.3
1.36
1
56
59
example 3
comparative
0.190
−72
69
0.1
−0.2
1.63
2
58
63
example 4
comparative
0.207
−61
81
−0.4
0.0
1.68
31
65
71
example 5
comparative
0.063
−50
73
3.8
−3.0
1.31
37
84
90
example 6
comparative
0.153
−44
74
−3.6
0.0
2.14
22
61
68
example 7
comparative
0.121
−7
80
−8.1
0.0
2.18
82
84
87
example 8
comparative
0.165
−128
59
3.6
−0.5
1.23
25
75
88
example 9
comparative
0.171
−127
49
−1.1
0.0
1.87
24
63
85
example 10
comparative
0.187
−108
50
0.1
0.0
1.72
45
75
81
example 11
comparative
0.145
−73
58
−0.7
−0.1
1.85
27
73
91
example 12
comparative
0.192
−139
31
1.2
−0.1
1.36
39
65
81
example 13
comparative
0.120
−72
49
−0.2
−0.1
1.86
20
70
87
example 14
comparative
0.065
−38
53
−0.6
0.1
1.78
15
57
90
example 15
work hardening
hardness
age
surface
hardness(Hv)
amount (Δ Hv)
after 50%
hardening
handness
30%
50%
30%
50%
rolling and
amount
after
annealing
rolling
rolling
rolling
rolling
aging(Hv)
(Δ Hv)
nitriding(Hv)
practical
289
419
450
130
161
623
173
890
example 1
practical
258
388
450
130
192
623
173
937
example 2
practical
303
375
392
72
89
592
200
865
example 3
practical
315
367
391
52
76
517
126
912
example 4
comparative
410
466
487
56
77
538
51
1126
example 1
comparative
434
489
507
55
73
549
42
1163
example 2
comparative
274
569
610
295
336
614
4
1219
example 3
comparative
346
536
552
190
206
562
10
1136
example 4
comparative
459
547
572
88
113
607
35
1186
example 5
comparative
248
405
484
157
236
592
108
1122
example 6
comparative
282
507
535
225
253
540
5
1140
example 7
comparative
321
451
487
130
166
563
76
1092
example 8
comparative
225
532
551
307
326
635
84
1080
example 9
comparative
280
450
530
170
250
585
55
1166
example 10
comparative
416
485
508
69
92
602
94
1136
example 11
comparative
287
440
455
153
168
565
110
1227
example 12
comparative
415
469
508
54
93
566
58
1194
example 13
comparative
272
438
459
166
187
557
98
1171
example 14
comparative
231
401
426
170
195
520
94
1198
example 15
According to a manufacturing process shown in FIG. 9 , steel strips with each composition of practical example 2 and comparative example 7 were processed into hoops for a continuously variable transmission of an automobile. In each hoop, the thickness was 0.18 mm, the width was 9 mm, and the circumferential length was 600 mm. A hoop with the composition of practical example 2 was practical example 5, a hoop with the composition of comparative example 7 was comparative example 16, and Table 3 respectively shows hardness before and after the aging after the rolling of each hoop.
TABLE 3
(Hv)
before aging
after aging
practical example 5
448~465
615~624
comparative example 16
609~618
620~631
In comparative example 16, since the martensite amount in the annealing condition is small, the work hardening amount is large, and since the martensite forming amount after the rolling is also small, the hardening is hardly observed even if the aging is performed. In contrast, in practical example 5, hardness after the rolling is drastically lower in comparison with that of comparative example 16, however, hardness after the aging is equivalent to that of comparative example 16.
FIG. 10 is a sectional view of a product hoop after the aging, and Δt in FIG. 10 shows dimensional accuracy of the hoop. As a result of measurement, Δt was 3 to 12 μm in comparative example 16 while Δt was not more than 2 μm in practical example 5. The circumferential length accuracy of the hoops was also measured although it is not shown. According to the result of the measurement, the accuracy in practical example 5 was about ±10 μm which is excellent while the accuracy in comparative example 16 was about ±50 μm.
According to these results, comparative example 16 in which the work hardening amount is large is not preferable for a hoop for a continuously variable transmission of an automobile since sufficient dimensional accuracy for use by laminating cannot be obtained. In practical example 5, dimensional accuracy is extremely superior by small work hardening amount. Therefore, practical example 5 is preferable for a hoop for a continuously variable transmission of an automobile since sufficient dimensional accuracy for use by laminating can be obtained.
Fatigue strength of a hoop is an important characteristic in actually using the hoop for a continuously variable transmission of an automobile. Then, as shown by a side view in FIG. 11 , fatigue lives of hoop 12 of various tensile strength F were compared by a fatigue strength test device comprised of 2 rollers 10 and 11 . Repeatedly bended time to rupture was fatigue life. The fatigue life was defined by multiplying rotated times of hoop 12 by 2. The test was continued until whether the hoop was broken or fatigue life reached 10 8 times. This test was performed by using rollers of 55 mm diameter and by setting the rotational rate to be 6000 rpm. FIG. 12 shows the result. The plot shown in FIG. 12 concerns practical example 5 and comparative example 16. As shown in FIG. 12 , practical example 5 has fatigue lives which are equivalent to those of comparative example 16, and practical example 5 has sufficient fatigue characteristics in use for a continuously variable transmission of an automobile.
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A steel strip made of martensitic steel contains C+N at not more than 0.12 wt %, Si at not more than 1 wt %, Mn at not more than 7 wt %, Ni at 2 to 24 wt %, Cr at 2 to 16 wt %, Mo at not more than 2.5 wt %, and Ni-Bal value and Ms value defined by the following equations shown by weight percentage of each composition are respectively Ni-Bal≧1.2, Ms≧−28.
Ni-Bal=Ni+0.5Mn+30(C+N)−1.1(Cr+1.5Si)+8.2
Ms=502−810C 1230N−13Mn−30Ni−12Cr−54Cu−46Mo
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a conveyor installation for hanging items, in particular for pieces of clothing hanging on hangers, comprising a transport rail with a bearing; a drive chain which is guided in said bearing and is drivable in a direction of conveyance and which comprises upper coupling members located at a lower side of said drive chain; retaining members for said hanging items, which retaining members are displaceably mounted in the direction of conveyance below the drive chain by means of rollers, with the upper ends of the retaining members being provided with lower coupling members, and with in each case one upper coupling member and one lower coupling member forming a drive connection of the drive chain with a retaining member for conveyance of said retaining member in the direction of conveyance.
2. Background Art
A conveyor installation of this type is known from DE 10 2005 006 455 A1 where a strand of a circulating drive chain, which is drivable in a transport direction, is arranged in a transport rail. The drive chain is embodied with downwardly protruding bolts. Below the drive chain, retaining means are provided which are mounted on rollers in the transport rail, the lower end of which being provided with an opening for receiving the hook of a hanger with a piece of clothing. Each of the retaining means is provided with lugs at their upper ends which project upwards between adjacent bolts so as to form a positive drive connection between the drive chain and the retaining means. The conveyor installation, which is referred to as transport system, comprises no device which allows retaining means to accumulate while the drive chain is being driven continuously.
EP 0 623497 B1 discloses an accumulatable conveyor where a carrier for items to be transported is mounted on a carrier rail via rotatably drivable rollers, the carrier being drivable in a direction of conveyance by a traction means in the form of a friction belt which is also mounted to the transport rail. In order for carriers to accumulate in a desired manner, a stopping device comprising a retaining finger is provided, which retaining finger is extendable into the movement area of the carriers and acts on a spreader device mounted to the carrier, thus causing the carrier to be pivoted laterally and therefore to be lifted off the friction belt.
The disadvantage of this arrangement is that lifting succeeding carriers off the friction belt requires the spreading devices, which are assigned to the individual carriers, to come into direct contact with each other. Lifting the carriers off the friction belt, in other words bringing about a state in which the carrier is not driven, is however impossible if the transported items have a dimension in the direction of conveyance, in other words a thickness, which is greater than the distance of carriers which are in close contact with each other. This results in a frictional drive connection between stopped carriers and the continuously running friction belt, which in turn results in excessive wear and undesirable downtimes required to perform repair works at the conveyor installation. Another disadvantage is that lifting the carrier off the friction belt is performed by pivoting the carrier, which causes the elastically deformable spreading devices of plastic material to be subjected to inertial forces depending on the mass of the trans-ported items, thus resulting in premature wear.
DE 296 21 786 U1 discloses a pawl conveyor where a traction means, which is drivable in a direction of conveyance, is provided with pivotable pawls having a hook-shaped end allowing the pawls to displaceably seize and convey hangers loaded with items to be transported along a rail. The particular shape of the pawls allows hangers to accumulate by means of a device which lifts a pawl by means of a stopping member which comes into contact with the lower side of the pawl and thus disengages the hook-shaped end from the hanger and causes succeeding pawls to be lifted by the hanger which has just been brought to a standstill. One disadvantage of this conveyor is that a continuous accumulation of hangers is only possible if particular design specifications have been determined for the dimensions of the pawls and accordingly, the thickness of the transported items. Another particular disadvantage is that the hook-shaped ends of the pawls may be subjected to an excessive load during an accumulation process if pivoting a pawl is impossible due to a previously transported item having an excessive thickness. The last-mentioned disadvantage is to be remedied by a pawl designed according to DE 299 15 523 U1.
DE 40 17 821 C2 discloses a conveyor installation where carriages for items to be transported are moved along guide rails by means of bristles which are arranged, in the form of drivers, on a driven belt strand and come into frictional contact with a portion of the carriages. If it is desired to accumulate transported items, the carriages are stopped while the bristles keep on moving so that a residual frictional force is exerted on the carriages. In this conveyor installation, the bristles are to act as a slip coupling which forms a releasable drive connection independently of other criteria and allows continuous accumulation of transported items independently of their thickness. In this type of drive connection where the drivers come into engagement with the bristles and are moved relative to each other during an accumulation process, the bristles are subjected to a considerable amount of wear. This results in downtimes required to replace worn-out bristles by new ones.
An overhead conveyor installation is disclosed in DE 297 09 547 U1 where hanger carriers, which are mounted on rollers and are driven by a conveyor chain located thereabove, are movable along a main conveyance path. To this end, the conveyor chain is provided with drivers which are mounted thereto at regular distances and cooperate with rigid coupling members at the hanger carriers. A switch station allows the hanger carriers to be moved to the side, i.e. from the main conveyance path to an accumulation path, which causes the drive connection to be released. The diverted hanger carriers are then driven by a separate drive device. In the region of an accumulation path, a stopping device referred to as accumulation stop is provided where hanger carriers accumulate. As it is required to install a separate, complex drive device for driving the hanger carriers to be accumulated along the accumulation path, the design of the overhead conveyor installation is extremely complicated.
SUMMARY OF THE INVENTION
It is the object of the invention to develop the system of the generic type in such a way as to achieve a reliable and substantially wear-free functioning of the system for conveying and continuously accumulating items independently of their properties.
This object is achieved in the conveyor installation for hanging items, in particular for pieces of clothing hanging on hangers, comprising a transport rail with a bearing; a drive chain which is guided in said bearing and is drivable in a direction of conveyance and which comprises upper coupling members located at a lower side of said drive chain; retaining members for said hanging items, which retaining members are displaceably mounted in the direction of conveyance below the drive chain by means of rollers, with the upper ends of the retaining members being provided with lower coupling members, and with in each case one upper coupling member and one lower coupling member forming a drive connection of the drive chain with a retaining member for conveyance of said retaining member in the direction of conveyance, wherein the bearing is designed such that the drive chain is displaceable upwards by a distance a in a direction opposite to gravity; the coupling members are designed such that the transmission of a drive force of the drive chain takes place via a normal force component and a lifting force component which is opposite to gravity, with a line of action of the normal force component forming an angle W with a line of action of the drive force of the drive chain, wherein the line of action is parallel to the direction of conveyance; and an actuable stopping device is provided for accumulating retaining members, with the lifting force component causing the upper coupling member to be lifted upwards by a displacement path v for releasing the drive connection, with v<a.
By means of the invention, a substantially wear-free positive or non-positive drive connection between the retaining members, which carry items to be transported, and the drive chain is achieved with a lowest-possible number of simple components. A particular advantage is that the drive chain is a standardized mass production component which is available on the market at low prices but forms an essential feature of the invention by the arrangement of a single component. Furthermore, the subject matter of the invention is distinguished by the fact that forces occurring during an accumulation process are independent of the mass of the trans-ported item and that a continuous accumulation of transported items is possible independently of the dimensions of the transported items.
A conveyor installation wherein the transport rail is substantially horizontal in a region of the stopping device; a conveyor installation wherein seen in the direction of conveyance, the upper coupling member comprises a front boundary surface which runs obliquely to the direction of conveyance and forms an angle W 1 with the line of action of the driving force of the drive chain, with 0°<W<90°; and a conveyor installation wherein 90°>W>0° applies to the angle W result in advantageous force relations. The developments of the conveyor installation wherein the drive chain comprises joints which are pivotable about vertical axes and of the conveyor installation wherein the joints comprise bores which extend along the axes, with pins of the upper coupling members being received therein, result in a particularly simple and cost-saving design. A conveyor installation wherein the pins are provided with a snap fit is a simple, advantageous embodiment which allows easy mounting and, if necessary, easy replacement of a wornout coupling member by a new one. A conveyor installation wherein the upper coupling members are formed of plastics results in a cost-saving production of the upper coupling members.
Further features, advantages and details of the invention will become apparent from the ensuing description of an embodiment by means of the drawing.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a partial front view of a conveyor installation;
FIG. 2 is an enlarged sectional view of the conveyor installation along section line II-II in FIG. 1 ;
FIG. 3 is a side view of a drive chain with upper coupling members according to arrow III-III in FIG. 2 ;
FIG. 4 is a perspective view of the upper coupling member shown in FIG. 3 ;
FIG. 5 is a view of the drive chain according to arrow V in FIG. 3 ;
FIG. 6 is a an enlarged side view of the conveyor installation according to arrow III-III in FIG. 2 , with the front wall of a transport rail being broken away;
FIG. 7 is a schematic view of the conveyor installation according to the view of FIG. 6 ; and
FIG. 8 is an enlarged detail Z of FIG. 7 .
DESCRIPTION OF THE PREFERRED EMBODIMENT
A transport rail 1 is substantially horizontally mounted to a wall or a ceiling. The transport rail 1 is continuously cast from aluminium and has a box-shaped and symmetrical cross-section with a slot 3 at the lower side 2 .
The transport rail 1 has side walls 5 , 6 which extend downwards from an upper wall 4 and comprise recesses with projections arranged therein on their inner sides which face each other. Profiles made of plastics and serving as bearings 7 , 8 are in each case positively retained and firmly embedded in the recesses.
The facing rectangular ends of the bearings 7 , 8 accommodate a strand of an endless drive chain 9 with a certain amount of clearance. The drive chain 9 is drivable for circulation by means of an electric motor which is not shown in FIG. 1 . Being a conventional roller chain, the drive chain 9 comprises joints 11 which are pivotable about vertical axes 10 , with sheet metal lugs 12 being interconnected by hollow rivets 10 b which are provided with bores 10 a . The joints 11 of the drive chain 9 are designed to have a normal amount of clearance, which allows the drive chain 9 to describe a slight curve as shown by the partially curved drive chain 9 in FIG. 6 .
The drive chain 9 is arranged in the transport rail 1 in such a way that it is on the one hand guided horizontally by means of the rollers 13 which are rotatably mounted on the rivets 10 b . On the other hand, a vertical guidance is achieved in such a way that the lower sides of lugs 14 of the drive chain 9 rest on the bearings 7 , 8 due to the own weight of the drive chain 9 . Furthermore, the bearings 7 , 8 are dimensioned in such a way in the vertical direction that the drive chain 9 is mounted for displacement in a direction opposite to the direction of gravity along a distance a.
On the lower side 15 of the drive chain 9 , each chain link is provided with an upper coupling member 16 which is preferably made of plastics. The coupling member 16 is designed to have two pins 17 , 18 which are received in the bores 10 a of the hollow rivets 10 b . According to FIG. 4 , the flattened, slotted and spreaded ends form in each case a snap fit 19 by means of which the coupling members 16 are firmly secured to the drive chain 9 . The snap fits 19 allows the coupling members 16 to be easily mounted to the drive chain 9 without requiring any tooling.
Relative to a direction of conveyance 40 , the upper coupling member 16 comprises a front boundary surface 20 , a rear boundary surface 21 and a lower side 22 . A line of action 23 of a drive force F of the drive chain 9 is parallel to the lower side 22 and to the direction of conveyance 40 ( FIG. 8 ).
The front boundary surface 20 is designed in such a way that a normal n, in other words the vertical line of action of the normal force component N, to the boundary surface 20 forms an angle W with the line of action 23 of the drive force F, the angle amounting to W>0 degrees and W<90 degrees. As a result, it follows that the boundary surface 20 forms an angle W 1 >0 and W 1 <90 degrees with the lower side 22 . In the exemplary embodiment, the angles amount to W=70 degrees and W 1 =20 degrees.
The rear boundary surface 21 is mirror symmetric to the boundary surface 20 . It is however conceivable as well to design the rear boundary surface 21 in such a way as to have different angles than the front boundary surface 20 .
According to FIG. 2 , the transport rail 1 has bearing surfaces 24 , 25 on its lower side 2 on which rollers 26 , 27 are supported. These rollers 26 , 27 are rotatably mounted to an axle 28 which is an integral component of a retaining member 29 made of plastics. The retaining member 29 comprises an opening 30 with an angled web 31 that forms the lower end of the opening 30 into which a hook 32 of a hanger 33 carrying an item 34 to be trans-ported is inserted. The retaining member 29 firmly encloses the axle 28 and extends up to an upper end which is in the shape of a T-shaped projection and forms a lower coupling member 35 . The retaining member 29 is furthermore provided with a memory chip 36 for identifying the hanger 33 inserted therein. According to FIG. 2 , the lower coupling member 35 of the retaining member 29 projects into a gap 37 which is located between two adjacent upper coupling members 16 and is formed between the rear boundary surface 21 of a leading—relative to the direction of conveyance 40 —upper coupling member 16 and the directly trailing front boundary surface of a directly trailing upper coupling member 16 .
Furthermore, the transport rail 1 is provided with a stopping device 38 ( FIG. 6 ) comprising an axially displaceable, bolt-shaped stopping member 39 which is pneumatically or electrically displaceable into a rest position which provides access to the movement area of the retaining members 29 or a working position where no access is provided to the movement area of the retaining members 29 .
The functioning is as follows:
When the conveyor installation is in operation, the retaining members 29 are conveyed, whether unloaded or loaded with items, in the direction of conveyance 40 in such a way that the lower coupling members 35 of the retaining members 29 project into the gaps 37 located between adjacent upper coupling members 16 so that the two coupling members 16 , 35 come into contact with each other so as to form a drive connection in the direction of conveyance 40 . This operating state is for example outlined in FIG. 7 and shown as an enlarged detail in FIG. 8 . The lower coupling member 35 of a retaining member 29 abuts against the front boundary surface of an upper coupling member 16 .
FIG. 8 shows that if frictional forces at the point of contact of the coupling members 16 , 35 are neglected, a drive force F exerted by the drive chain 9 may be regarded as the resultant of a normal force component N and a lifting force component H; in the process of conveying items, the lifting force component H is smaller than the force which is required to lift the upper coupling member 16 , together with the proportionate own weight of the drive chain 9 , upwards from its lower position by the length of a displacement path v. The displacement path v makes up only a portion of the distance a, it is therefore smaller than the distance a.
Having initiated a desired accumulation process, in other words an accumulation of retaining members 29 independently of their loading state by activating the stopping device 38 so as to form an accumulation path, the stopping member 39 , which is axially displaced into the path of the retaining members 29 , brings the next arriving retaining member 29 to a stop. When the drive chain 9 keeps on moving, the previously observed force relations are changed in such a way that the lifting force component H increases to such an extent that the upper coupling member 16 is displaced upwards by the displacement path v together with the proportionate own weight of the drive chain 9 ( FIG. 7 ). As can be seen in FIGS. 6 and 7 , the drive chain 9 is then slightly lifted up by the displacement path v, which causes the drive chain 9 to be curved. After lifting, the upper coupling member 16 slides across the lower coupling member 35 , with the lower side 22 of the upper coupling member 16 being in contact with the lower coupling member 35 . Furthermore, it shall be noted that during conveyance, static friction is active between the two coupling members 16 , 35 while the lower dynamic friction is active during the accumulation process.
This state is outlined in FIG. 7 . When the drive chain 9 keeps on moving, resulting in the development of the accumulation path, this process of releasing the drive connection and re-engagement of coupling members 16 and 35 passing each other is repeated.
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A conveyor installation for conveying and accumulating hanging items comprises a drive chain which is mounted to a guide rail, and retaining members which are mounted on rollers below the drive chain. The retaining members—together with the items to be transported which are suspended therefrom—are conveyed by the drive chain in a direction of conveyance and, if required, stopped and accumulated by means of a stopping device, with the drive connection being released between the drive chain and the retaining members by displacing the drive chain upwards due to a particular design of coupling members arranged on the lower side of the drive chain.
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This application is a Divisional of U.S. application Ser. No. 13/014,993, filed on Jan. 27, 2011, now PAT 8653025.
FIELD OF THE INVENTION
The present invention relates to novel polyheterocyclic based compounds with both linear and macrocyclic structure, especially with tri-heterocyclic functional groups, which are highly potent and effective to inhibit the NS3 protease replication of hepatitis C virus (HCV). The invention also relates to preparation and the uses thereof as HCV inhibitors.
BACKGROUND OF THE INVENTION
Hepatitis C virus (HCV) is the major causative agent for most cases of non-A, non-B hepatitis. The virus is a single-stranded positive RNA virus in the Flaviviridae family. It includes a nucleocapsid protein (C), envelope proteins (E1 and E2), and several non-structural proteins (NS1, NS2, NS3, NS4a, NS5a, and NS5b). The NS3 protein possesses serine protease activity and is considered essential for viral replication and infectivity, and the essentiality of the NS3 protease was inferred from the fact that mutations in the yellow fever virus NS3 protease decreased viral infectivity [reference: Chamber et al, Proc. Natl. Acad. Sci. USA 87, 8898-8902 (1990).
So far, HCV infection is one of major human health problems since HCV infection leads to chronic liver disease such as cirrhosis and hepatocellular carcinoma. Due to the fact that the number of HCV infected individuals is estimated 2-15% of the world's population while no any effective vaccines or therapeutic agents are available to control or cure HCV [reference: WO 89/04669; Lavanchy, J. Viral Hepatitis, 6, 35-47 (1999); Alter, J. Hepatology, 31 (Suppl. 1), 88-91 (1999); and Alberti et al, J. Hepatology, 31 (Suppl. 1), 17-24 (1999)].
It has been demonstrated that mutations at the active site of the HCV NS3 protease completely inhibited the HCV infection in chimpanzee model [reference: Rice et al, J. Virol. 74 (4) 2046-51 (2000)]. Furthermore, the HCV NS3 serine protease has been found to facilitate proteolysis at the NS3/NS4a, NS4a/NS4b, NS4b/NS5a, NS5a/NS5b junctions and is thus responsible for generating four viral proteins during viral replication [reference: US 2003/0207861]. Consequently, the HCV NS3 serine protease enzyme is an attractive and effective target to develop new inhibitors for HCV infection. So far, there are different kinds of potential NS3 HCV protease inhibitors reported by global research institutes and pharmaceuticals, such as WO2010033466, WO2010075127, US20100003214, US20100022578, US20100029715, US20100041889, WO2009134624, WO2009010804, US20090269305, WO2008057209, WO2008057208, WO2007015787, WO2005037214, WO200218369, WO200009558, WO200009543, WO199964442, WO199907733, WO199907734, WO199950230, WO199846630, WO199817679, U.S. Pat. No. 5,990,276, Dunsdon et al, Biorg. Med. Chem. Lett. 10, 1571-1579 (2000); Llinas-Brunet et al, Biorg. Med. Chem. Lett. 10, 2267-2270 (2000); and S. LaPlante et al., Biorg. Med. Chem. Lett. 10, 2271-2274 (2000).
Currently, due to lack of immunity or remission associated with HCV infection, hepatitis caused by HCV infection is more difficult to treat comparing to other forms of hepatitis. Now, the only available anti-HCV therapies are interferon-a, interferon-a/ribavirin combination, and pegylated interferon-a. However, sustained response rates for interferon-a or interferon-a/ribavirin combination were found to be <50% and patients suffer greatly from side effects of these therapeutic agents [reference: Walker, DDT, 4, 518-529 (1999); Weiland, FEMS Microbial. Rev., 14, 279-288 (1994); and WO 02/18369]. Based on the significant importance for controlling HCV infection, the aim of the present invention is to develop more effective and better-tolerated therapeutic drugs for inhibiting HCV NS3 protease replication.
SUMMARY OF THE INVENTION
The present invention relates to two classes of novel polyheterocyclic based compounds of the following formulas Ia-Ib with macrocyclic structure and IIa-IIb with linear structure, especially with tri-heterocyclic functional groups, which has been evaluated to be highly potent and effective for inhibiting the NS3 protease replication of hepatitis C virus (HCV). This invention further relates to pharmaceutical compositions comprising one or more of new developed compounds (in a pure form or mixture of stereoisomers, solvates, hydrates, tautomers, prodrugs, or pharmaceutically acceptable salts thereof) and another agent(s) developed as therapeutic drugs for HCV treatment.
In the first aspect, the present invention provides polyheterocyclic based compounds having the following macrocyclic structure Ia and Ib:
and/or stereoisomers, solvates, hydrates, tautomers, esterification or amidation prodrugs, pharmaceutically acceptable salt, or mixtures thereof,
wherein:
m=0, 1 or 2;
n=0, 1 or 2;
p=0, 1 or 2;
q=0, 1 or 2;
r=0, 1, 2 or 3;
each dashed line “ ” is, independently, a single bond or double bond;
wherein when D and E are connected by a single bond, D and E are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
wherein when D and E are connected by a double bond, D and E each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when E 1 and G are connected by a single bond, E 1 and G are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
wherein when E 1 and G are connected by a double bond, E 1 and G are each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when the dashed line connecting R 10 to the macrocycle is a double bond, R 10 is O or S;
wherein when the dashed line connecting R 10 to the macrocycle is a single bond, R 10 is hydrogen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
Ra, Rb and Rc are each, independently, selected from the group consisting of hydrogen, halogen atom, cyano, nitro, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 6 -C 20 aryl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, C 2 -C 20 heterocyclic alkoxycarbonyl, C 2 -C 20 heterocyclic aryl, C 1 -C 20 alkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 aryl amino, C 1 -C 20 aminocarbonyl, C 1 -C 20 amido, C 1 -C 20 amidocarbonyl, C 1 -C 20 carbonylamino, C 1 -C 20 alkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, C 6 -C 20 arylsulfonamido, and C 1 -C 20 aminosulfonamido group;
wherein when r=0, E is nothing, and the D group is directly linked to the E 1 group;
L is oxygen, sulfur, —S(O)—, —S(O) 2 —, carbonyl, —C(Rb)(Rc)-, —C(Rb)=C(Rc)-, C 1 -C 20 alkoxy, C 2 -C 20 heterocyclyl, C 2 -C 20 heterocyclic alkoxy, —N(Ra)-, C 1 -C 20 aminocarbonyl, C 1 -C 20 alkoxycarbonyl, C 6 -C 20 aryl, C 6 -C 20 aryloxy, or C 6 -C 20 aryloxycarbonyl group, wherein Ra, Rb and Rc are as defined above;
T is N, O or CH, wherein when T is O, R 1 is not present;
U is C, S, —S(O)—, P or phosphate;
W is O or S;
X is O, S or —NRa-, wherein Ra is defined above;
Y is N or CH;
Z is hydroxyl, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 3 -C 20 cycloalkoxy, C 1 -C 20 alkylamino, C 3 -C 20 cycloalkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 aryl, C 6 -C 20 arylamino, C 4 -C 20 heteroarylamino, C 1 -C 20 alkyl sulfonamido, C 3 -C 20 cycloalkylsulfonamido, C 6 -C 20 arylsulfonamido, C 1 -C 20 alkoxy sulfonamido, C 3 -C 20 cycloalkoxy sulfonamido, C 1 -C 20 alkylamino sulfonamido, C 3 -C 20 cycloalkylamino sulfonamido, C 6 -C 20 arylamino sulfonamido, C 1 -C 20 uramido, C 1 -C 20 thioureido, C 1 -C 20 phosphate, or C 1 -C 20 borate;
R 1 and R 2 are each, independently, selected from the group consisting of hydrogen, hydroxyl, amino, C 1 -C 2 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 3 -C 20 cycloalkoxy, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 alkylamino, C 3 -C 20 cycloalkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 arylamino, C 1 -C 20 alkoxycarbonylamino, C 6 -C 20 aryloxycarbonylamino, C 1 -C 20 alkylsulfonamido, C 3 -C 20 cycloalkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, C 6 -C 20 arylsulfonamido, and C 1 -C 20 aminosulfonamido group;
R 3 , R 4 , R 5 and R 6 are each, independently, selected from the group consisting of hydrogen, halogen, hydroxyl, cyano, nitro, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylamino, C 2 -C 20 heterocyclicamino, C 6 -C 20 aryl, C 6 -C 20 arylamino, C 1 -C 20 alkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, and C 6 -C 20 arylsulfonamido group; and
R 7 , R 8 and R 9 are each, independently, selected from the group consisting of hydrogen, cyano, nitro, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, and C 2 -C 20 heterocyclic group.
In the second aspect, the present invention provides a kind of novel polyheterocyclic based compounds having the following structure IIa and IIb:
and/or its stereoisomers, solvates, hydrates, tautomers, esterification or amidation prodrugs, pharmaceutically acceptable salt, or mixtures thereof.
wherein:
p=0, 1 or 2;
q=0, 1 or 2;
r=0, 1, 2 or 3,
each dashed line “ ” is, independently, a single bond or double bond;
wherein when D and E are connected by a single bond, D and E are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
wherein when D and E are connected by a double bond, D and E each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when E 1 and G are connected by a single bond, E 1 and G are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
wherein when E 1 and G are connected by a double bond, E 1 and G are each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when the dashed line connecting R 10 to the macrocycle is a double bond, R 10 is O or S;
wherein when the dashed line connecting R 10 to the macrocycle is a single bond, R 10 is hydrogen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
Ra, Rb and Rc are each, independently, selected from the group consisting of hydrogen, halogen atom, cyano, nitro, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 6 -C 20 aryl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, C 2 -C 20 heterocyclic alkoxycarbonyl, C 2 -C 20 heterocyclic aryl, C 1 -C 20 alkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 aryl amino, C 1 -C 20 aminocarbonyl, C 1 -C 20 amido, C 1 -C 20 amidocarbonyl, C 1 -C 20 carbonylamino, C 1 -C 20 alkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, C 6 -C 20 arylsulfonamido, and C 1 -C 20 aminosulfonamido group;
wherein when r=0, E is nothing, and the D group is directly linked to the E 1 group;
W is O or S;
X is O, S or —NRa-, wherein Ra is defined above;
Y is N or CH;
Z is hydroxyl, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 3 -C 20 cycloalkoxy, C 1 -C 20 alkylamino, C 3 -C 20 cycloalkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 aryl, C 6 -C 20 arylamino, C 4 -C 20 heteroarylamino, C 1 -C 20 alkyl sulfonamido, C 3 -C 20 cycloalkylsulfonamido, C 6 -C 20 arylsulfonamido, C 1 -C 20 alkoxy sulfonamido, C 3 -C 20 cycloalkoxy sulfonamido, C 1 -C 20 alkylamino sulfonamido, C 3 -C 20 cycloalkylamino sulfonamido, C 6 -C 20 arylamino sulfonamido, C 1 -C 20 uramido, C 1 -C 20 thioureido, C 1 -C 20 phosphate, or C 1 -C 20 borate;
R 1 and R 2 are each, independently, selected from the group consisting of hydrogen, hydroxyl, amino, C 1 -C 2 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 3 -C 20 cycloalkoxy, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 alkylamino, C 3 -C 20 cycloalkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 arylamino, C 1 -C 20 alkoxycarbonylamino, C 6 -C 20 aryloxycarbonylamino, C 1 -C 20 alkylsulfonamido, C 3 -C 20 cycloalkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, C 6 -C 20 arylsulfonamido, and C 1 -C 20 aminosulfonamido group;
R 3 , R 4 , R 5 and R 6 are each, independently, selected from the group consisting of hydrogen, halogen, hydroxyl, cyano, nitro, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylamino, C 2 -C 20 heterocyclicamino, C 6 -C 20 aryl, C 6 -C 20 arylamino, C 1 -C 20 alkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, and C 6 -C 20 arylsulfonamido group; and
R 7 , R 8 and R 9 are each, independently, selected from the group consisting of hydrogen, cyano, nitro, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, and C 2 -C 20 heterocyclic group; and
R 11 is hydrogen, C 1 -C 20 alkyl, C 1 -C 20 alkylcarbonyl, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 6 -C 20 aryl, C 6 -C 20 arylcarbonyl, C 6 -C 20 aryloxycarbonyl, C 1 -C 20 alkylsulfonamido, C 6 -C 20 arylsulfonamido, C 1 -C 20 aminosulfonamido, C 2 -C 20 heterocyclic group.
In the third aspect, the present invention provides a kind of novel polyheterocyclic based compounds having the following structure Va and Vb:
wherein:
p=0, 1 or 2;
q=0, 1 or 2;
r=0, 1, 2 or 3;
each dashed line “ ” is, independently, a single bond or double bond;
wherein when D and E are connected by a single bond, D and E are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
wherein when D and E are connected by a double bond, D and E each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when E 1 and G are connected by a single bond, E 1 and G are each, independently, selected from the group consisting of O, S, amino, and —C(Ra)(Rb)-; and R 10 is hydrogen, oxygen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 12 heterocyclic group;
wherein when E 1 and G are connected by a double bond, E 1 and G are each, independently, selected from the group consisting of N or —C(Rc)-;
wherein when the dashed line connecting R 10 to the macrocycle is a double bond, R 10 is O or S;
wherein when the dashed line connecting R 10 to the macrocycle is a single bond, R 10 is hydrogen, halogen atom, cyano, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, or C 2 -C 20 heterocyclic group;
Ra, Rb and Rc are each, independently, selected from the group consisting of hydrogen, halogen atom, cyano, nitro, C 1 -C 20 alkyl, C 3 -C 20 cycloalkyl, C 6 -C 20 aryl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, C 2 -C 20 heterocyclic alkoxycarbonyl, C 2 -C 20 heterocyclic aryl, C 1 -C 20 alkylamino, C 2 -C 20 heterocyclic amino, C 6 -C 20 aryl amino, C 1 -C 20 aminocarbonyl, C 1 -C 20 amido, C 1 -C 20 amidocarbonyl, C 1 -C 20 carbonylamino, C 1 -C 20 alkylsulfonamido, C 2 -C 20 heterocyclic sulfonamido, C 6 -C 20 arylsulfonamido, and C 1 -C 20 aminosulfonamido group;
wherein when r=0, E is nothing, and the D group is directly linked to the E 1 group;
R 7 , R 8 and R 9 are each, independently, selected from the group consisting of hydrogen, cyano, nitro, trifluoromethyl, C 1 -C 20 alkyl, C 1 -C 20 alkoxy, C 1 -C 20 alkylthio, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 1 -C 20 carbonylamino, C 6 -C 20 aryl, C 6 -C 20 aryloxy, C 6 -C 20 aryloxycarbonyl, and C 2 -C 20 heterocyclic group; and
R 13 is hydrogen, C 1 -C 20 alkyl, C 1 -C 20 alkylcarbonyl, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 cycloalkoxycarbonyl, C 1 -C 20 aminocarbonyl, C 6 -C 20 aryl, C 6 -C 20 arylcarbonyl, C 6 -C 20 aryloxycarbonyl, C 1 -C 20 alkylsulfonyl, C 6 -C 20 arylsulfonyl, C 1 -C 20 aminosulfonyl, or C 2 -C 20 heterocyclic group.
The fourth aspect of the present invention provides a pharmaceutical composition comprising one or more compounds selected from the structure Ia-Ib or IIa-IIb.
The fifth aspect of the present invention provides a pharmaceutical combination of any one or more compounds of the structure Ia-Ib or IIa-IIb in a therapeutically effective dose and/with a second or a third medicament in a therapeutically effective dose. Thus, the present invention provides a pharmaceutical composition, comprising at least one compound described above in a therapeutically effective dose and at least one additional medicament in a therapeutically effective dose
The sixth aspect of the present invention provides a pharmaceutical combination of any compound of the structure Ia-Ib or IIa-IIb and/with any HIV inhibitor including but not limited to Ritonavir. Thus, the present invention provides a A pharmaceutical composition, comprising at least one compound described above in a therapeutically effective dose and at least one HIV inhibitor in a therapeutically effective dose.
The seventh aspect of the present invention provides a pharmaceutical combination of at least one compound described above and any-hepatitis B virus (HBV) inhibitor including but not limited to Heptodin, Sebivo, Hepsera, Emtriva, Baraclude, or Viread.
The eighth aspect of the present invention provides a method for inhibiting HCV by using one or more compounds of the structure Ia-Ib or IIa-IIb in a therapeutically effective dose and a second or a third medicament in a therapeutically effective dose. Thus, the present invention provides a method of inhibiting HCV, comprising administering an effect amount of a compound or composition described above to a subject in need thereof.
The ninth aspect of the present invention provides a method for inhibiting HCV by using one or more compounds of the structure Ia-Ib or IIa-IIb and in combination with any or combined one or more of (1) Immune modulators including but not limited to Interferons, pegulated-interferons, or interferon derivatives, (2) HCV protease inhibitors, (3) HCV polymerase inhibitors, (4) nucleosides and its derivatives, (5) Cyclophilin inhibitors, (6) Glucosidase I inhibitors, (7) IMPDH inhibitors, (8) Caspase inhibitors, (9) TLR agonists, (10) HIV inhibitors, (11) anti-inflammatory drugs, (12) Cancer drugs, or (13) other compounds not covered from above (1)-(12).
Overall, furthermore, all prepared new polyheterocyclic based compounds have been evaluated for their potency in vitro and in vivo, and the present invention explores the relationship between the structures of new polyheterocyclic compounds and efficacy of HCV inhibition and provides valuable clue and potential HCV inhibitors.
DETAILED DESCRIPTION OF THE INVENTION
Details of the present invention are set forth in the following description for preparation and biological activity study of new HCV inhibitors Ia-Ib and IIa-IIb. The advantages of the present invention will be significantly observed from the following detailed description.
As used herein, the term “alkyl” refers to any linear or branched chain alkyl group having a number of carbon atoms and/or “alkylene” in the specified range, wherein one or more hydrogens could be replaced by one or more halogens.
The term “alkoxy” refers to an “alkyl-O—” group.
The term “cycloalkyl” refers to any cyclic ring of an alkane or alkene having a number of carbon atoms and/or “alkylene” in the specified range, wherein one or more hydrogens could be replaced by one or more halogens.
The term “halogen” (or “halo”) refers to fluorine, chlorine, bromine and iodine atoms (or referred as fluoro, chloro, bromo, and iodo).
The term “carbonyl” refers to an “—C(O)—” group.
The term “alkyl carbonyl” refers to an “alkyl-C(O)—” group.
The term “alkoxy carbonyl” refers to an “alkyl-O—C(O)—” group.
The term “alkylamino carbonyl” refers to an “alkyl-NH—C(O)—” or “dialkyl-N—C(O)—” group.
The term “sulfonamido” refers to an “—S(O) 2 NH—” or “—S(O) 2 N(R)—” group, wherein R is alkyl or alkylcarbonyl group.
The term “alkyl sulfonamido” refers to an “alkyl-S(O) 2 NH—” or “alkyl-S(O) 2 N(R)—” group, wherein R is alkyl or alkylcarbonyl group.
The term “alkoxy sulfonamido” refers to an “alkyl-O—S(O) 2 NH—” or “alkyl-O—S(O) 2 N(R)—” group, wherein R is alkyl or alkylcarbonyl group.
The term “polyheterocyclic” refers to a tri-cyclic or tetra-cyclic functional group with 1-5 hetero atoms (e.g., O, N, S, and P) in one or more fused rings.
The term “composition” is intended to encompass a product comprising the specified ingredients, as well as any product which results, directly or indirectly, from combining the specified ingredients.
The term “pharmaceutically acceptable” means that the ingredients of the pharmaceutical composition must be compatible with each other and not deleterious to the recipient thereof.
The term “effective amount” means that amount of active compound or pharmaceutical agent that elicits the biological or medicinal response in a tissue, system, animal or human that is being sought by a researcher, veterinarian, medical doctor or other clinician. The term also includes herein the amount of active compound sufficient to inhibit HCV NS3 protease and thereby elicit the response being sought (i.e., an “inhibition effective amount”). When the active compound (i.e., active ingredient) is administered as the salt, references to the amount of active ingredient are to the free acid or free base form of the compound.
The present invention provides two classes of novel polyheterocyclic based compounds Ia-Ib and IIa-IIb, and pharmaceutically acceptable salts, and/or hydrates as HCV NS3 protease inhibitors with high potency. Moreover, toxicity study is is determined to be non-toxic (LD 50 >10,000) for most of highly potent HCV inhibitors.
Synthesis of New Polyheterocyclic Based Compounds with General Structure Ia-Ib and IIa-IIb:
Using previously published and the synthetic methods described herein, different kinds of synthetic methods have been carried out effectively to prepare different compounds with the structure Ia-Ib and IIa-IIb.
In the present invention, compounds VIa-VIf are prepared first as in the following Scheme 1:
In Scheme 1, in the presence of inorganic base (e.g., sodium hydroxide, sodium methoxide, or sodium hydrogen), SM-1 was dissolved in organic solvents (methanol, THF, DMF, or DMSO) and heated to 30-120° C., then reacted with ClCH 2 Cl, ClCH 2 CH 2 Cl, or BrCH 2 CH 2 CH 2 Br, respectively, to form five, six, or seven membered polyheterocyclic compound 1-1, 1-2, or 1-3, followed by deprotection to obtain the key tri-heterocyclic compounds VIa-VIc by removing the protecting group (Bn: benzyl) with Pd/C catalyst and hydrogen in methanol or ethanol.
In Scheme 2, SM-2 was dissolved in organic solvents (methanol, THF, DMF, or DMSO) and heated to 30-120° C., then reacted with BrCH 2 CH 2 CH 2 Br, ClCH 2 CH 2 Cl or ClCH 2 Cl, respectively, to form seven, six or five membered polyheterocyclic compound 2-1, 2-2, or 2-3, followed by deprotection to obtain the key tri-heterocyclic compounds VId-VIf by removing the protecting group (Bn: benzyl) with Pd/C catalyst and hydrogen in methanol or ethanol.
Preparation of the following specific compounds IIIa-IIIb has been carried out as follows in Scheme 3.
R 11 is preferred to be selected from the following group: SM-4a (Boc) or SM-4b:
In the presence of coupling reagent CDI, starting material SM-4 (e.g., SM-4a or SM-4b) was reacted with compounds VIa-VIf, respectively to obtain polyheterocyclic compounds 4a-4h and 6a-6d (IIIa-IIIb) as shown below amidation reaction.
After the key intermediates 4a-4f and 6a-6f were prepared, there were several synthetic methods developed as in Schemes 4-11 for preparation of different kinds of new HCV inhibitors. The detail for each reaction condition and analytical results of products is listed in the detailed examples.
In Scheme 4 above, the product 4 (e.g., compounds 4a-4f and 6a-6f) prepared as shown in Scheme 3 was deprotected to obtain an intermediate carboxylic acid (5) by removing HCl group, followed by amidation with an N-Boc protected amino acid SM-5 to form compound 6 in the presence of coupling reagent HATU. After hydrolysis of compound 6 in LiOH-Water/MeOH solution, another carboxylic acid (7) was obtained, and followed by amidation with another amino acid (methyl or ethyl ester) SM-6 in the presence of coupling reagent HATU to form product 9 (e.g., compounds 9a-9f shown below). In anhydrous oxygen-free organic solvents (DCM, DCE, or toluene), Diene 9 intermediate was carried out an olefin ring-closing metathesis (RCM) reaction in the presence of metathesis catalyst (e.g., Zhan catalyst-1 or Zhan catalyst-1B used in this invention) at 20-80□ to form 14-16 membered macrocyclic olefin-linked product 10, then the methyl/ethyl ester was hydrolyzed with LiOH in water-MeOH solution to offer a new carboxylic acid 11. Finally, in the presence of a coupling reagent such as EDCI or HATU, the carboxylic acid 11 reacted with different kinds of alkylsulfonamide, cycloalkylsulfonamide or arylsulfonamide [RdS(O) 2 NH 2 ], respectively, to form a series of novel polyheterocyclic based macrocyclic compounds Ia-Ib, such as 12a-12xx shown below).
The structure of Zhan catalysts (Zhan Catalyst-1 & 1B) used for RCM of diene intermediate 9 is shown below:
In order to obtain more compounds efficiently for potency screening, there is another alternative synthetic route developed effectively for preparation of different new macrocyclic compounds Ia-Ib in Scheme 5.
In Scheme 5, first of all, the protecting group (Boc) in the starting material SM-7 was removed by HCl acid, followed by amidation with an N-Boc protected amino acid SM-5 to form compound 8 in the presence of coupling reagent HATU. In the presence of coupling reagent CDI, compound 8 was reacted with compounds VIa-VIf, respectively, to obtain polyheterocyclic compounds 9. In anhydrous oxygen-free organic solvents (DCM, DCE, or toluene), an olefin ring-closing metathesis (RCM) reaction was carried out for the diene 9 intermediate in the presence of metathesis catalyst (e.g., Zhan catalyst-1 or Zhan catalyst-1B used in this invention) at 20-80□ to form 14-16 membered macrocyclic olefin-linked product 10, then the methyl/ethyl ester was hydrolyzed with LiOH in water-MeOH solution to offer a new carboxylic acid 11 as shown below.
Finally, in the presence of a coupling reagent such as EDCI or HATU, the carboxylic acid product 11 reacted with different kinds of alkylsulfonamide, cycloalkylsulfonamide or arylsulfonamide [RdS(O) 2 NH 2 ], respectively, to form a series of novel polyheterocyclic based macrocyclic compounds Ia-Ib.
In order to optimize efficacy and biological property of new HCV inhibitors, there are more structure modified compounds designed and synthesized in Schemes 6-11. In Scheme 6, there is a kind of cycloalkylsulfonamide products prepared for potency screening.
In Scheme 6 above, the compound 10c-d prepared in Schemes 4 and 5 were used for deprotection first by removing Boc with HCl acid, followed by amidation with an alkylsulfonyl chloride reagent (RdSO 2 Cl or R 17 SO 2 Cl, SM-9) to obtain an alkylsulfonamide product 13. In the presence of inorganic base (e.g., NaOH or KOH), the intramolecular cyclization was conducted to form sulfonamide compound 11. Finally, in the presence of a coupling reagent such as EDCI or HATU, the carboxylic acid 11 reacted with different kinds of alkylsulfonamide, cycloalkylsulfonamide or arylsulfonamide [RdS(O) 2 NH 2 , SM-8], respectively, to form a series of novel polyheterocyclic based macrocyclic compounds Ia-Ib, such as 12j-12m as shown below. Furthermore, the compound 10c-d was deprotected first by removing Boc with HCl acid, followed by amidation with an alkylsulfonyl chloride reagent (RdSO 2 Cl or R 17 SO 2 Cl, SM-9) to obtain another kind of alkylsulfonamide product 13, then in the presence of a base (e.g., NaH or NaOMe), the alkylsulfonamide product 13 was reacted with another reagent R 16 —Cl (or R 16 —Br, SM-10) or (Boc) 2 O to form another kind of new desired products Ia-Ib (12s-12u) as herein, wherein, R 16 is C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, C 1 -C 6 alkoxycarbonyl, C 3 -C 6 cycloalkoxycarbonyl, C 6 -C 10 aryl, C 6 -C 10 arylcarbonyl, C 6 -C 10 aryloxycarbonyl or C 2 -C 10 heterocyclic group.
In the following Scheme 7, the product 12 (e.g., 12a-12f and 12-Ref) was used for deprotection first by removing Boc with HCl acid, followed by either alkylation or amidation with reagent SM-10 (R 16 —Cl or R 16 —Br) to obtain an N-alkylated product 15 or amidation with an alkylsulfonyl or arylsulfonyl chloride reagent SM-9 [R 17 S(O) 2 Cl)] to form product 16, wherein R 16 and R 17 each is C 1 -C 6 alkyl, C 3 -C 6 cycloalkyl, C 1 -C 6 alkoxycarbonyl, C 3 -C 6 cycloalkoxycarbonyl, C 6 -C 10 aryl, C 6 -C 10 arylcarbonyl, C 6 -C 10 aryloxycarbonyl or C 2 -C 10 heterocyclic group, which generates more polyheterocyclic compounds 15a-15b and 16a-16c shown below.
In order to optimize efficacy and biological property of new HCV inhibitors, there are two more different macrocyclic structure designed and synthesized in the following Schemes 8 and 9.
In Scheme 8, in the presence of coupling reagent HATU, an acid SM-11 was reacted with another amine SM-12 to form a diene product 17 by amidation, followed by RCM reaction in the presence of Zhan catalyst-1B to form a 14-16 membered macrocyclic product 18. In the presence of coupling reagent CDI, product 18 was reacted with compounds VIa-VIf, respectively to obtain polyheterocyclic compounds 21a-21f, then the methyl/ethyl ester was hydrolyzed with LiOH in water-MeOH solution to offer a new carboxylic acid 11. Finally, in the presence of a coupling reagent such as EDCI or HATU, the carboxylic acid 20 reacted with different kinds of alkylsulfonamide, cycloalkylsulfonamide or arylsulfonamide [RdS(O) 2 NH 2 ], respectively, to form a series of novel polyheterocyclic based macrocyclic compounds Ia-Ib (21a-21j), shown below:
In Scheme 9, in the presence of coupling reagent CDI, SM-7 was reacted with compounds VIa-VIf, respectively to obtain polyheterocyclic compounds 23a-23f, followed by reacting with a reagent chloroformic acid 4-nitrophenyl ester and SM-12 to form a diene product 24. In the presence of Zhan catalyst-1B, the diene product 24 was conducted a RCM reaction to form a desired macrocyclic product 25, then the methyl/ethyl ester was hydrolyzed with LiOH in water-MeOH solution to offer a new carboxylic acid 26. Finally, in the presence of a coupling reagent such as EDCI or HATU, the carboxylic acid 26 reacted with different kinds of alkylsulfonamide, cycloalkylsulfonamide or arylsulfonamide [RdS(O) 2 NH 2 ], respectively, to form a series of novel polyheterocyclic based macrocyclic compounds Ia-Ib (27a-27c and 27-Ref), shown below:
To evaluate the difference in potency and other biological activities between the macrocyclic and linear structures for the novel polyheterocyclic based HCV inhibitors, there are different kinds of linear compounds IIa-IIb (30 and 33) with polyheterocyclic groups VIa-VIf prepared as shown in the following Schemes 10 and 11, respectively.
In Scheme 10 above, in the presence of coupling reagent EDCI, an amine SM-13 was reacted with a sulfonamide RdS(O) 2 NH 2 ], (SM-8) to form product 28, followed by removing Boc protecting group to obtain a de-Boc product 29. Finally, in the presence of a coupling reagent such as EDCI or HATU, the amine intermediate 29 was reacted with different kinds of amino acid derivatives SM-14 selected from a list of chemical reagents shown below to form various products IIa-IIb (30a-30ar) as shown as follows, wherein Rd and R 18 each is C 1 -C 6 alkyl or C 3 -C 6 cycloalkyl group, and R 19 is C 1 -C 20 alkyl, C 1 -C 20 alkylcarbonyl, C 1 -C 20 alkoxycarbonyl, or C 1 -C 20 alkylsulfonamido groups as shown below from compounds 30a-30ar.
In Scheme 11 above, in the presence of coupling reagent HATU in DMF, an acid SM-15 was reacted with another amine reagent SM-16 to form an amide product 31 by amidation, followed by removing Boc protecting group with HCl-THF solution to obtain an amine product 32. Finally, in the presence of a coupling reagent such as EDCI or HATU, the amine intermediate 32 reacted with various carboxylic acids SM-14, respectively to form different kinds of novel polyheterocyclic based linear compounds IIa-IIb (33a-33d) shown as follows, wherein R 18 each is C 1 -C 6 alkyl or C 3 -C 6 cycloalkyl group, and R 19 is C 1 -C 20 alkyl, C 1 -C 20 alkylcarbonyl, C 1 -C 20 alkoxycarbonyl, or C 1 -C 20 alkylsulfonamido groups.
Additional polyheterocyclic based compounds within the scope of the present invention can be prepared using other suitable starting materials through the above synthetic routes or other developed procedures as reported from different references. The methods described in Schemes 1-11 above may also additionally include steps, either before or after the steps described specifically herein, to add or remove suitable protecting groups in order to ultimately allow synthesis of the compounds in this invention. In addition, various synthetic steps may be performed in an alternate sequence or order to give the desired compounds.
Synthetic chemistry transformations and protecting group methodologies (protection and deprotection) useful in synthesizing applicable compounds in this invention are known in the art and include, for example, those described in R. Larock, Comprehensive Organic Transformations , VCH Publishers (1989); T. W. Greene and P. G. M. Wuts, Protective Groups in Organic Synthesis, 2 nd Ed., John Wiley and Sons (1991); L. Fieser and M. Fieser, Fieser and Fieser's Reagents for Organic Synthesis , John Wiley and Sons (1994); and L. Paquette, ed., Encyclopedia of Reagents for Organic Synthesis , John Wiley and Sons (1995) and subsequent editions thereof.
The compounds mentioned herein may contain a non-aromatic double bond and one or more asymmetric centers. Thus, they can occur as racemates and racemic mixtures, single enantiomers, individual diastereomers, diastereomeric mixtures, tautomers, and cis- or trans-isomeric forms, and/or hydrates. All such isomeric forms are contemplated.
So far, there is no any effective animal model for scientists to evaluate the efficacy of new compounds for inhibiting the HCV NS3 protease. The compounds described above in the present invention can be preliminarily screened by evaluating the IC 50 and/or EC 50 results for their activity and efficacy in treating HCV infection by an in vitro and/or in vivo assay as follows, then have some highly potent HCV inhibitors selected for other PK and toxicity studies before clinic trial during new drug development. Other methods will also be apparent for scientists in pharmaceuticals.
HCV NS3-4A Protease Assay In Vitro.
The assay was conducted in Buffer A containing 30 mM NaCl, 5 mM CaCl 2 , 10 mM DTT, 50 mM Tris (pH7.8), using the Ac-Asp-Glu-Asp(EDANS)-Glu-Glu-Abu-ψ-[COO]-Ala-Ser-Lys (DABCYL)-NH 2 (FRET-S) fluorescent peptide (AnaSpec, USA) as substrate. Briefly, 140 μL buffer A, 20 μL compounds dissolved in buffer A with different concentration and 20 μL HCV NS3-4A protease diluted in buffer A were added into 96-well plate respectively and mixed well. The reaction was initiate with adding 20 μL of FRET-S. Reactions were continuously monitored at 37° C. using a BMG Polarstar Galaxy (MTX Lab Systems, Inc. USA), with excitation and emission filters of 355 nm and 520 nm, respectively. The 50% inhibitory concentration (IC 50 ) was calculated with Reed & Muench methods.
Antiviral Assay:
Antiviral assays were carried out in black-walled, clear bottomed 96-well plates. Renila luciferase reporter replicon cells were seeded at a density of 7×10 3 cells/well in 100 μl complete DMEM culture without selection antibiotics. Eight twofold serial dilutions of compounds were prepared in complete DMEM and added to the appropriate wells, yielding final concentrations in 200 μl of complete DMEM culture. Following 3 days of incubation, cells were incubated with 100 μl fresh culture containing EnduRen™ Live Cell Substrate (Promega) at final concentrations of 60 μM at 37° C. in 5% CO 2 for 2 h in the dark. Luminescence was then measured using an EnVision (Perkin-Elmer) microplate reader. Data were normalized to percentage of the control, and the 50% effective concentration (EC 50 ) values were calculated using the method of Reed-Muench.
Acute Toxicity Study (MTD):
Materials and Methods for MTD Study are as follows:
Animals:
320 KM mice, Certificate Number: 2007000510144, male and female were each half, 40 Wistar rats, certificate number: 2007000510555, male and female were each half. Animals were purchased from SLAC Laboratory Animal Limited Co., Feed: Breeding fodder of Radiation, special for rats and mice, was purchased from SLAC Laboratory Animal Limited Co.
Test Group:
Animals were fed freely for adaptation more than 1 week. Healthy rats, body weight between 170-190 g, were divided randomly into 3 groups, 5 male and 5 female in each group. Healthy mice, body weight between 18-20 g, were divided randomly into 22 groups, 5 male and 5 female in each group.
Administration Method:
In rats, the compound weighing 21.00 g, serial number 1-3 respectively, adding 0.7% sodium carboxymethyl cellulose solution 30.00 g, high-speed homogenizer machine 15000 RPM, 10 min mixing, the rats were fed once, oral dose 10000 mg/kg. In mice, the compound weighing 2.00 g, serial number 4-25 respectively, adding 0.7% sodium carboxymethyl cellulose solution 8.00 g, high-speed homogenizer machine 10000 RPM, 10 min mixing, the mice were fed once, oral dose 10000 mg/kg.
Clinical Observation:
Animals were observed every hour after administration in the first day, and behavior observation daily continuous for a week. Dead animals were necropsied, gross pathology of the organs were observed and recorded.
Evaluation of Toxicity:
Toxicity was evaluated by animal mortality, signs of clinical behavior and others.
Among all of synthesized polyheterocyclic compounds 11a-11p, 12a-12u, 15a-15b, and 16a-16c, 30a-30ar, 33a-33d and some reference compounds 12-Ref, 21-Ref, 27-Ref, the results of HCV protease (HCV NS3-4A) inhibition test are listed in Table 1; where the scope of potent activity (IC 50 ): ≧200 nM labeled “A”, active in the range of 30-200 nM labeled “B”, active range ≦30 nM labeled “C”.
TABLE 1
Activity of Novel Polyheterocyclic Based Compounds
for Inhibiting HCV NS3 Protease
NS3-NS4A
Entry
Compound
IC 50
1
11a
A
2
11b
A
3
11c
A
4
11d
A
5
12a
C
6
12b
C
7
12c
C
8
12d
C
9
12e
C
10
12f
C
11
12g
C
12
12h
C
13
12j
B
14
12k
C
15
12m
B
16
12n
C
17
12p
C
18
12q
C
19
12r
C
20
12s
C
21
12t
C
22
12u
C
23
12-Ref
C
24
15a
C
25
15b
C
26
16a
C
27
16b
C
28
16c
C
29
21a
B
30
21b
B
31
21c
C
32
21d
B
33
21e
C
34
21f
B
35
27a
B
36
27b
B
37
27c
B
38
27-Ref
B
39
27-Ref-2
B
40
30a
C
41
30b
C
42
30c
C
43
30d
C
44
30e
C
45
30f
C
46
30g
C
47
30h
C
48
30j
C
49
30k
C
50
30m
C
51
30n
C
52
30p
C
53
30r
C
54
30s
C
55
30t
C
51
30v
C
52
30w
C
53
30x
C
54
30y
C
55
30z
C
56
30aa
C
57
30ab
C
58
30ac
C
59
30ad
B
60
30ae
B
61
30af
C
62
30ag
C
63
30ah
C
64
30aj
C
65
30ak
C
66
30am
C
67
30an
C
68
30ap
C
69
30aq
C
70
30ar
C
71
30-Ref
C
72
33a
B
73
33b
B
74
33c
B
75
33d
A
76
30-Ref
B
The potent screening results in Table 1 show that: (1) the polyheterocyclic based macrocyclic compounds (e.g., 12a-12u) containing cyclopropyl sulfonamide and isopropylsulfonamide have much better HCV inhibition activity than the polyheterocyclic based carboxyl acid products (e.g., 11a-11m) that do not have cyclopropylsulfonamide or isopropylsulfonamide group incorporated by amidation, (2) in general, the polyheterocyclic based macrocyclic compounds Ia-Ib (e.g., 12a-12u) have better efficacy and biological activity than the polyheterocyclic based linear compounds IIa-IIb (e.g., 30a-30ar and 33a-33d), and (3) several of the novel polyheterocyclic based macrocyclic sulfonamide compounds Ia-Ib (e.g., 12a-12d, 12q-12u) are highly effective (EC 50 : 0.001-1.0 uM) as HCV inhibitors, and many of new polyheterocyclo based HCV inhibitors have excellent biological activities to inhibit HCV in comparison with some referred HCV inhibitors already in clinical Phase II and III, such as InterMune (ITMN-191, 12Ref)-Roche, and Merck MK-7009.
Overall, all prepared new polyheterocyclic based compounds have been evaluated for their potency and efficacy in vitro and/or in vivo, and there are two novel classes of polyheterocyclic based compounds found highly effective to inhibit HCV. Moreover, the present invention explores the insight relationship between the structures of new polyheterocyclic compounds and efficacy of HCV inhibition, which provides valuable clue to develop an effective potential HCV inhibitors among the developed novel polyheterocyclic compounds Ia-Ib and IIa-IIb.
Abbreviations of chemical materials, reagents, and solvents related to the present invention are listed as follows:
SM4: N-Boc-trans-4-hydroxy-L-proline methyl ester
SM5: Boc-L-2-amino-8-azelaic acid
SM6: (1R,2S)-1-amino-2-cyclopropyl methyl vinyl
AIBN: azobisisobutyronitrile
(Boc)2O: di-tert-butyl carbonate
CDI: N,N′-carbonyldiimidazole imidazole
DBU: 1,8-Diazabicyclo[5.4.0]undec-7-ene
EDCI: N-ethyl-N-(3-dimethyl aminopropyl)carbodiimide hydrochloride
HATU: 2-(7-benzotriazole azo)-N,N,N′,N′-tetramethyl urea phosphate hexafluoride
NBS: N-bromosuccinimide
DMAP: 4-dimethylaminopyridine
DIEA: N,N-diisopropyl ethylamine
SOCl2: thionyl chloride
Pd/C: Palladium carbon
HMTA: hexamethylene tetramine
HOAc: acetic acid
HBr: Hydrobromic acid
HCl: hydrochloric acid
TFA: trifluoroacetic acid
TsOH: p-toluenesulfonate
NaOH: sodium hydroxide
ACN: acetonitrile
DCM: dichloromethane
DCE: dichloroethane
DMF: N,N-dimethylformamide
DMSO: dimethyl sulfoxide
Et2O: diethyl ether
EA: ethyl acetate
PE: petroleum ether
THF: tetrahydrofuran
TBME: tert-butyl methyl ether
EXAMPLES
General
Infrared (IR) spectra were recorded on a Fourier Transform AVATAR™ 360 E.S.P™ spectrophotometer (Unit: cm −1 ). Bands are characterized as broad (br), strong (s), medium (m), and weak (w). 1 H NMR spectra were recorded on a Varian-400 (400 MHz) spectrometer. Chemical shifts are reported in ppm from tetramethylsilane with the solvent resonance as the internal standard (CDCl 3 : 7.26 ppm). Data are reported as follows: chemical shift, multiplicity (s=singlet, d=doublet, t=triplet, q=quartet, br=broad, m=multiplet), coupling constants (Hz), integration, and assignment. 19 F and 31 P NMR spectra were recorded on a Varian-400 (400 MHz) and Varian-500 (500 MHz) spectrometers. The chemical shifts of the fluoro resonances were determined relative to trifluoroacetic acid as the external standard (CF 3 CO 2 H, 0.00 ppm), and the chemical shifts of the phosphorus resonances were determined relative to phosphoric acid as the external standard (H 3 PO 4 : 0.00 ppm). Mass spectra were obtained at Thermo Finnigan LCQ Advantage. Unless otherwise noted, all reactions were conducted in oven- (135° C.) and flame-dried glassware with vacuum-line techniques under an inert atmosphere of dry Ar. THF and Et 2 O were distilled from sodium metal dried flask, DCM, pentane, and hexanes were distilled from calcium hydride. Most chemicals were obtained from commercial sources or ordered by contract synthesis from Zannan SciTech Co., Ltd. in China. General procedures for preparation of different polyheterocyclic intermediates and products (Ia-Ib and IIa-IIb) are described in the following examples, respectively.
Example 1
Synthesis of Compound VIa
SM-1 (12.2 g, 0.5 mol) and 100 mL DCM were added into a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. After the reaction was completed, the mixture was poured into ice water and extracted three times with DCM. The combined organic layer was washed with brine, then dried and concentrated, finally purified by column chromatography with silica gel to obtain the cyclized product 1-1 (7.7 g), yield 61%. ESI-MS (M+H + ): m/z calculated: 253.1. founded: 253.2.
The product 1-1 (5.0 g, 0.2 mol) was dissolved in ethanol, catalyst Pd/C (0.5 g) was added under hydrogen pressure (0.6 MPa). When the reaction was completed, the mixture was filtered and washed with ethanol, then the filtrate was concentrated to offer crude product (3.0 g). After purified by flash column, the desired product VIa (2.5 g) was obtained with purity over 99%, yield 76%. Total yield for two steps: 46%.
1 H-NMR for the product VIa (CDCl3, 500 MHz): δ 6.71 (s, 2H), 5.91 (s, 2H), 4.20 (s, 2H), 4.15 (s, 2H), 2.22 (s, 1H, NH). ESI-MS (M+H + ): m/z calculated 164.1, founded 164.2.
Example 2
Synthesis of Compound VIb
SM-1 (12 g, 0.5 mol) and 30 mL DCE were added to a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. After the reaction was completed, the mixture was poured into ice water and extracted three times with DCM. The combined organic layer was washed with brine, then dried and concentrated. After purified by flash column, the desired product 1-2 (9.4 g) was obtained, yield 71%. ESI-MS (M+H + ): m/z calculated 268.1. founded 268.2.
The product of 2-1 (5.0 g) was dissolved in ethanol, Pd/C (0.5 g) was added with hydrogen pressure (0.6 MPa). When the reaction was completed, the mixture was filtered and washed with ethanol, the filtrate was concentrated to give crude product (3.0 g). After purified by flash column, the desired product VIb (2.9 g) was obtained. Total yield for two steps: 61%.
1 H-NMR for the product VIb (CDCl3, 500 MHz): δ 6.77-6.75 (d, J=8.0 Hz, 1H), 6.72-6.70 (d, J=8.0 Hz, 1H), 4.29-4.28 (m, 2H), 4.27-4.26 (m, 2H), 4.19 (s, 2H), 4.17 (s, 2H), 2.27 (s, 1H, NH). ESI-MS (M+H + ): m/z calculated 178.1. founded 178.2.
Example 3
Synthesis of Compound VIc
SM-1 (12 g, 0.5 mol) and Br(CH2)3Br (20 mL) were added to a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. The reaction condition was the same as done in Example 2. After the cyclization and purification, the desired product VIc was obtained. Total yield for two steps: 47%.
1H-NMR for the product VIc (CDCl3, 500 MHz): δ 10.09 (s, 2H), 6.96-6.94 (d, J=8.0 Hz, 1H), 6.92-6.90 (d, J=7.5 Hz, 1H), 4.40-4.39 (m, 4H), 4.20-4.17 (t, J=5.0 Hz, 2H), 4.13-4.11 (t, J=5.0 Hz, 2H), 2.19-2.09 (m, 2H). ESI-MS [(M+H)+]: m/z calculated 192.1. founded 192.1.
Example 4
Synthesis of Ru Complex VId
SM-2 (12 g, 0.5 mol) and Br(CH2)3Br (20 mL) were added to a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. The reaction condition was the same as done in Example 2. After the cyclization and purification, the desired product VIc was obtained. Total yield for two steps: 41%.
1 H-NMR for the product VId (CDCl3, 500 MHz): δ 6.86 (s, 2H), 4.30 (brs, 1H), 4.20 (s, 4H), 4.15-4.17 (t, J=5.8 Hz, 4H), 2.16-2.18 (m, 2H). ESI-MS [(M+H) + ]: m/z calculated 192.1. founded 192.1.
Example 5
Synthesis of Compound VIe
SM-2 (12 g, 0.5 mol) and DCE (30 mL) were added to a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. The reaction condition was the same as done in Example 2. After the cyclization and purification by flash column, the desired product VIe was obtained. Total yield for two steps: 56%.
1H-NMR for the product VIe (CDCl3, 500 MHz): δ 6.74 (s, 2H), 4.23 (s, 4H), 4.13 (s, 4H). ESI-MS (M+H+): m/z calculated 178.1. founded 178.2.
Example 6
Synthesis of Compound VIf
SM-2 (12 g, 0.5 mol) and DCM (100 mL) were added to a 250 mL reaction flask, then NaOH (5 g) and DMSO (50 mL) were added and heated to 100° C. The reaction condition was the same as done in Example 1. After the cyclization and purification is by flash column, the desired product VIf was obtained. Total yield for two steps: 51%.
1H-NMR for the product VIf (CDCl3, 500 MHz): δ 6.69 (s, 2H), 5.95 (s, 2H), 4.14 (s, 4H). ESI-MS (M+H+): m/z calculated 164.1. founded 164.2.
Example 7
Synthesis of Compound 4a
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane (DCM) and stirred overnight, followed by adding another compound VIa (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4a (5.2 g) was obtained, yield 71%.
1 H-NMR for the product 4a (CDCl 3 , 500 MHz): δ 6.78-6.80 (m, 1H), 6.69-6.75 (m, 1H), 6.00 (s, 2H), 5.34 (m, 1H), 4.67-4.70 (d, J=13.5 Hz, 2H), 4.60-4.63 (d, J=15 Hz, 2H), 4.40-4.48 (m, 1H), 3.66-3.78 (m, 5H), 2.48 (m, 1H), 2.24-2.26 (m, 1H), 1.48 (s, 4H), 1.45 (s, 5H). ESI-MS (M+H + ): m/z calculated 435.2. founded 435.3.
Example 8
Synthesis of Compound 4b
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane and stirred at room temperature overnight, followed by adding another compound VIb (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4b (6.1 g), yield 82%.
1 H-NMR for the product 4b (CDCl 3 , 500 MHz): δ 6.81-6.84 (m, 1H), 6.68-6.75 (m, 1H), 5.33 (m, 1H), 4.67 (s, 2H), 4.60 (s, 2H), 4.39-4.48 (m, 1H), 4.30 (m, 2H), 4.28 (m, 2H), 3.63-3.79 (m, 5H), 2.47-2.49 (m, 1H), 2.22-2.26 (m, 1H), 1.48 (s, 4H), 1.45 (s, 5H). ESI-MS (M+H + ): m/z calculated 449.2. founded 449.3.
Example 9
Synthesis of Compound 4c
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane and stirred at room temperature overnight, followed by adding another compound VIc (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4c (6.1 g), yield 82%.
The product 4c was confirmed by ESI-MS (M+H + ): m/z calculated 449.2. founded 449.3.
Example 10
Synthesis of Compound 4d
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane and stirred at room temperature overnight, followed by adding another compound VId (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4d (6.1 g), yield 82%.
The product 4d was confirmed by ESI-MS (M+H + ): m/z calculated 449.2. founded 449.3.
Example 11
Synthesis of Compound 4e
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane and stirred at room temperature overnight, followed by adding another compound VIe (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4e (5.7 g), yield 75%.
1 H-NMR for the product 4e (CDCl 3 , 500 MHz): δ 6.77 (s, 1H), 6.73 (s, 1H), 5.32 (m, 1H), 4.63 (s, 2H), 4.56 (s, 2H), 4.37-4.48 (m, 1H), 4.26 (s, 4H), 3.64-3.79 (m, 5H), 2.47 (m, 1H), 2.21-2.26 (m, 1H), 1.48 (s, 4H), 1.44 (s, 5H). ESI-MS (M+H + ): m/z calculated 449.2. founded 449.3.
Example 12
Synthesis of Compound 4f
SM-4 (5.37 g, 21.9 mmol) and CDI (14.2 g, 87.5 mmol, 4 eq.) were dissolved in 100 mL anhydrous dichloromethane and stirred at room temperature overnight, followed by adding another compound VIf (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 4f (5.9 g), yield 74%.
1 H-NMR for the product 4f (CDCl 3 , 500 MHz): δ 6.71 (s, 1H), 6.67 (s, 1H), 5.97 (s, 2H), 5.32 (m, 1H), 4.63 (s, 2H), 4.57 (s, 2H), 4.38-4.47 (m, 1H), 3.64-3.76 (m, 5H), 2.47 (m, 1H), 2.23-2.25 (m, 1H), 1.47 (s, 4H), 1.44 (s, 5H). ESI-MS (M+H + ): m/z calculated 435.2. founded 435.3.
Example 13
Synthesis of Compound 6a
The product of 4a (2 g, 4.9 mmol) was dissolved in 40 mL 4N HCl/Et 2 O solvent and stirred at 30° C. until the completely deprotecting of Boc to give product 5a.
The concentrated 5a was dissolved in 50 mL DMF, compound SM-5 (1.40 g, 5.14 mmol, 1.05 eq.) and HATU (2.05 g, 5.39 mmol, 1.1 eq.) were added. After cooled in ice bath for 15 minute, DIEA (2.53 g, 19.6 mmol, 4 eq.) was added dropwise, the mixture was warmed to room temperature and stirred overnight until completed (monitored by HPLC-ELSD). The organic layer was separated and the water phase was extracted twice with ethyl acetate (2×100 mL). The combined organic layer as was washed with 1N hydrochloric acid, water, saturated sodium bicarbonate, and brine, dried and evaporated, finally purified by flash column to obtain desired product 6a (2.5 g), yield 87%, confirmed by ESI-MS (M+H + ): m/z calculated: 588.3. founded: 588.3.
Example 14
Synthesis of Compound 7a
The product of 6a (2.3 g, 4.2 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (0.54 g, 12.8 mmol, 3 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 7a (2.18 g), yield >95%, confirmed by ESI-MS (M+H + ): m/z calculated 574.3. founded 574.4.
Example 15
Synthesis of Compound 8
The raw material SM-7 (6.5 g, 18 mmol) was dissolved in HCl/Et 2 O solution (4M, 80 mL) and stirred at 30° C. until completed.
The above de-Boc product was concentrated and dissolved in 150 mL DMF. Compound (L)-N-Boc-2-amino-8-azelaic acid (SM-5, 5.2 g, 19 mmol, 1.05 eq.) and HATU (7.6 g, 20 mmol, 1.1 eq.) were added. After cooled in ice bathed for 15 minute, DIEA (9.5 g, 76 mmol, 4 eq.) was added dropwise, the mixture was warmed to room temperature and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 8 (2.5 g), yield 87%.
1 H-NMR for the product 8 (CDCl3, 500 MHz): δ 7.73 (s, 1H), 5.70-5.79 (m, 2H), 5.27-5.31 (d, 1H, J=17 Hz), 5.22-5.24 δ (d, 1H, J=8 Hz), 5.11-5.13 (m, 1H), 4.93-5.01 (m, 2H), 4.68-4.71 (t, 1H, J=7.5 Hz), 4.54 (br, 1H), 4.36-4.37 (m, 1H), 3.94-3.97 (d, 1H, J=11.5 Hz), 3.65 (s, 3H), 3.55-3.58 (m, 1H), 3.39 (br, 1H), 2.97 (s, 1H), 2.89 (s, 1H), 2.49-2.52 (m, 1H), 2.12-2.16 (m, 1H), 2.02-2.04 (m, 4H), 1.83-1.85 (m, 1H), 1.74-1.78 (m, 1H), 1.59-1.61 (m, 1H), 1.43 (s, 9H), 1.31-1.40 (m, 4H), confirmed by ESI-MS (M+H + ): m/z calculated: 508.3. founded: 508.5.
Example 16
Synthesis of Compound 9a
The two methods of synthesis of compounds 9a-9d shown above.
Method I:
The product 7a (2.0 g, 4 mmol) and vinyl substituted cyclopropyl amino acid methyl ester reagents SM-6 (1.3 g, 4.2 mmol, 1.05 eq.) and the coupling reagent HATU (1.83 g, 4.82 mmol, 1.1 eq.) were dissolved in 80 mL DMF. After cooled in ice bathed for 15 minute, DIEA (2.27 g, 17.5 mmol, 4 eq.) was added dropwise, the mixture was warmed to room temperature and stirred overnight, followed by adding the product VIa (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9a (2.4 g), yield 81%, confirmed by ESI-MS (M+H + ): m/z calculated 699.3. founded 699.4.
Method II:
The product of the above Experiment 9 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL anhydrous dichloromethane and stirred at room temperature overnight. When HPLC-ELSD shows the reaction was completed, the product of Experiment 1 VIa (5.12 mmol, 2 eq.) was added and stirred at room temperature until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9a (1.4 g), yield 86%, confirmed by ESI-MS (M+H + ): m/z calculated: 699.3. founded: 699.4.
Example 17
Synthesis of Compound 9b
The synthesis of compounds 9b adopted method II shown above: the product 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous dichloromethane at room temperature overnight, followed by adding the product VIb (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9b (1.6 g), yield 94%, confirmed by ESI-MS (M+H + ): m/z calculated 711.4. founded 711.5.
Example 18
Synthesis of Compound 9c
The synthesis of compounds 9c adopted method II shown above: the product 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous dichloromethane at room temperature overnight, followed by adding the product VIc (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9c (1.3 g), yield 77%, confirmed by ESI-MS (M+H + ): m/z calculated 711.4. founded 711.5.
Example 19
Synthesis of Compound 9d
The synthesis of compounds 9d adopted method II shown above: the product 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous dichloromethane at room temperature overnight, followed by adding the product VId (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9d (1.3 g), yield 77%, confirmed by ESI-MS (M+H + ): m/z calculated 711.4. founded 711.5.
Example 20
Synthesis of Compound 9e
The synthesis of compounds 9e adopted method II shown above: the product of the above mentioned Experiment 9 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous dichloromethane at room temperature overnight, followed by adding the product VIe (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9e (1.4 g), yield 83%, and confirmed by ESI-MS (M+H + ): m/z calculated 711.4. founded 711.5.
Example 21
Synthesis of Compound 9f
The synthesis of compounds 9f adopted method II shown above: the product 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous dichloromethane at room temperature overnight, followed by adding the product VIf (5.12 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9f (1.3 g), yield 78%, and confirmed by ESI-MS (M+H + ): m/z calculated: 697.3. founded: 697.4.
Example 22
Synthesis of Compound 9-Ref
Synthesis of compounds 9-Ref adopted method II shown above: the product 8 (1.3 g, 2.56 mmol) and CDI (1.66 g, 10.2 mmol, 4 eq.) were dissolved in 50 mL of anhydrous DCE at room temperature overnight, followed by adding another compound SM-8 (43.7 mmol, 2 eq.) until completed. The reaction mixture was worked out and purified by flash column to obtain the product 9e (1.4 g), yield 81%.
1 H-NMR for the product 9-Ref (CDCl 3 , 500 MHz): δ 7.65-7.70 (d, 1H, J=9 Hz), 6.96-7.07 (m, 2H), 5.72-5.78 (m, 2H), 5.40 (br, 1H), 5.28-5.31 (d, 1H, J=16.5 Hz), 5.12-5.14 (d, 1H, J=10.5 Hz), 5.07-5.09 (d, 1H, J=7.5 Hz), 4.93-5.00 (m, 2H), 4.64-4.79 (m, 5H), 4.36-4.37 (m, 1H), 4.06 (m, 1H), 3.72-3.75 (m, 1H), 3.67 (s, 3H), 2.78 (m, 1H), 2.26 (m, 1H), 2.14-2.16 (m, 1H), 2.01-2.03 (m, 2H), 1.86-1.88 (m, 1H), 1.70-1.73 (m, 1H), 1.57-1.60 (m, 1H), 1.45-1.49 (m, 2H), 1.37-1.40 (m, 4H), 1.32 (s, 4H), 1.29 (s, 5H), and confirmed by Mass spectrometry, ESI-MS (M+H + ): m/z calculated 691.3. founded 691.4.
Example 23
Synthesis of Compound 10a
Under argon protection atmosphere, compound 9a (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10a (1.2 g), yield 64%, and confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.4.
Example 24
Synthesis of Compound 10b
Under argon protection atmosphere, compound 9b (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10b (1.3 g), yield 67%, and confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.5.
Example 25
Synthesis of Compound 10e
Under argon protection atmosphere, compound 9c (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10c (1.2 g), yield 56%, and confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.5.
Example 2
Synthesis of Compound 10d
Under argon protection atmosphere, compound 9d (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10d (1.3 g), yield 61%, and confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.5.
Example 27
Synthesis of Compound 10e
Under argon protection atmosphere, compound 9e (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10e (1.1 g), yield 51%, and confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.5.
Example 28
Synthesis of Compound 10f
Under argon protection atmosphere, compound 9f (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10f (0.9 g), yield 47%, and confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.4.
Example 29
Synthesis of Compound 10-Ref
Under argon protection atmosphere, compound 9-Ref (2.25 mmol) was dissolved in 450 mL of anhydrous dichloromethane, and Zhan Catalyst-1B (RC-303, 74.4 mg, 0.113 mmol, 0.05 eq.) was added. The reaction flask was stirred in a preheated oil bath at 80° C. overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 10-Ref (1.4 g), yield 71%.
1 H-NMR for the product 10-Ref (CDCl 3 , 500 MHz): δ 6.96-7.07 (m, 3H), 5.53-5.55 (m, 1H), 5.39 (m, 1H), 5.23-5.28 (m, 2H), 4.69-4.84 (m, 5H), 4.49 (m, 1H), 4.05-4.07 (m, 1H), 3.86-3.89 (m, 1H), 3.67 (s, 3H), 2.82-2.85 (m, 1H), 2.25-2.27 (m, 1H), 2.16-2.19 (m, 3H), 1.85-1.88 (m, 2H), 1.56-1.73 (m, 3H), 1.38-1.43 (m, 4H), 1.35 (s, 4H), 1.34 (s, 5H), and confirmed by ESI-MS (M+H + ): m/z calculated 643.3. founded 643.5.
Example 30
Synthesis of Compound 11a
The compound 10a (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11a (466 mg), yield >95%, and confirmed by ESI-MS (M+H + ): m/z calculated 655.3. founded 655.3.
Example 31
Synthesis of Compound 11b
The compound 10b (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11b (439 mg), yield >95%, and confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.3.
Example 32
Synthesis of Compound 11c
The compound 10c (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11c (453 mg), yield >95%, and confirmed by ESI-MS (M+H + ): m/z calculated 673.3. founded 673.3.
Example 33
Synthesis of Compound 11d
The compound 10d (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11d (457 mg), yield >95%, and confirmed by ESI-MS (M+H + ): m/z calculated 673.3. founded 673.3.
Example 34
Synthesis of Compound 11e
The compound 10e (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11e (418 mg), yield 85%, and confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.3.
Example 35
Synthesis of Compound 11f
The compound 10f (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11f (453 mg), yield >95%, and confirmed by ESI-MS (M+H + ): m/z calculated 655.3. founded 655.4.
Example 36
Synthesis of Compound 11j
Compound 10e (0.55 g, 0.81 mmol) was suspended in 10 mL 4N HCl/ether solvent, stirred for 2 h and concentrated. 10 mL DCM and triethylamine (0.82 g, 8 mmol) were added and cooled to 0-5° C. The raw material sulfonyl chloride (0.29 g, 1.6 mmol) was added slowly and the reaction was stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column, and the product 13j (0.43 g, yield: 73%).
Compound 13j (0.4 g) was to added to the mixture solvent of NaOH (120 mg, 3 mmol), 10 mL methanol and 0.5 mL of water. The reaction mixture was stirred at 60° C. for 5 hr until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11j (0.31 g, yield: 80%).
1 H-NMR for the product 11j (CDCl 3 , 500 MHz): δ 7.30 (s, 1H); 6.76 (s, 1H); 6.68 (s, 1H); 5.69 (q, J=8.0 Hz, 1H); 5.48 (s, 1H); 5.15 (t, J=8.0 Hz, 1H); 4.63-4.48 (m, 5H); 4.24 (s, 4H); 4.23-4.14 (m, 2H); 3.86 (m, 1H); 3.71 (m, 1H); 3.39 (m, 1H); 3.07-2.91 (m, 2H); 2.57 (m, 1H); 2.44 (m, 1H); 2.36-2.22 (br, 4H); 2.04 (m, 1H); 1.93 (m, 1H); 1.81 (m, 1H); 1.64-1.55 (br, 3H); 1.46-1.29 (br, 4H); 1.24-1.20 (br, 2H), and confirmed by ESI-MS (M+H + ): m/z calculated 673.2. founded 673.3.
Example 37
Synthesis of Compound 11k
The synthesis of compound 11k was the same as 11j.
Compound 10f (0.55 g, 0.81 mmol) was suspended in 10 mL 4N HCl/ether solvent, stirred for 2 h and concentrated. 10 mL DCM and triethylamine (0.82 g, 8 mmol) were added and cooled to 0-5° C. The raw material sulfonyl chloride (0.29 g, 1.6 mmol) was added slowly and the reaction was stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column, and the product 13k (0.48 g, yield: 91%).
Compound 13k (0.4 g) was added to the mixture solvent of NaOH (120 mg, 3 mmol), 10 mL methanol and 0.5 mL of water. The reaction mixture was stirred at 60° C. for 5 hr until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11k (0.30 g, yield: 78%).
1 H-NMR for the product 11k (CDCl 3 , 500 MHz): δ 7.32 (s, 1H); 6.71 (s, 1H); 6.63 (s, 1H); 5.96 (s, 2H); 5.69 (q, J=8.0 Hz, 1H); 5.48 (s, 1H); 5.15 (t, J=8.0 Hz, 1H); 4.64-4.49 (m, 5H); 4.23-4.15 (m, 2H); 3.89 (m, 1H); 3.72 (m, 1H); 3.40 (m, 1H); 3.09-2.89 (m, 2H); 2.58 (m, 1H); 2.48 (m, 1H); 2.39-2.26 (br, 4H); 2.08 (m, 1H); 1.96 (m, 1H); 1.82 (m, 1H); 1.69-1.54 (br, 3H); 1.46-1.29 (br, 4H); 1.26-1.20 (br, 2H) and confirmed by ESI-MS (M+H + ): m/z calculated 659.2. founded 659.3.
Example 38
Synthesis of Compound 11m
The synthesis of compound 11m was the same as 11j.
Compound 10-Ref (0.55 g, 0.81 mmol) was suspended in 10 mL 4N HCl/ether solvent, stirred for 2 h and concentrated. 10 mL DCM and triethylamine (0.82 g, 8 mmol) were added and cooled to 0-5° C. The raw material sulfonyl chloride (0.29 g, 1.6 mmol) was added slowly and the reaction was stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column, and the product 13m (0.35 g, yield: 65%).
Compound 13m (0.3 g) was added to the mixture solvent of NaOH (120 mg, 3 mmol), 10 mL methanol and 0.5 mL of water. The reaction mixture was stirred at 60° C. for 5 hr until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11m (0.21 g, yield: 76%).
1 H-NMR for the product 11m (CDCl 3 , 500 MHz): δ 7.25 (m, 1H); 7.06-6.95 (m, 2H); 5.71 (q, J=8.0 Hz, 1H); 5.49 (s, 1H); 5.32 (s, 1H); 5.14 (t, J=8.0 Hz, 1H); 4.80-4.4.61 (m, 5H); 4.31 (m, 1H); 4.16 (m, 1H); 3.86 (m, 1H); 3.72 (q, J=5.6 Hz, 1H); 3.40 (q, J=5.6 Hz, 1H); 3.02 (m, 1H); 2.92 (m, 1H); 2.61 (br, 1H); 2.52-2.41 (br, 2H); 2.33-2.24 (br, 3H); 2.06 (br, 1H); 1.93 (br, 1H); 1.83 (br, 1H); 1.63-1.54 (br, 3H); 1.42-1.22 (br, 6H) and confirmed by ESI-MS (M+H + ): m/z calculated 633.2. founded 633.3.
Example 39
Synthesis of Compound 11-Ref
Synthesis of compound 11-Ref was the same as 11a.
The compound 10-Ref (0.6 mmol) was dissolved in 30 mL THF, 15 mL methanol and 15 mL water. Lithium hydroxide monohydrate (122.9 mg, 2.93 mmol, 5 eq.) was added and stirred overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 11-Ref (438 mg), yield >95%.
1 H-NMR for the product 11-Ref (CDCl 3 , 500 MHz): δ 7.16 (m, 1H), 6.96-7.07 (m, 2H), 5.63-5.64 (m, 1H), 5.32 (m, 1H), 5.20-5.28 (m, 2H), 4.68-4.78 (m, 5H), 4.34-4.40 (m, 1H), 4.19 (m, 1H), 3.89 (m, 1H), 2.68-2.78 (m, 1H), 2.32 (m, 2H), 2.21 (m, 1H), 2.10 (m, 1H), 1.84-1.87 (m, 2H), 1.59-1.62 (m, 2H), 1.40-1.45 (m, 5H), 1.32 (s, 4H), 1.30 (s, 5H) and confirmed by ESI-MS (M+H + ): m/z calculated 629.3. founded 629.4.
Example 40
Synthesis of Compound 12a
Compound 11a (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture above was dissolved in 10 mL of anhydrous DCE, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12a (56 mg; Yield: 58%).
1 H-NMR for the product 12a (CDCl 3 , 500 MHz): δ 10.29-10.30 (d, 1H), 6.97-7.02 (d, 2H), 6.60-6.78 (m, 2H), 5.98-5.99 (m, 2H), 5.70-5.73 (m, 1H), 5.47 (m, 1H), 4.98-5.08 (m, 2H), 4.56-4.70 (m, 5H), 4.37-4.40 (m, 1H), 4.21-4.23 (m, 1H), 3.84-3.86 (m, 1H), 2.90-2.93 (m, 1H), 2.50-2.56 (m, 2H), 2.46-2.48 (m, 1H), 2.25-2.28 (m, 1H), 1.89-1.95 (m, 2H), 1.74-1.79 (m, 2H), 1.46-1.58 (m, 6H), 1.36-1.39 (m, 2H), 1.29 (s, 4H), 1.25 (s, 5H), 1.08-1.16 (m, 2H), 0.90-0.95 (m, 1H); and confirmed by ESI-MS (M+H + ): m/z calculated 758.3. founded 758.4.
Example 41
Synthesis of Compound 12b
Compound 11b (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12b (53 mg; Yield: 51%).
1 H-NMR for the product 12b (CDCl 3 , 500 MHz): δ 10.25-10.25 (d, 1H), 6.88-6.91 (m, 1H), 6.77-6.80 (m, 1H), 6.58-6.60 (m, 1H), 5.68-5.74 (m, 1H), 5.45 (m, 1H), 4.98-5.06 (m, 2H), 4.64-4.68 (m, 2H), 4.52-4.60 (m, 3H), 4.35-4.39 (m, 1H), 4.22-4.29 (m, 5H), 3.82-3.84 (m, 1H), 2.88-2.91 (m, 1H), 2.45-2.56 (m, 2H), 2.41-2.45 (m, 1H), 2.23-2.29 (m, 1H), 1.82-1.93 (m, 1H), 1.60-1.79 (m, 3H), 1.36-1.56 (m, 8H), 1.23-1.29 (m, 9H), 0.93-1.06 (m, 2H), 0.89-0.93 (m, 1H); and confirmed by ESI-MS (M+H + ): m/z calculated 772.3. founded 773.4.
Example 42
Synthesis of Compound 12c
Compound 11e (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12c (47 mg; Yield: 42%).
1 H-NMR for the product 12c (CDCl 3 , 500 MHz): δ 10.27 (s, 1H), 6.92 (s, 1H), 6.77 (s, 1H), 6.65 (s, 1H), 5.72-5.73 (m, 1H), 5.46 (m, 1H), 5.09 (m, 1H), 5.00 (m, 1H), 4.64 (m, 2H), 4.53-4.56 (m, 3H), 4.37-4.40 (m, 1H), 4.25 (m, 5H), 3.84-3.86 (m, 1H), 2.90 (m, 1H), 2.46-2.53 (m, 3H), 2.27-2.29 (m, 1H), 1.87-1.94 (m, 2H), 1.72 (m, 2H), 1.58 (m, 1H), 1.47 (m, 5H), 1.38 (m, 2H), 1.31 (s, 9H), 1.11 (m, 2H), 0.91 (m, 1H); and confirmed by ESI-MS (M+H + ): m/z calculated 772.3. founded 773.4.
Example 43
Synthesis of Compound 12d
Compound 11f (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12d (65 mg; Yield: 67%).
1 H-NMR for the product 12d (CDCl 3 , 500 MHz): δ 10.24 (s, 1H), 6.80 (s, 1H), 6.72 (s, 1H), 6.59 (s, 1H), 5.98 (s, 2H), 5.70-5.76 (m, 1H), 5.47 (m, 1H), 5.03 (m, 2H), 4.65 (m, 2H), 4.53-4.57 (m, 3H), 4.38-4.41 (m, 1H), 4.23 (m, 1H), 3.85 (d, 1H), 2.92 (m, 1H), 2.51-2.57 (m, 2H), 2.45 (m, 1H), 2.28 (m, 1H), 1.95 (m, 2H), 1.59 (m, 1H), 1.59-1.65 (m, 2H), 1.48 (m, 5H), 1.38 (m, 2H), 1.30 (s, 9H), 1.12 (m, 2H), 0.92 (m, 1H).
ESI-MS (M+H + ): m/z calculated 758.3. founded 758.5.
Example 44
Synthesis of Compound 12e
Compound 11a (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=isopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12e (53 mg; Yield: 49%).
1 H-NMR for the product 12e (CDCl 3 , 500 MHz): δ 9.91-9.93 (d, 1H), 6.72-6.83 (m, 3H), 5.95-5.99 (m, 2H), 5.72-5.73 (m, 1H), 5.47 (m, 1H), 4.99-5.05 (m, 2H), 4.57-4.71 (m, 5H), 4.40-4.42 (m, 1H), 4.22 (m, 1H), 3.83-3.85 (d, 1H), 3.70-3.72 (m, 1H), 2.55-2.57 (m, 2H), 2.46-2.48 (m, 1H), 2.27-2.30 (m, 1H), 1.97 (m, 1H), 1.76-1.86 (m, 3H), 1.42-1.46 (m, 6H), 1.32-1.37 (m, 4H), 1.24-1.28 (d, 9H), 0.89-0.91 (m, 3H). ESI-MS (M+H + ): m/z calculated 760.3. founded 760.4.
Example 45
Synthesis of Compound 12f
Compound 11b (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=isopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12f (50 mg; Yield: 46%).
1 H-NMR for the product 12f (CDCl 3 , 500 MHz): δ 9.94 (s, 1H), 6.73-6.78 (m, 2H), 6.59-6.73 (m, 1H), 5.69-5.75 (m, 1H), 5.47 (m, 1H), 4.99-5.05 (m, 2H), 4.63-4.67 (m, 2H), 4.42-4.53 (m, 3H), 4.29-4.38 (m, 1H), 4.25-4.29 (m, 5H), 3.83-3.86 (m, 1H), 3.68-3.75 (m, 1H), 2.53-2.58 (m, 2H), 2.43-2.48 (m, 1H), 2.28-2.30 (m, 1H), 1.96-2.00 (m, 1H), 1.69-1.93 (m, 3H), 1.42-1.47 (m, 6H), 1.32-1.44 (m, 4H), 1.24-1.29 (m, 9H), 0.86-0.93 (m, 3H); and confirmed by ESI-MS (M+H + ): m/z calculated 774.3. founded 774.4.
Example 46
Synthesis of Compound 12g
Compound 11c (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=isopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out to obtain the white solid product 12g (45 mg; Yield: 38%).
1 H-NMR for the product 12g (CDCl 3 , 500 MHz): δ 9.91 (s, 1H), 6.77-6.78 (m, 2H), 6.65 (s, 1H), 5.69-5.75 (m, 1H), 5.47 (m, 1H), 5.01-5.03 (m, 2H), 4.60-4.64 (m, 2H), 4.53-4.60 (m, 3H), 4.39-4.42 (m, 1H), 4.26 (m, 5H), 3.84-3.85 (m, 1H), 3.69-3.72 (m, 1H), 2.54-2.56 (m, 2H), 2.43-2.48 (m, 1H), 2.28-2.29 (m, 1H), 1.96 (m, 1H), 1.74-1.86 (m, 2H), 1.59 (m, 1H), 1.37-1.43 (m, 7H), 1.32-1.33 (m, 15H); and confirmed by ESI-MS (M+H + ): m/z calculated 774.3. founded 774.4.
Example 47
Synthesis of Compound 12h
Compound 11d (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=isopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12h (53 mg; Yield: 48%).
1 H-NMR for the product 12h (CDCl 3 , 500 MHz): δ 9.95 (s, 1H), 6.90 (s, 1H), 6.71 (s, 1H), 6.59 (s, 1H), 5.98 (s, 2H), 5.73 (m, 1H), 5.47 (m, 1H), 5.04 (m, 2H), 4.65 (m, 2H), 4.53-4.57 (m, 3H), 4.39-4.41 (m, 1H), 4.23 (m, 1H), 3.84-3.85 (d, 1H), 3.70 (m, 1H), 2.53 (m, 2H), 2.48 (m, 1H), 2.28 (m, 1H), 1.95 (m, 1H), 1.76-1.86 (m, 3H), 1.57 (m, 1H), 1.41-1.46 (m, 7H), 1.30 (m, 15H); and confirmed by ESI-MS (M+H + ): m/z calculated 760.3. founded 760.4.
Example 48
Synthesis of Compound 12j
Compound 11j (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12j (73 mg; Yield: 61%).
1 H-NMR for the product 12j (CDCl 3 , 500 MHz): δ 10.35 (s, 1H), 7.35 (s, 1H), 6.74 (s, 1H), 6.67 (s, 1H), 5.72-5.77 (q, 1H, J=8.5 Hz), 5.52 (m, 1H), 5.00-5.04 (t, 1H, J=9.5 Hz), 4.57-4.64 (m, 2H), 4.46-4.57 (m, 3H), 4.23-4.25 (m, 5H), 4.08-4.11 (d, 1H), 3.88-3.90 (m, 1H), 3.65-3.69 (m, 1H), 3.32-3.37 (m, 1H), 2.92-3.05 (m, 2H), 2.88-2.92 (m, 1H), 2.66-2.74 (m, 1H), 2.40-2.53 (m, 2H), 2.26-2.35 (m, 3H), 1.80-2.05 (m, 3H), 1.48-1.68 (m, 3H), 1.26-1.48 (m, 6H), 1.08-1.13 (m, 2H), 0.90-0.94 (m, 1H). ESI-MS (M+H + ): m/z calculated 776.3. founded 776.4.
Example 49
Synthesis of Compound 12k
Compound 11k (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12k (54 mg; Yield: 38%).
1 H-NMR for the product 12k (CDCl 3 , 500 MHz): δ 10.36 (s, 1H), 7.39 (s, 1H), 6.70 (s, 1H), 6.64 (s, 1H), 5.97 (s, 2H), 5.74-5.76 (m, 2H), 5.53 (m, 1H), 5.01-5.05 (t, 1H, J=9.5 Hz), 4.46-4.64 (m, 5H), 4.24-4.26 (d, 1H), 4.10-4.13 (m, 1H), 3.88-3.91 (m, 1H), 3.66-3.68 (m, 1H), 3.33-3.38 (m, 1H), 2.90-3.03 (m, 3H), 2.71 (m, 1H), 2.49-2.51 (m, 1H), 2.42-2.45 (m, 1H), 2.28-2.34 (m, 3H), 1.81-2.02 (m, 4H), 1.62-1.69 (m, 4H), 1.44-1.49 (m, 4H), 1.08-1.14 (m, 2H), 0.86-0.96 (m, 1H). ESI-MS (M+H + : m/z calculated 762.2. founded 762.3.
Example 50
Synthesis of Compound 12m
Compound 11m (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12m (61 mg; Yield: 52%).
1 H-NMR for the product 12m (CDCl 3 , 500 MHz): δ 10.38-10.41 (d, 1H), 7.51-7.55 (d, 1H, J=20 Hz), 6.94-7.05 (m, 2H), 5.73-5.79 (m, 2H), 5.54 (m, 1H), 5.02-5.06 (t, 1H, J=9.5 Hz), 4.75-4.85 (m, 2H), 4.54-4.64 (m, 3H), 4.29-4.33 (t, 1H, J=11 Hz), 4.08-4.10 (d, 1H), 3.85-3.89 (m, 1H), 3.65-3.68 (m, 1H), 3.31-3.36 (m, 3H), 2.73-2.74 (m, 1H), 2.51-2.52 (m, 2H), 2.27-2.36 (m, 3H), 1.72-2.02 (m, 4H), 1.27-1.66 (m, 9H), 1.09-1.13 (m, 2H), 0.91-0.95 (m, 1H). ESI-MS (M+H): m/z calculated 736.2. founded 736.4.
Example 51
Synthesis of Compound 12n
Compound 11c (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12n (47 mg; Yield: 42%).
1 H-NMR for the product 12n (CDCl 3 , 500 MHz): δ10.27 (s, 1H), 6.89-6.92 (m, 2H), 6.67-6.79 (m, 1H), 5.72-5.74 (m, 1H), 5.46-5.47 (m, 1H), 4.99-5.07 (m, 2H), 4.55-4.69 (m, 5H), 4.39 (m, 1H), 4.21-4.25 (m, 5H), 3.84-3.86 (m, 1H), 2.90-2.93 (m, 1H), 2.45-2.56 (m, 3H), 2.19-2.29 (m, 3H), 1.89-1.95 (m, 2H), 1.71-1.79 (m, 2H), 1.58 (m, 1H), 1.34-1.50 (m, 7H), 1.29 (s, 5H), 1.25 (s, 4H), 1.08-1.16 (m, 2H), 0.92-0.94 (m, 1H). ESI-MS (M+H + ): m/z calculated 786.3. founded 786.4.
Example 52
Synthesis of Compound 12p
Compound 11d (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid mixture was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.36 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12p (65 mg; Yield: 67%).
1 H-NMR for the product 12p (CDCl 3 , 500 MHz): δ 10.28 (s, 1H), 7.00 (s, 1H), 6.87 (s, 1H), 6.75 (s, 1H), 5.70-5.72 (m, 1H), 5.45 (m, 1H), 4.97-5.09 (m, 2H), 4.52-4.63 (m, 5H), 4.35-4.38 (m, 1H), 4.14-4.22 (m, 5H), 3.83-3.84 (m, 1H), 2.88-2.91 (m, 1H), 2.44-2.53 (m, 3H), 2.17-2.27 (m, 3H), 1.76-1.91 (m, 4H), 1.57 (m, 1H), 1.37-1.51 (m, 7H), 1.28 (s, 9H), 1.06-1.13 (m, 2H), 0.89-0.93 (m, 1H). ESI-MS (M+H + : m/z calculated 786.3. founded 786.4.
Example 53
Synthesis of Compound 12q
Compound 12d (0.18 mmol) was dissolved in 20 mL HCl-Et 2 O (2N) and stirred at 30° C. until completed to obtain de-Boc product, followed by reacting with another reagent iPrOC(O)Cl (1.2 eq) to obtain the product 12q. yield: 72%.
1 H-NMR for the product 12q (CDCl 3 , 500 MHz): δ10.27 (s, 1H), 6.97 (br, 1H), 6.70 (s, 1H), 6.59 (s, 1H), 5.95 (s, 2H), 5.70 (q, J=8.1 Hz, 1H), 5.44 (s, 1H), 5.14 (s, 1H), 4.99 (t, J=8.1 Hz, 1H), 4.65-4.47 (m, 5H), 4.35 (m, 2H), 4.24 (br, 1H), 3.82 (m, 1H), 2.91 (m, 1H), 2.45 (m, 3H), 2.23 (m, 1H), 1.92 (br, 2H), 1.74 (br, 2H), 1.59 (m, 1H), 1.47-1.27 (br, 8H), 1.11-1.06 (br, 5H), 1.01 (d, J=4.7 Hz, 3H), 0.96 (m, 1H). ESI-MS (M+H + ): m/z calculated 744.3. founded 744.3.
Example 54
Synthesis of Compound 12r
Compound 12d (0.18 mmol) was dissolved in 20 mL HCl-Et 2 O (2N) and stirred at 30° C. until completed to obtain de-Boc product, followed by reacting with another reagent iPrOC(O)Cl (1.2 eq) to obtain the product 12r. yield: 76%.
1 H-NMR for the product 12r (CDCl 3 , 500 MHz): δ 10.35 (s, 1H), 7.26 (s, 1H), 6.68 (s, 1H), 6.57 (s, 1H), 5.92 (s, 2H), 5.67 (q, J=8.1 Hz, 1H), 5.42 (s, 1H), 4.95 (t, J=8.1 Hz, 1H), 4.58 (m, 5H), 4.29 (m, 2H), 3.81 (m, 1H), 2.86 (m, 1H), 2.42 (br, 3H), 2.24 (m, 1H), 1.77 (m, 4H), 1.58-1.25 (m, 18H), 1.07 (m, 2H), 0.90 (m, 1H). ESI-MS (M+H + ): m/z calculated 770.3. founded 770.4.
Example 55
Synthesis of Compound 12s
The synthetic procedure is the same as in Examples 48-50 starting 10f with in 0.3 mmol scale. Finally, 32 mg of product 12s was obtained, and confirmed by ESI-MS (M+H + ): m/z calculated 770.3. founded 770.4.
Example 56
Synthesis of Compound 12t
The synthetic procedure is the same as in Examples 48-50 starting 10f with in 0.3 mmol scale. Finally, 41 mg of product 12s was obtained, and confirmed by ESI-MS (M+H + ): m/z calculated 770.3. founded 770.4.
Example 57
Synthesis of Compound 12u
The synthetic procedure is the same as in Examples 48-50 starting 10-Ref with in 0.3 mmol scale. Finally, 52 mg of product 12u was obtained, and confirmed by ESI-MS (M+H + ): m/z calculated 810.3. founded 810.4.
Example 58
Synthesis of Compound 12-Ref
Compound 11-Ref (0.18 mmol) was dissolved in 10 mL anhydrous dichloromethane, EDCI (69.8 mg, 0.36 mmol, 2 eq.) was added and stirred at room temperature overnight until completed. The reaction mixture was worked out and concentrated.
The obtained solid was dissolved in 10 mL of anhydrous dichloromethane, DBU (61.0 mg, 0.40 mmol) and RSO 2 NH 2 (0.363 mmol, R=cyclopropyl) were added and stirred at room temperature overnight until completed. The reaction mixture was worked out and purified by flash column to obtain the product 12-Ref (62 mg; Yield: 53%).
1 H-NMR for the product 12-Ref (CDCl3, 500 MHz): δ 10.28-10.29 (d, 1H), 6.87-7.07 (m, 3H), 5.72-5.74 (m, 1H), 5.48 (br, 1H), 4.99-5.03 (m, 2H), 4.58-4.79 (m, 5H), 4.42 (m, 1H), 4.21 (m, 1H), 3.83-3.85 (m, 1H), 2.90-2.93 (m, 1H), 2.48-2.57 (m, 3H), 2.27-2.30 (m, 1H), 1.88-1.97 (m, 2H), 1.67-1.79 (m, 2H), 1.45-1.58 (m, 6H), 1.34-1.40 (m, 2H), 1.27 (s, 4H), 1.24 (s, 5H), 1.08-1.15 (m, 2H), 0.91-0.94 (m, 1H). ESI-MS (M+H + ): m/z calculated 732.3. founded 732.5.
Example 59
Synthesis of Compound 15a
Compound 12d (3.0 mmol) was dissolved in 30 mL HCl-Et2O (4N) to remove Boc group, followed by adding phenyl borate and Cu(AcO)2 (2 eq/each) in DCE (30 mL) to obtain the product 15a (Yield: 62%). ESI-MS (M+H + ): m/z calculated 734.3. founded 734.4.
Example 60
Synthesis of Compound 15b
Compound 12d (3.0 mmol) was dissolved in 30 mL HCl-Et2O (4N) to remove Boc group, followed by adding m-fluorophenyl borate and Cu(AcO)2 (2 eq/each) in DCE (30 mL) to obtain the product 15b (Yield: 53%). ESI-MS (M+H + ): m/z calculated 752.3. founded 752.3.
Example 61
Synthesis of Compound 16a
Compound 12d (3.0 mmol) was dissolved in 30 mL HCl-Et2O (4N) to remove Boc group, followed by adding p-chlorophenylsulfonyl chloride (1.3 eq) in DCE (30 mL) to obtain the product 16a (Yield: 81%). ESI-MS (M+H + ): m/z calculated 832.2. founded 832.2.
Example 62
Synthesis of Compound 16b
Compound 12d (3.0 mmol) was dissolved in 30 mL HCl-Et2O (4N) to remove Boc group, followed by adding phenylsulfonyl chloride (1.3 eq)) in DCE (30 mL) to obtain the product 16b (Yield: 74%). ESI-MS (M+H + ): m/z calculated 798.2. founded 798.3.
Example 63
Synthesis of Compound 16c
Compound 12d (3.0 mmol) was dissolved in 30 mL HCl-Et2O (4N) to remove Boc group, followed by adding p-methoxyphenylsulfonyl chloride (1.3 eq) in DCE (30 mL) to obtain the product 16c (Yield: 79%). ESI-MS (M+H + ): m/z calculated: 828.2. founded: 828.3.
Example 64
Synthesis of Compound 17
SM-11 (35 g), DMF (350 mL) were added to a flask, followed by adding SM-12 (17 g) and HATU (10.4 g) into the reaction mixture in ice-water bath. After stirred for 10 minutes, DIEA (125 mL) was added, the mixture was allowed to room temperature. The mixture was stirred overnight and concentrated under reduced pressure. The reaction mixture was worked out and purified by flash column to obtain the foamy solid product 17 (18.6 g). Confirmed by ESI-MS (M+H + ): m/z calculated 407.3. founded 407.5.
Example 65
Synthesis of Compound 21a
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21a. After purification, 59 mg of product 21a was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.4.
Example 66
Synthesis of Compound 21b
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21b. After purification, 46 mg of product 21b was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.4.
Example 67
Synthesis of Compound 21c
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21c. After purification, 49 mg of product 21c was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 643.3. founded 643.4.
Example 68
Synthesis of Compound 21d
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21d. After purification, 63 mg of product 21d was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 683.3. founded 683.4.
Example 69
Synthesis of Compound 21e
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21e. After purification, 63 mg of product 21e was obtained.
1 H-NMR for the product 21e (CDCl 3 , 500 MHz): δ 10.60 (s, 1H), 7.10 (s, 1H), 6.61-6.74 (m, 3H), 5.95 (s, 2H), 5.65-5.69 (m, 1H), 5.26-5.29 (m, 1H), 4.98-5.09 (m, 1H), 4.65-4.68 (m, 1H), 4.41-4.56 (m, 4H), 3.88-3.91 (m, 1H), 3.47-3.53 (m, 2H), 3.19-3.26 (m, 1H), 3.07 (s, 1H), 2.96-3.01 (m, 1H), 2.90 (s, 3H), 2.50-2.64 (m, 1H), 2.24-2.28 (m, 1H), 2.04-2.16 (m, 3H), 1.67-1.99 (m, 4H), 1.08-1.49 (m, 8H), 0.86-0.96 (m, 2H). ESI-MS (M+H + ): m/z calculated 657.3. founded 657.4
Example 70
Synthesis of Compound 21f
The synthetic procedure starting with intermediate 17 is the same as in Examples 16-47 for preparation of 12a-12h in 1.0 mmol scale to prepare 21f. After purification, 63 mg of product 21f was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 669.3. founded 669.5.
Example 71
Synthesis of Compound 27a
The synthetic procedure starting with SM-7 in 5.0 mmol scale is the same as in Examples 7-47 for preparation of 12a-12h to prepare 27a. After purification, 69 mg of product 27a was obtained.
1 H-NMR for the product 27a (CDCl 3 , 500 MHz): δ 6.71 (s, 1H), 6.66 (s, 1H), 5.97-5.98 (s, 2H), 5.70-5.73 (m, 1H), 5.31-5.37 (m, 1H), 5.13-5.17 (m, 1H), 4.83-4.86 (m, 1H), 4.51-4.62 (m, 4H), 3.80-3.83 (m, 1H), 3.78-3.79 (m, 1H), 3.52-3.54 (m, 1H), 3.06-3.09 (m, 1H), 2.90 (s, 3H), 2.48-2.49 (m, 1H), 2.23-2.35 (m, 2H), 2.00-2.08 (m, 4H), 1.63-1.72 (m, 2H), 1.38-1.51 (m, 8H), 1.80-1.82 (m, 3H). ESI-MS (M+H + ): m/z calculated 658.3. founded 658.4.
Example 72
Synthesis of Compound 27b
The synthetic procedure starting with SM-7 in 5.0 mmol scale is the same as in Examples 7-47 for preparation of 12a-12h to prepare 27b. After purification, 83 mg of product 27b was obtained.
1 H-NMR for the product 27b (CDCl 3 , 500 MHz): δ 6.72-6.76 (m, 2H), 5.71-5.72 (m, 1H), 5.36-5.37 (m, 1H), 5.15-5.17 (m, 1H), 4.84-4.85 (m, 1H), 4.53-4.61 (m, 4H), 4.25 (s, 4H), 3.79-3.82 (m, 2H), 3.51-3.53 (m, 1H), 2.93-3.04 (m, 2H), 2.89 (s, 3H), 2.48-2.49 (m, 1H), 2.24-2.35 (m, 2H), 1.93-2.03 (m, 3H), 1.69-1.73 (m, 1H), 1.49-1.51 (m, 2H), 1.27-1.38 (m, 3H), 1.06-1.14 (m, 2H), 0.80-0.88 (m, 3H). ESI-MS (M+H + ): m/z calculated 672.3. founded 672.4.
Example 73
Synthesis of Compound 27c
The synthetic procedure starting with SM-7 in 5.0 mmol scale is the same as in Examples 7-47 for preparation of 12a-12h to prepare 27c. After purification, 57 mg of product 27c was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 630.3. founded 630.5
Example 74
Synthesis of Compound 27-Ref
The synthetic procedure starting with SM-7 in 5.0 mmol scale is the same as in Examples 7-47 for preparation of 12a-12h to prepare 27-Ref. After purification, 89 mg of product 27-Ref was obtained.
1 H-NMR for the product 21e (CDCl 3 , 500 MHz): δ 7.41-7.43 (m, 1H), 6.96-7.07 (m, 2H), 5.71-5.73 (m, 1H), 5.38-5.39 (m, 1H), 5.13-5.18 (m, 1H), 4.84-4.88 (m, 1H), 4.73-4.77 (m, 2H), 4.67-4.70 (m, 2H), 3.80-3.84 (m, 1H), 3.65-3.68 (m, 1H), 3.52-3.56 (m, 1H), 3.06-3.09 (m, 1H), 2.93-2.96 (m, 1H), 2.89 (s, 3H), 2.49-2.52 (m, 2H), 2.24-2.36 (m, 2H), 2.00-2.10 (m, 2H), 1.68-1.69 (m, 2H), 1.48-1.51 (m, 2H), 1.27-1.38 (m, 5H), 1.07-1.31 (m, 2H). ESI-MS (M+H + ): m/z calculated 632.3. founded 632.4.
Example 75
Synthesis of Compound 27-Ref-2
The synthetic procedure starting with SM-7 in 5.0 mmol scale is the same as in Examples 7-47 for preparation of 12a-12h to prepare 27-Ref-2. After purification, 61 mg of product 27-Ref-2 was obtained. Confirmed by ESI-MS (M+H + ): m/z calculated 658.3. founded 658.4.
Example 76
Synthesis of Compound 30a
Chemical SM-13a (5.4 g, 10 mmol), sulfonamide (SM-8a, 1.1 eq) and DMF (80 mL) were added into 250 mL flask reactor, followed by adding coupling reagent EDCI (1.3 eq) to keep the amidation at 55° C. until completed. The reaction mixture was worked out to obtain crude product 28a, followed by removing Boc group with HCl-THF solution to obtain 29a (3.7 g, yield: 83%), which was purified by precipitation in hexane-EtOAc and dried directly for next step. ESI-MS (M+H + ): m/z calculated 533.2. founded 533.2.
In the presence of coupling reagent HATU (1.3 eq) in DMF (1.0 mL), compound 29a (60 mg, 0.1 mmol) was reacted with another acid derivative SM-14a to obtain product 30a. After purification by flash column, 39 mg of 30a was obtained.
1 H-NMR for the product 30a (CDCl 3 , 500 MHz): δ 9.98 (s, 1H), 9.39 (m, 1H), 8.77 (m, 1H), 8.56 (m, 1H), 8.19 (d, J=9.0 Hz, 1H), 7.32 (s, 1H), 6.89 (m, 1H), 6.71 (s, 1H), 6.67 (s, 1H), 5.95-5.96 (d, J=5.1 Hz, 2H), 5.72-5.81 (m, 1H), 5.26-5.30 (m, 1H), 5.13-5.16 (m, 1H), 5.40 (s, 1H), 4.63-4.70 (m, 2H), 4.52-4.60 (m, 3H), 4.43-4.48 (m, 2H), 4.20-4.22 (d, J=1.8 Hz, 1H), 3.88-3.91 (m, 1H), 2.81-2.86 (m, 1H), 2.35-2.38 (m, 1H), 2.06-2.13 (m, 1H), 2.04 (s, 1H), 1.95 (m, 2H), 1.87 (m, 1H), 1.61-1.73 (m, 6H), 1.46-1.50 (m, 1H), 1.24-1.31 (m, 4H), 0.99-1.06 (m, 12H). ESI-MS [(M+H) + ]: m/z calculated 891.4. founded 891.5
Example 77
Synthesis of Compound 30b
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30b. After purification, 46 mg of product 30b was obtained.
1 H-NMR for the product 30b (CDCl 3 , 500 MHz): δ 9.99 (s, 1H), 9.39 (m, 1H), 8.76 (m, 1H), 8.55 (m, 1H), 8.19 (d, J=9.0 Hz, 1H), 7.24 (s, 1H), 6.87-6.89 (d, J=8.6 Hz, 1H), 6.72 (s, 1H), 6.67 (s, 1H), 5.95-5.96 (d, J=5.1 Hz, 2H), 5.40 (s, 1H), 4.64-4.70 (m, 2H), 4.53-4.59 (m, 3H), 4.44-4.49 (m, 2H), 4.18-4.20 (d, J=1.8 Hz, 1H), 3.86-3.89 (m, 1H), 2.96 (s, 1H), 2.88 (m, 1H), 2.04 (s, 1H), 1.95 (m, 2H), 1.85 (m, 1H), 1.53-1.73 (m, 9H), 1.17-1.35 (m, 6H), 0.96-1.03 (m, 12H). ESI-MS [(M+H) + ]: m/z calculated 893.4. founded 893.4
Example 78
Synthesis of Compound 30c
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30c. After purification, 41 mg of product 30c was obtained.
1 H-NMR for the product 30e (CDCl 3 , 500 MHz): δ 10.37 (s, 1H), 9.26 (s, 1H), 8.74 (m, 1H), 8.57 (m, 1H), 8.34-8.36 (m, 1H), 7.31-7.32 (m, 1H), 6.76 (m, 1H), 6.79 (m, 1H), 5.92 (m, 1H), 5.39 (s, 1H), 5.30-5.33 (m, 1H), 5.13-5.15 (m, 2H), 4.72-4.74 (m, 1H), 4.61 (m, 2H), 4.49 (m, 2H), 4.40-4.43 (m, 2H), 4.25 (m, 4H), 2.87 (m, 1H), 2.47 (m, 1H), 2.25 (m, 2H), 1.89 (m, 4H), 1.78-1.80 (m, 4H), 1.65-1.67 (m, 1H), 1.44-1.48 (m, 2H), 1.13-1.21 (m, 8H), 1.02 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 905.4. founded 905.4
Example 79
Synthesis of Compound 30d
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30d. After purification, 38 mg of product 30d was obtained.
1 H-NMR for the product 30d (CDCl 3 , 500 MHz): δ10.38 (s, 1H), 9.27 (s, 1H), 8.74 (m, 1H), 8.57 (m, 1H), 8.34-8.36 (m, 1H), 7.30-7.32 (m, 1H), 6.82 (m, 1H), 6.64-6.71 (m, 1H), 5.90 (m, 1H), 5.39 (s, 1H), 5.30-5.32 (m, 1H), 5.13-5.15 (m, 2H), 4.73-4.75 (m, 1H), 4.64 (m, 2H), 4.46-4.52 (m, 2H), 4.37-4.39 (m, 2H), 4.27-4.29 (m, 4H), 2.88 (m, 1H), 2.46 (m, 1H), 2.23 (m, 2H), 1.87-1.90 (m, 6H), 1.78-1.80 (m, 4H), 1.65-1.67 (m, 1H), 1.43-1.49 (m, 2H), 1.14-1.231 (m, 6H), 1.03 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 905.4. founded 905.4.
Example 80
Synthesis of Compound 30e
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30e. After purification, 43 mg of product 30e was obtained.
1 H-NMR for the product 30e (CDCl 3 , 500 MHz): δ10.39 (s, 1H), 9.27 (s, 1H), 8.74 (m, 1H), 8.57 (m, 1H), 8.38 (m, 1H), 7.30-7.32 (m, 1H), 6.78 (m, 1H), 6.69-6.74 (m, 1H), 5.99 (s, 2H), 5.87-5.95 (m, 1H), 5.40 (s, 1H), 5.31-5.34 (m, 1H), 5.12-5.14 (m, 2H), 4.73-4.76 (m, 1H), 4.65-4.66 (m, 2H), 4.47-4.58 (m, 3H), 4.37-4.42 (m, 1H), 2.88 (m, 1H), 2.47 (m, 1H), 2.24 (m, 2H), 1.89 (m, 3H), 1.78-1.80 (m, 4H), 1.65-1.67 (m, 1H), 1.42-1.47 (m, 2H), 1.14-1.23 (m, 6H), 1.03 (s, 9H), 0.84-0.88 (m, 3H), ESI-MS [(M+H) + ]: m/z calculated 891.4. founded 891.4
Example 81
Synthesis of Compound 30f
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30f. After purification, 43 mg of product 30f was obtained.
1 H-NMR for the product 30f (CDCl 3 , 500 MHz): δ9.97-9.99 (m, 1H), 9.40 (s, 1H), 8.76 (m, 1H), 8.55 (m, 1H), 8.19 (m, 1H), 7.32-7.35 (m, 1H), 7.00 (m, 1H), 6.65-6.77 (m, 2H), 5.92-5.97 (m, 2H), 5.41 (s, 1H), 4.47-4.76 (m, 7H), 4.21-4.26 (m, 1H), 3.88-3.90 (m, 1H), 2.84-2.91 (m, 1H), 2.33-2.40 (m, 2H), 2.21 (m, 3H), 1.83 (m, 1H), 1.55-1.65 (m, 9H), 1.12-1.42 (m, 6H), 0.96-1.03 (m, 13H). ESI-MS [(M+H) + ]: m/z calculated 893.4. founded 893.5
Example 82
Synthesis of Compound 30g
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30g. After purification, 26 mg of product 30g was obtained. Confirmed by ESI-MS [(M+H) + ]: m/z calculated 919.4. founded 919.4.
Example 83
Synthesis of Compound 30h
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30h. After purification, 43 mg of product 30h was obtained.
1 H-NMR for the product 30h (CDCl 3 , 500 MHz): δ9.99 (s, 1H), 9.38 (m, 1H), 8.76 (m, 1H), 8.56 (m, 1H), 8.15-8.17 (m, 1H), 7.10 (s, 1H), 6.89 (s, 1H), 6.84 (s, 1H), 6.73-6.75 (m, 2H), 5.40 (s, 1H), 4.62-4.72 (m, 2H), 4.52-4.60 (m, 3H), 4.41-4.46 (m, 2H), 4.16-4.21 (m, 5H), 3.85-3.88 (m, 1H), 2.84-2.91 (m, 1H), 2.36-2.45 (m, 1H), 2.32-2.36 (m, 1H), 2.16-2.21 (m, 2H), 1.87 (m, 1H), 1.72-1.75 (m, 6H), 1.65-1.68 (m, 3H), 1.57-1.59 (m, 2H), 1.49-1.5 (m, 2H), 1.31-1.33 (m, 2H), 1.27 (m, 1H), 1.21-1.23 (m, 2H), 1.08-1.09 (m, 3H), 1.01 (s, 9H), 0.97-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 921.4. founded 921.4.
Example 84
Synthesis of Compound 30j
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30j. After purification, 43 mg of product 30j was obtained.
1 H-NMR for the product 30j (CDCl 3 , 500 MHz): δ 9.98-10.02 (m, 1H), 9.40-9.41 (m, 1H), 8.75 (m, 1H), 8.52-8.55 (m, 1H), 8.18-8.21 (m, 1H), 7.09 (s, 1H), 6.89-6.92 (m, 1H), 6.79-6.81 (d, J=8.0 Hz, 1H), 6.74-6.75 (d, J=8.0 Hz, 1H), 5.42 (s, 1H), 4.67-4.76 (m, 2H), 4.54-4.61 (m, 3H), 4.42-4.49 (m, 2H), 4.24-4.26 (t, J=5.5 Hz, 2H), 4.16-4.20 (m, 3H), 3.87-3.93 (m, 1H), 2.84-2.91 (m, 1H), 2.40-2.46 (m, 1H), 2.30-2.36 (m, 1H), 2.18-2.23 (m, 2H), 1.88 (m, 1H), 1.80 (m, 3H), 1.63-1.71 (m, 5H), 1.57-1.61 (m, 3H), 1.36-1.41 (m, 1H), 1.30 (m, 2H), 1.18-1.26 (m, 2H), 1.08-1.10 (m, 2H), 1.02-1.04 (m, 2H), 0.99 (s, 9H), 0.96-0.98 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 921.4. founded 921.4.
Example 85
Synthesis of Compound 30k
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30k. After purification, 42 mg of product 30k was obtained.
1 H-NMR for the product 30k (CDCl 3 , 500 MHz): δ10.36 (s, 1H), 9.27 (m, 1H), 8.74 (m, 1H), 8.57 (m, 1H), 8.34-8.37 (m, 1H), 7.30 (m, 1H), 7.08 (m, 1H), 6.98 (m, 2H), 5.92 (m, 1H), 5.41 (s, 1H), 5.30-5.33 (m, 1H), 5.13-5.15 (m, 2H), 4.75 (m, 3H), 4.65-4.68 (m, 1H), 4.59 (m, 1H), 4.47-4.51 (m, 1H), 4.38-4.42 (m, 1H), 2.87 (m, 1H), 2.49 (m, 1H), 2.37 (m, 1H), 2.23-2.26 (m, 1H), 1.89 (m, 1H), 1.79 (m, 4H), 1.67 (m, 2H), 1.42-1.45 (m, 2H), 1.26-1.31 (m, 4H), 1.14-1.19 (m, 4H), 1.01-1.06 (m, 12H). ESI-MS [(M+H) + ]: m/z calculated 865.4. founded 865.6
Example 86
Synthesis of Compound 30m
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30m. After purification, 43 mg of product 30m was obtained.
1 H-NMR for the product 30m (CDCl 3 , 500 MHz): δ 10.02 (m, 1H), 7.20 (s, 1H), 6.71 (s, 1H), 6.64 (m, 2H), 5.95-5.97 (m, 2H), 5.38 (s, 1H), 4.82-4.83 (m, 1H), 4.62-4.69 (m, 2H), 4.45-4.51 (m, 4H), 4.17-4.20 (m, 1H), 3.83-3.85 (m, 2H), 2.93 (m, 1H), 2.48 (m, 1H), 2.29 (m, 1H), 1.89 (m, 1H), 1.63-1.72 (m, 5H), 1.53-1.60 (m, 5H), 1.49 (s, 9H), 1.34-1.37 (m, 3H), 1.16-1.21 (m, 2H), 1.04-1.06 (m, 4H), 1.00 (s, 9H), 0.97-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 887.4. founded 887.4.
Example 87
Synthesis of Compound 30n
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30n. After purification, 43 mg of product 30n was obtained.
1 H-NMR for the product 30n (CDCl 3 , 500 MHz): δ 10.10 (s, 1H), 7.39 (s, 1H), 6.94 (m, 1H), 6.68 (s, 1H), 6.61 (m, 1H), 5.96 (s, 2H), 5.42 (s, 1H), 5.25 (br, 1H), 4.52-4.64 (m, 4H), 4.42-4.49 (m, 2H), 4.17-4.19 (m, 1H), 3.88-3.89 (m, 1H), 3.65 (m, 1H), 2.94 (m, 1H), 2.90 (s, 1H), 2.36-2.41 (m, 2H), 1.93 (m, 1H), 1.73 (m, 3H), 1.58-1.64 (m, 6H), 1.35 (m, 2H), 1.19-1.26 (m, 5H), 1.03-1.06 (m, 3H), 1.03 (s, 9H), 0.98-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 865.3. founded 865.4
Example 88
Synthesis of Compound 30p
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30p. After purification, 33 mg of product 30p was obtained.
1 H-NMR for the product 30p (CDCl 3 , 500 MHz): δ 10.24 (s, 1H), 8.65 (m, 1H), 8.08 (m, 1H), 8.01 (m, 1H), 7.9 (m, 1H), 7.67 (m, 1H), 7.58 (m, 1H), 7.48 (m, 1H), 7.40 (m, 1H), 6.68 (m, 1H), 6.62 (s, 1H), 6.44 (s, 1H), 5.86-5.91 (m, 2H), 5.63 (s, 1H), 5.40 (s, 1H), 4.44-4.62 (m, 4H), 4.37-4.40 (m, 2H), 3.99-4.01 (m, 1H), 3.83 (m, 1H), 3.26 (m, 1H), 2.96 (m, 1H), 2.46 (m, 1H), 2.35 (m, 1H), 1.86 (m, 1H), 1.56-1.65 (m, 4H), 1.46-1.48 (m, 4H), 1.39-1.42 (m, 4H), 1.09 (m, 3H), 0.99-1.02 (m, 4H), 0.84 (s, 9H), 0.72 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 977.4. founded 977.4.
Example 89
Synthesis of Compound 30q
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30q. After purification, 39 mg of product 30q was obtained. Confirmed by ESI-MS [(M+H) + ]: m/z calculated 891.4. founded 891.5.
Example 90
Synthesis of Compound 30r
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30r. After purification, 44 mg of product 30r was obtained.
1 H-NMR for the product 30r (CDCl 3 , 500 MHz): δ 10.51 (s, 1H), 7.65-7.67 (d, J=7.4 Hz, 2H), 7.47-7.51 (m, 2H), 7.34-7.37 (t, J=7.8 Hz, 2H), 6.98-6.99 (m, 1H), 6.54 (s, 1H), 6.30 (s, 1H), 5.87 (s, 1H), 5.81 (s, 2H), 5.45 (s, 1H), 4.55-4.63 (m, 3H), 4.46-4.49 (m, 1H), 4.19-4.26 (m, 2H), 4.05-4.07 (m, 1H), 3.85-3.87 (m, 1H), 3.18 (m, 1H), 2.96 (m, 1H), 2.68 (m, 1H), 2.42 (m, 1H), 1.84 (m, 1H), 1.65-1.67 (m, 2H), 1.51-1.55 (m, 9H), 1.25-1.37 (m, 5H), 1.08-1.13 (m, 5H), 0.99 (s, 9H), 0.85 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 927.4. founded 927.4.
Example 91
Synthesis of Compound 30s
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30s. After purification, 37 mg of product 30s was obtained.
1 H-NMR for the product 30s (CDCl 3 , 500 MHz): δ 10.52 (s, 1H), 8.10 (m, 1H), 7.84-7.88 (t, J=9.0 Hz, 2H), 7.76-7.78 (m, 1H), 7.66-7.67 (m, 1H), 7.59-7.62 (m, 1H), 7.51-7.54 (m, 1H), 6.98 (m, 1H), 6.49 (s, 1H), 6.24 (s, 1H), 5.88-5.91 (m, 2H), 5.72 (s, 1H), 5.49 (s, 1H), 5.41 (s, 1H), 4.59-4.66 (m, 3H), 4.49-4.51 (m, 1H), 4.19-4.24 (m, 2H), 4.03-4.05 (m, 1H), 3.85-3.87 (m, 1H), 3.25 (m, 1H), 2.98 (m, 1H), 2.68 (m, 1H), 2.45 (m, 1H), 1.87 (m, 1H), 1.64-1.66 (m, 2H), 1.50-1.59 (m, 8H), 1.30-1.36 (m, 4H), 0.99-1.05 (m, 5H), 0.94 (s, 9H), 0.88 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 977.4. founded 977.4
Example 92
Synthesis of Compound 30t
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30t. After purification, 21 mg of product 30t was obtained.
1 H-NMR for the product 30t (CDCl 3 , 500 MHz): δ 10.05 (m, 1H), 7.32 (s, 1H), 6.71 (m, 1H), 6.63 (m, 1H), 6.59 (m, 1H), 5.96 (m, 2H), 5.39 (s, 1H), 4.91 (m, 1H), 4.43-4.66 (m, 7H), 4.19 (m, 1H), 3.87-3.95 (m, 1H), 3.68-3.77 (m, 1H), 2.93 (m, 1H), 2.49 (m, 1H), 2.33 (m, 1H), 1.96 (s, 1H), 1.81 (m, 1H), 1.71 (m, 3H), 1.57-1.63 (m, 6H), 1.36 (m, 3H), 1.25 (s, 3H), 1.15 (s, 2H), 1.11 (s, 3H), 0.99-1.04 (m, 18H). ESI-MS [(M+H) + ]: m/z calculated 899.4. founded 899.4
Example 93
Synthesis of Compound 30v
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30v. After purification, 45 mg of product 30v was obtained.
1 H-NMR for the product 30v (CDCl 3 , 500 MHz): δ 10.04 (s, 1H), 7.23 (s, 1H), 6.72 (s, 1H), 6.64 (m, 2H), 5.96-5.97 (m, 2H), 5.38 (s, 1H), 4.97-4.98 (m, 1H), 4.59-4.69 (m, 2H), 4.47-4.52 (m, 4H), 4.18-4.20 (m, 1H), 3.94 (m, 1H), 3.84 (m, 1H), 2.94 (m, 1H), 2.47 (m, 1H), 2.33 (m, 1H), 1.87 (m, 1H), 1.66-1.69 (m, 5H), 1.56-1.58 (m, 5H), 1.36 (m, 3H), 1.22-1.27 (m, 3H), 1.17-1.19 (m, 2H), 1.14-1.16 (m, 2H), 1.03-1.08 (m, 4H), 1.00 (s, 9H), 0.97-0.98 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 859.4. founded 859.4
Example 94
Synthesis of Compound 30w
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30w. After purification, 40 mg of product 30w was obtained.
1 H-NMR for the product 30w (CDCl 3 , 500 MHz): δ 10.02 (m, 1H), 7.19 (s, 1H), 6.72 (s, 1H), 6.65 (m, 2H), 5.96-5.97 (m, 2H), 5.38 (s, 1H), 4.89 (m, 2H), 4.60-4.69 (m, 2H), 4.47-4.51 (m, 4H), 4.20-4.22 (m, 1H), 3.83-3.90 (m, 2H), 2.94 (m, 1H), 2.48 (m, 1H), 2.33 (m, 1H), 1.88 (m, 1H), 1.64-1.69 (m, 5H), 1.56-1.58 (m, 5H), 1.36-1.37 (m, 3H), 1.25 (s, 3H), 1.24 (s, 3H), 1.14-1.19 (m, 3H), 0.97-1.05 (m, 12H), 0.82-0.91 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 873.4. founded 873.5
Example 95
Synthesis of Compound 30x
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30x. After purification, 41 mg of product 30x was obtained.
1 H-NMR for the product 30x (CDCl 3 , 500 MHz): δ 10.09 (s, 1H), 7.34 (br, 1H), 6.71 (s, 1H), 6.65 (m, 2H), 5.96-5.97 (m, 2H), 5.38 (s, 1H), 5.05 (m, 1H), 4.59-4.689 (m, 2H), 4.49-4.52 (m, 4H), 4.17-4.19 (m, 1H), 3.96 (m, 1H), 3.88 (m, 1H), 3.68 (s, 3H), 2.92 (m, 1H), 2.43 (m, 1H), 2.34 (m, 1H), 1.88 (m, 1H), 1.64-1.69 (m, 5H), 1.56-1.57 (m, 5H), 1.35 (m, 3H), 1.26 (m, 4H), 1.17-1.20 (m, 2H), 1.01 (s, 9H), 0.88-0.89 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 845.4. founded 845.4
Example 96
Synthesis of Compound 30y
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30y. After purification, 43 mg of product 30y was obtained. Confirmed by ESI-MS [(M+H) + ]: m/z calculated 921.4. founded 921.4
Example 97
Synthesis of Compound 30z
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30z. After purification, 31 mg of product 30z was obtained. Confirmed by ESI-MS [(M+H) + ]: m/z calculated 907.4. founded 907.5.
Example 98
Synthesis of Compound 30aa
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30aa. After purification, 31 mg of product 30aa was obtained.
1 H-NMR for the product 30aa (CDCl 3 , 500 MHz): δ 10.00 (s, 1H), 7.76-7.78 (d, J=7.3 Hz, 2H), 7.58-7.62 (d, J=7.4 Hz, 2H), 7.38-7.42 (m, 2H), 7.30-7.34 (m, 2H), 7.03 (s, 1H), 6.69 (m, 2H), 6.65 (s, 1H), 5.93-5.96 (m, 2H), 5.38 (s, 1H), 5.13-5.15 (m, 1H), 4.59-4.69 (m, 2H), 4.52 (s, 2H), 4.39-4.48 (m, 4H), 4.17-4.20 (m, 1H), 3.95 (m, 1H), 3.83-3.87 (m, 1H), 2.91 (m, 1H), 2.43 (m, 1H), 2.30 (m, 1H), 1.86 (s, 1H), 1.68-1.73 (m, 2H), 1.61-1.64 (m, 3H), 1.53-1.58 (m, 3H), 1.33-1.36 (m, 2H), 1.26-1.30 (m, 2H), 1.15-1.20 (m, 3H), 0.97-1.03 (m, 15H). ESI-MS [(M+H) + ]: m/z calculated 1009.4. founded 1009.4
Example 99
Synthesis of Compound 30ab
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ab. After purification, 46 mg of product 30ab was obtained.
1 H-NMR for the product 30ab (CDCl 3 , 500 MHz): δ 10.49 (brs, 1H), 7.40 (brs, 1H), 6.68 (s, 1H), 6.64 (m, 2H), 5.92-5.95 (m, 2H), 5.81 (brs, 1H), 5.43 (m, 1H), 5.28-5.30 (m, 1H), 5.11-5.19 (m, 1H), 4.87 (m, 1H), 4.55-4.64 (m, 3H), 4.25-4.51 (m, 3H), 4.19 (m, 1H), 3.92-4.04 (m, 2H), 2.83 (m, 1H), 2.28-2.39 (m, 2H), 2.20 (m, 1H), 1.98 (m, 1H), 1.67-1.81 (m, 3H), 1.41-1.62 (m, 5H), 1.30 (s, 9H), 1.12-1.26 (m, 3H), 1.07-1.09 (m, 3H), 1.03 (s, 9H), 0.86-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 884.4. founded 884.5
Example 100
Synthesis of Compound 30ac
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ac. After purification, 42 mg of product 30ac was obtained.
1 H-NMR for the product 30ac (CDCl 3 , 500 MHz): δ 7.35 (brs, 1H), 6.63-6.68 (m, 2H), 5.93-5.95 (m, 2H), 5.39 (m, 1H), 4.89 (m, 1H), 4.33-4.59 (m, 6H), 4.16 (m, 1H), 3.92-4.00 (m, 2H), 2.85 (m, 1H), 2.32-2.39 (m, 3H), 1.67-1.80 (m, 5H), 1.52-1.62 (m, 5H), 1.40-1.48 (m, 3H), 1.30 (s, 9H), 1.13-1.26 (m, 4H), 1.05-1.10 (m, 3H), 1.04 (s, 9H), 0.89-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 886.4. founded 886.5.
Example 101
Synthesis of Compound 30ad
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ad. After purification, 31 mg of product 30ad was obtained.
1 H-NMR for the product 30ad (CDCl 3 , 500 MHz): δ 10.03 (m, 1H), 7.20 (s, 1H), 6.88 (s, 1H), 6.81 (s, 1H), 6.72 (m, 1H), 5.38 (m, 1H), 4.85 (m, 1H), 4.59-4.68 (m, 2H), 4.43-4.51 (m, 4H), 4.18-4.20 (m, 5H), 3.85 (m, 2H), 2.86-2.96 (m, 2H), 2.42 (m, 1H), 2.34 (m, 1H), 2.19 (m, 2H), 1.60-1.70 (m, 5H), 1.51-1.58 (m, 5H), 1.44 (s, 9H), 1.36-1.39 (m, 3H), 1.13-1.21 (m, 2H), 1.04-1.07 (m, 4H), 1.01 (s, 9H), 0.97-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 915.5. founded 915.6.
Example 102
Synthesis of Compound 30ae
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ae. After purification, 31 mg of product 30ae was obtained.
1 H-NMR for the product 30ae (CDCl 3 , 500 MHz): δ 10.03 (m, 1H), 7.19 (s, 1H), 6.88 (s, 1H), 6.80 (s, 1H), 6.64 (m, 1H), 5.38 (m, 1H), 5.07 (m, 1H), 4.89 (m, 1H), 4.60-4.69 (m, 2H), 4.45-4.54 (m, 4H), 4.20 (m, 5H), 3.86 (m, 2H), 2.91-2.96 (m, 1H), 2.44-2.49 (m, 1H), 2.32-2.34 (m, 1H), 2.17-2.21 (m, 2H), 1.81-1.90 (m, 4H), 1.64-1.71 (m, 8H), 1.52-1.57 (m, 7H), 1.33-1.36 (m, 2H), 1.05-1.28 (m, 7H), 1.01 (s, 9H), 0.93-0.99 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 927.5. founded 927.6
Example 103
Synthesis of Compound 30af
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30af. After purification, 31 mg of product 30af was obtained.
1 H-NMR for the product 30af (CDCl 3 , 500 MHz): δ 10.03 (s, 1H), 7.20 (s, 1H), 6.70 (s, 1H), 6.58 (s, 1H), 5.97 (s, 2H), 5.74 (m, 1H), 5.40 (br, 1H), 5.21-5.28 (m, 2H), 5.14-5.16 (m, 1H), 4.66 (m, 2H), 4.44-4.55 (m, 3H), 4.21-4.23 (m, 2H), 3.87 (m, 1H), 2.89 (m, 1H), 2.37 (m, 2H), 2.08 (m, 1H), 1.94 (m, 1H), 1.78 (m, 1H), 1.40-1.48 (m, 2H), 1.34 (s, 9H), 1.07 (m, 2H), 1.02 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 746.3. founded 746.4
Example 104
Synthesis of Compound 30ag
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ag. After purification, 31 mg of product 30ag was obtained.
Confirmed by ESI-MS [(M+H) + ]: m/z calculated 748.3. founded 748.4.
Example 105
Synthesis of Compound 30ah
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ah. After purification, 31 mg of product 30ah was obtained.
1 H-NMR for the product 30ah (CDCl 3 , 500 MHz): δ 10.02 (s, 1H), 7.16-7.18 (m, 1H), 6.76 (m, 1H), 6.62-6.72 (m, 1H), 5.98 (s, 1H), 5.97 (m, 1H), 5.76 (m, 1H), 5.41 (s, 1H), 5.29 (m, 1H), 5.21 (m, 1H), 5.14-5.16 (m, 1H), 4.66-4.69 (m, 2H), 4.53-4.58 (m, 2H), 4.46 (m, 1H), 4.20-4.25 (m, 2H), 3.85 (m, 1H), 2.92 (m, 1H), 2.37-2.43 (m, 2H), 2.08 (m, 1H), 1.96 (m, 1H), 1.71 (m, 1H), 1.44-1.48 (m, 2H), 1.30-1.33 (m, 9H), 1.04-1.05 (m, 2H), 1.02 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 746.3. founded 746.4
Example 106
Synthesis of Compound 30aj
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30aj. After purification, 23 mg of product 30aj was obtained.
Confirmed by ESI-MS [(M+H) + ]: m/z calculated 720.3. founded 720.4.
Example 107
Synthesis of Compound 30ak
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ak. After purification, 39 mg of product 30ak was obtained.
1 H-NMR for the product 30ak (CDCl 3 , 500 MHz): δ 10.01 (s, 1H), 7.21 (s, 1H), 6.71 (s, 1H), 6.68 (s, 1H), 5.96 (m, 2H), 5.76 (m, 1H), 5.40 (s, 1H), 5.26-5.30 (m, 2H), 5.15-5.17 (m, 1H), 4.73 (br, 1H), 4.60-4.69 (m, 2H), 4.47-4.52 (m, 2H), 4.23 (m, 2H), 3.83 (m, 1H), 2.93 (m, 1H), 2.42 (m, 1H), 2.36 (m, 1H), 2.09 (m, 1H), 1.98 (m, 1H), 1.63-1.68 (m, 7H), 1.44-1.47 (m, 4H), 1.36 (m, 3H), 1.02 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 758.3. founded 758.4
Example 108
Synthesis of Compound 30am
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30am. After purification, 40 mg of product 30am was obtained.
Confirmed by ESI-MS [(M+H) + ]: m/z calculated 760.3,
Example 109
Synthesis of Compound 30an
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30an. After purification, 31 mg of product 30an was obtained.
1 H-NMR for the product 30an (CDCl 3 , 500 MHz): δ 9.98 (s, 1H), 7.25 (s, 1H), 6.77 (m, 1H), 6.62-6.75 (m, 1H), 5.95 (m, 2H), 5.75 (m, 1H), 5.40 (s, 1H), 5.25-5.32 (m, 2H), 5.14-5.16 (m, 1H), 4.65-4.75 (m, 3H), 4.47-4.62 (m, 3H), 4.22-4.27 (m, 2H), 3.85 (m, 1H), 2.90 (m, 1H), 2.42 (m, 1H), 2.37 (m, 1H), 2.08 (m, 1H), 1.96 (m, 1H), 1.73 (m, 1H), 1.54-1.62 (m, 6H), 1.44 (m, 3H), 1.34 (m, 2H), 1.01-1.05 (m, 11H). ESI-MS [(M+H) + ]: m/z calculated 758.3. founded 758.4.
Example 110
Synthesis of Compound 30ap
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ap. After purification, 23 mg of product 30ap was obtained.
Confirmed by ESI-MS [(M+H) + ]: m/z calculated 762.3. founded 762.4.
Example 111
Synthesis of Compound 30aq
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30aq. After purification, 39 mg of product 30aq was obtained.
1 H-NMR for the product 30aq (CDCl 3 , 500 MHz): δ 10.08 (s, 1H), 7.18 (brs, 1H), 6.69 (s, 1H), 6.58 (s, 1H), 5.96 (s, 2H), 5.40 (m, 1H), 4.47-4.64 (m, 4H), 4.3-4.44 (m, 2H), 4.29-4.31 (m, 1H), 3.89 (m, 1H), 2.92 (m, 1H), 2.34 (m, 2H), 1.58-1.68 (m, 3H), 1.36-1.43 (m, 2H), 1.28-1.33 (m, 1H), 1.26 (s, 9H), 1.05-1.07 (m, 3H), 1.01 (s, 9H), 0.95-0.98 (t, J=7.5 Hz, 1H). ESI-MS [(M+H) + ]: m/z calculated 747.4. founded 747.5
Example 112
Synthesis of Compound 30ar
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30ar. After purification, 33 mg of product 30ar was obtained.
1 H-NMR for the product 30ar (CDCl 3 , 500 MHz): δ 10.18 (s, 1H), 7.11 (brs, 1H), 6.71 (s, 1H), 6.60 (s, 1H), 5.97 (s, 2H), 5.80-5.88 (m, 1H), 5.25-5.27 (d, J=9.5 Hz, 1H), 5.14-5.16 (d, J=10.5 Hz, 1H), 4.57-4.67 (m, 3H), 4.45-4.50 (m, 1H), 4.36-4.37 (m, 2H), 4.25-4.29 (m, 1H), 3.89 (m, 1H), 2.92 (m, 1H), 2.34-2.41 (m, 2H), 2.08-2.13 (m, 1H), 1.96-1.98 (m, 1H), 1.51-1.54 (m, 1H), 1.30-1.39 (m, 3H), 1.26 (s, 9H), 1.14-1.23 (m, 2H), 1.05 (m, 1H), 1.02 (s, 9H). ESI-MS [(M+H) + ]: m/z calculated 745.4. founded 745.5.
Example 113
Synthesis of Compound 30-Ref
The synthetic procedure was carried out as the same as in Example 76 for preparation of compound 30-Ref. After purification, 37 mg of product 30-Ref was obtained.
1 H-NMR for the product 30-Ref (CDCl 3 , 500 MHz): δ 9.99 (s, 1H), 7.28 (s, 1H), 7.07 (m, 1H), 6.96 (m, 2H), 5.75 (m, 1H), 5.41 (s, 1H), 5.26-5.31 (m, 2H), 5.15-5.17 (m, 1H), 4.63-4.85 (m, 5H), 4.50-4.53 (m, 1H), 4.29-4.32 (m, 1H), 4.22-4.24 (m, 1H), 3.83 (m, 1H), 2.91 (m, 1H), 2.42 (m, 1H), 2.38 (m, 1H), 2.09 (m, 1H), 1.94 (m, 1H), 1.60 (m, 4H), 1.51 (m, 3H), 1.44 (m, 3H), 1.35 (m, 2H), 1.01-1.05 (m, 11H). ESI-MS [(M+H) + ]: m/z calculated 732.3. founded 732.4.
Example 114
Synthesis of Compound 33a
Chemical SM-15a (5.4 g, 10 mmol), SM-16 (1.1 eq) and DMF (80 mL) were added into 250 mL flask reactor, followed by adding coupling reagent EDCI (1.3 eq) to keep the amidation at 55° C. until completed. The reaction mixture was worked out to obtain crude product 31a, followed by removing Boc group with HCl-THF solution to obtain 32a (3.9 g, yield: 86%), which was purified by precipitation in hexane-EtOAc and dried directly for next step. ESI-MS (M+H + ): m/z calculated 487.2. founded 487.2.
In the presence of coupling reagent HATU (1.3 eq) in DMF (1.0 mL), compound 32a (60 mg, 0.1 mmol) was reacted with another acid derivative SM-14a to obtain product 33a. After purification by flash column, 41 mg of 33a was obtained.
1 H-NMR for the product 33a (CDCl 3 , 500 MHz): δ 9.40 (s, 1H), 8.77 (s, 1H), 8.55 (s, 1H), 8.16-8.17 (m, 1H), 7.32-7.33 (m, 1H), 7.04 (m, 1H), 6.72 (s, 1H), 6.68 (s, 1H), 5.94-5.95 (m, 2H), 5.36 (m, 1H), 4.77-4.80 (m, 1H), 4.69-4.72 (m, 1H), 4.59-4.64 (m, 2H), 4.51-4.53 (m, 2H), 4.44-4.47 (m, 2H), 4.18-4.20 (m, 1H), 3.80-3.83 (m, 1H), 2.78 (m, 1H), 2.64 (m, 1H), 2.26 (m, 1H), 1.88-1.92 (m, 1H), 1.77-1.79 (m, 1H), 1.66-1.69 (m, 3H), 1.59-1.61 (m, 4H), 1.38-1.42 (m, 2H), 1.10-1.19 (m, 3H), 1.00-1.07 (m, 3H), 0.97-0.99 (m, 9H), 0.89-0.93 (m, 3H), 0.85-0.86 (m, 2H), 0.61 (m, 2H), ESI-MS [(M+H) + ]: m/z calculated 845.4. founded 845.4
Example 115
Synthesis of Compound 33b
The synthetic procedure was carried out as the same as in Example 114 for preparation of compound 33b. After purification, 41 mg of product 33b was obtained.
1 H-NMR for the product 33b (CDCl 3 , 500 MHz): δ 9.39 (m, 1H), 8.77 (m, 1H), 8.57 (m, 1H), 8.33 (m, 1H), 7.75 (m, 1H), 6.76 (s, 2H), 6.69 (s, 1H), 6.62 (m, 1H), 6.06 (br, 1H), 5.70 (br, 1H), 4.86 (m, 1H), 4.54-4.66 (m, 3H), 4.44-4.51 (m, 2H), 4.25-4.41 (m, 1H), 4.25 (m, 4H), 4.09 (m, 1H), 2.82 (m, 1H), 2.58 (m, 1H), 2.22 (m, 1H), 1.97 (m, 2H), 2.19 (m, 2H), 1.78 (m, 4H), 1.68 (m, 2H), 1.25-1.29 (m, 6H), 1.05-1.16 (m, 4H), 1.05 (s, 9H), 0.84-0.85 (m, 2H), 0.76-0.79 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 859.4. founded 859.5
Example 116
Synthesis of Compound 33c
The synthetic procedure was carried out as the same as in Example 114 for preparation of compound 33c. After purification, 21 mg of product 33c was obtained.
1 H-NMR for the product 33c (CDCl 3 , 500 MHz): δ 9.28 (s, 1H), 8.75 (s, 1H), 8.56 (m, 2H), 7.72 (m, 1H), 6.76-6.78 (m, 1H), 6.65-6.67 (m, 1H), 6.68 (s, 1H), 5.99 (m, 2H), 5.32 (s, 1H), 4.86 (m, 1H), 4.44-4.67 (m, 6H), 4.09 (m, 2H), 2.82 (m, 1H), 2.61 (m, 1H), 2.24 (m, 1H), 2.03 (m, 2H), 1.84-1.87 (m, 2H), 1.65-1.78 (m, 5H), 1.21-1.34 (m, 5H), 1.09-1.25 (m, 4H), 1.05-1.09 (m, 9H), 0.84-0.85 (m, 2H), 0.76 (m, 4H). ESI-MS [(M+H) + ]: m/z calculated 845.4. founded 845.4.
Example 117
Synthesis of Compound 33d
The synthetic procedure was carried out as the same as in Example 114 for preparation of compound 33d. After purification, 22 mg of product 33d was obtained.
1 H-NMR for the product 33d (CDCl 3 , 500 MHz): δ 9.28 (m, 1H), 8.76 (m, 1H), 8.56 (m, 2H), 7.77 (m, 1H), 6.80 (m, 1H), 6.76 (m, 1H), 6.65 (m, 1H), 6.60 (br, 1H), 4.47-4.69 (m, 6H), 4.26 (m, 4H), 4.09 (m, 1H), 2.83 (m, 1H), 2.59 (m, 1H), 2.22 (m, 1H), 1.85-1.87 (m, 2H), 1.62-1.72 (m, 8H), 1.26 (m, 6H), 1.05-1.19 (m, 4H), 1.01-1.05 (m, 9H), 0.85-0.86 (m, 2H), 0.76-0.79 (m, 3H). ESI-MS [(M+H) + ]: m/z calculated 859.4. founded 859.5.
Example 118
Synthesis of Compound 33-Ref
The synthetic procedure was carried out as the same as in Example 114 for preparation of compound 33-Ref. After purification, 28 mg of product 33-Ref was obtained.
1 H-NMR for the product 33-Ref (CDCl 3 , 500 MHz): δ 9.28 (m, 1H), 8.75 (s, 1H), 8.57 (m, 2H), 7.71 (m, 1H), 7.07 (m, 1H), 6.97-7.00 (m, 2H), 6.63 (m, 1H), 5.92 (m, 1H), 5.41 (s, 1H), 5.30-5.33 (m, 1H), 5.13-5.15 (m, 2H), 4.75 (m, 3H), 4.65-4.68 (m, 1H), 4.59 (m, 1H), 4.47-4.51 (m, 1H), 4.38-4.42 (m, 1H), 2.87 (m, 1H), 2.49 (m, 1H), 2.37 (m, 1H), 2.23-2.26 (m, 1H), 2.03 (m, 2H), 1.84-1.87 (m, 2H), 1.65-1.78 (m, 5H), 1.21-1.34 (m, 5H), 1.09-1.25 (m, 4H), 1.05-1.09 (m, 9H), 0.84-0.85 (m, 2H), 0.76 (m, 4H), ESI-MS [(M+H) + ]: m/z calculated 819.4. founded 819.4
This application claims priority to Chinese application No. CN 201010101403.7, filed on Jan. 27, 2010, and incorporated herein by reference.
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The present invention discloses the structure, preparation methods and uses of a series of novel polyheterocyclic based compounds (Ia-Ib and IIa-IIb) that are highly effective for inhibiting hepatitis C virus (HCV):
where the structural variables are defined herein. The present invention is also provides a method of treating HCV infection by the polyheterocyclic based HCV inhibitory compounds, compositions and therapeutic methods.
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BACKGROUND INFORMATION
[0001] A fuel injector having a valve housing in which a piezoelectric armature and an hydraulic coupler are arranged has already been proposed in German Patent Application No. 103 60 449, the piezoelectric actuator having a positive pole and an earth pole, an electrical plug with a positive terminal and a ground terminal being provided on the valve housing for the contacting with a voltage source. Via a cable in each case, the positive pole of the piezoelectric actuator is connected to the positive terminal of the plug, and the earth pole of the piezoelectric actuator is connected to the ground terminal of the plug. Since the hydraulic coupler between the valve housing and the actuator is arranged in a section of the fuel injector that faces the plug, the cables originating from the plug must be guided around the coupler to reach the actuator. Due to the fact that the hydraulic coupler executes thermally caused compensating movements, the cables cannot be taut, but must be non-tensioned by providing additional length. The cables are not allowed to be in contact with adjacent components, since the many compensating movements may otherwise cause them to fray over time. It is disadvantageous that the compensating movements put heavy mechanical stress on the cables, so that a cable fracture as a result of material fatigue will occur after a predefined service life of the fuel injector, or the solder or welding points of the cables will tear. This leads to malfunctioning of the fuel injector.
SUMMARY OF THE INVENTION
[0002] The fuel injector according to the present invention has the advantage that an improvement is achieved in a simple manner to the effect that the service life of the fuel injector is increased in that the earth pole of the actuator is electrically connected to the ground terminal of the plug, and the positive pole of the actuator is connected to the positive terminal in a cable-less manner. This prevents malfunctioning of the fuel injector due to a cable fracture. Since two cables are omitted, space is saved, so that the fuel injector is able to have a smaller design.
[0003] It is particularly advantageous if the earth pole of the actuator is electrically connected to the ground terminal of the plug via the valve housing and/or an actuator housing, since this utilizes an already existing electrically conductive connection in the fuel injector. Furthermore, the ground contacting of the actuator reduces electromagnetic interference radiation of the actuator.
[0004] In addition, it is advantageous if the positive pole of the actuator is electrically connected to the positive terminal by way of the hydraulic coupler, since in this way the current supply to the actuator is implemented via an existing electrically conductive connection.
[0005] According to an advantageous further development, the actuator is prestressed for compression in an actuator sleeve between an actuator top and an actuator base, and the earth pole of the actuator is electrically contacted to the actuator top, the actuator top being electrically connected to the actuator base via the actuator sleeve. The actuator base is electrically connected to the valve housing and/or the actuator housing via a valve needle, a shoulder of the valve needle and a restoring spring cooperating with the valve needle.
[0006] Furthermore, it is advantageous if the positive terminal of the plug is electrically connected to a head part of the hydraulic coupler, and the positive pole of the actuator is electrically connected to a foot part of the hydraulic coupler, the head part and the foot part of the hydraulic coupler in turn being interconnected in an electrically conducting manner via an elastic sealing element. This allows the current to be supplied by way of the hydraulic coupler.
[0007] It is advantageous if a first electrical insulation is provided between the hydraulic coupler and the actuator, and a second electrical insulation is provided between the hydraulic coupler and the valve housing since this prevents a short circuit.
BRIEF DESCRIPTION OF THE DRAWING
[0008] The FIGURE shows an exemplary embodiment of a fuel injector according to the present invention in a schematic representation.
DETAILED DESCRIPTION
[0009] The fuel injector is used in the so-called direct injection, for instance, and injects fuel such as gasoline or diesel into a combustion chamber of an internal combustion engine.
[0010] The fuel injector has a valve housing 1 with an input port 2 for the fuel. The valve housing includes a housing component 1 . 1 in the shape of a cup, for instance, and a housing lid 1 . 2 sealing cup-shaped housing component 1 . 1 . Input port 2 is provided in housing lid 1 . 2 , for example.
[0011] A schematically illustrated actuator 3 such as a piezoelectric or magneto-restrictive actuator is arranged in valve housing 1 for the axial adjustment of a valve needle 4 .
[0012] Valve needle 4 is provided in valve housing 1 so as to be axially displaceable, and has, for instance, a needle shaft 7 facing actuator 3 , and a valve-closure member 8 facing away from actuator 3 . Actuator 3 transmits its movement to needle shaft 7 of valve needle 4 , which causes valve-closure member 8 cooperating with a valve seat 9 to open or close the fuel injector. The fuel injector is a so-called outwardly opening valve, for instance, valve needle 4 executing a lift in the direction of a combustion chamber 10 . When the fuel injector is closed, the entire circumference of valve-closure member 8 rests sealingly against valve seat 9 with line and surface contact, forming a sealing seat 11 .
[0013] Piezoelectric actuator 3 is made up of a multitude of piezo-ceramic layers, which expand in the axial direction when an electrical voltage is applied. In the process, the so-called inverse piezoelectric effect is utilized in which electrical energy is converted into mechanical energy. The expansion of the piezo-ceramic layers caused by the application of the electrical voltage is transmitted to valve needle 4 , valve needle 4 executing a lift of 40 to 50 micrometer, for instance. After the valve has been opened, actuator 3 shortens in response to the electrical voltage being switched off, and restoring spring 14 moves valve needle 4 back again in the direction of valve seat 9 , closing the fuel injector.
[0014] To protect piezoelectric actuator 3 from tensile and bending stresses, it is arranged in an actuator sleeve 12 between an actuator top (head) 16 and an actuator base 17 , actuator sleeve 12 being designed as so-called tube spring and made from a metal such as steel.
[0015] Actuator top 16 is arranged on a front-side end of actuator sleeve 12 facing away from valve needle 4 and integrally and/or frictionally connected to actuator sleeve 12 , for instance by welding. Actuator base 17 is disposed at a front-side end, facing valve needle 4 , of actuator sleeve 12 and likewise integrally and/or frictionally connected to actuator sleeve 12 , for instance by welding.
[0016] Actuator sleeve 12 prestresses actuator 3 for compression between actuator top 16 and actuator base 17 .
[0017] Needle shaft 7 of valve needle 4 has a shoulder 18 against which restoring spring 14 rests by one end so as to press needle shaft 7 of valve needle 4 against actuator base 17 of actuator sleeve 12 and to press valve-closure member 8 in the direction of valve seat 9 .
[0018] Since actuator 3 and the other components of the fuel injector such as valve housing 1 expand to different degrees in response to temperature changes because of different thermal expansion coefficients, an hydraulic coupler 15 is provided, which compensates for the differences in the various linear expansions in order to ensure that the fuel injector with valve needle 4 will always implement the same lift regardless of the individual temperature of the fuel injector. No lift losses at which the lift of actuator 3 is not fully transmitted to valve needle 4 must occur, so that the lift of valve needle 4 is smaller than the lift of actuator 3 .
[0019] Hydraulic coupler 15 is arranged between housing lid 1 . 2 and actuator top 16 of actuator sleeve 12 , for instance.
[0020] Hydraulic coupler 15 includes a cup-shaped cylinder 21 , for example, and a piston 22 which is axially displaceable in cup-shaped cylinder 21 . A so-called coupler gap 23 is present between cup-shaped cylinder 21 and piston 22 . Starting from cup-shaped cylinder 21 , an elastic sealing element 24 , which is configured as convoluted bellows and made of metal, extends up to piston 22 . Elastic sealing element 24 encloses a coupler volume 25 , which is connected to coupler gap 23 via the fluid by way of a throttle element 28 . Coupler volume 25 and coupler gap 23 are filled with a fluid such as fuel or a second medium such as silicon oil, for instance. The pressure in the fluid of coupler volume 25 is increased with the aid of a spring element 26 , for example, in that spring element 26 exerts a pressure force on elastic sealing element 24 from the outside, or is provided within elastic sealing element 24 , for instance in piston 22 , and exerts a pressure force on the fluid of coupler volume 25 . For instance, piston 22 has a cavity which is connected to coupler gap 23 via throttle element 28 , and which is connected to the circumference of piston 22 via a flow opening.
[0021] In displacement processes acting rapidly on hydraulic coupler 15 , for instance the expansion of actuator 3 in response to an electrical voltage supply, hydraulic coupler 15 reacts as extremely rigid component since barely any fluid is able to flow out of coupler gap 23 through throttle element 28 into coupler volume 25 within the short period of time. Since coupler gap 23 thus remains constant in this situation, the lift of actuator 3 is transmitted to valve needle 4 in its entirety.
[0022] In displacement processes that act slowly on hydraulic coupler 15 , such as the expansion in response to temperature changes, coupler gap 23 becomes smaller or larger since the fluid has enough time to flow out of or into coupler gap 23 via throttle element 28 .
[0023] Cylinder 21 of hydraulic coupler 15 faces actuator 3 , for instance, and piston 22 of hydraulic coupler 15 faces housing lid 1 . 1 , or vice versa. The part of hydraulic coupler 15 facing housing lid 1 . 1 forms a head part 29 , and the part facing actuator 3 forms a foot part 30 of hydraulic coupler 15 .
[0024] Hydraulic coupler 15 , actuator 3 with actuator sleeve 12 , and valve needle 4 are arranged concentrically with respect to a valve axis 27 , for instance.
[0025] Actuator sleeve 12 and hydraulic coupler 15 are, for instance, centered and fixed relative to one another, for example with the aid of an extrusion coat 36 , which begins at actuator top 16 and extends to foot part 30 of hydraulic coupler 15 .
[0026] To encapsulate actuator 3 and hydraulic coupler 15 with respect to fuel, an actuator housing 31 which hermetically surrounds actuator 3 and hydraulic coupler 15 and seals them from the fuel, is provided in valve housing 1 . Actuator housing 31 has a cylindrical design, for example, and divides the interior space of valve housing 1 into a pressure chamber 32 loaded with fuel and connected to input port 2 via the fluid, and an actuator chamber having actuator 3 and hydraulic coupler 15 . Actuator housing 31 is arranged in valve housing 1 in a concentric manner, for example, and rests against valve housing 1 at the front-side ends. For example, on the front side facing housing lid 1 . 2 , actuator housing 31 is connected to housing lid 1 . 2 in an integral and/or non-positive manner, for instance by soldering. Starting from actuator base 17 , needle shaft 7 of valve needle 4 extends in actuator chamber 33 in the direction facing away from actuator 3 and projects through actuator housing 31 into pressure chamber 32 through an opening 34 ; opening 34 is sealed by an elastic seal 35 , so that no fuel is able to travel from pressure chamber 32 into actuator chamber 33 . Seal 35 is designed as elastic convoluted bellows, for instance, which is made of metal, for example, and extends in an annular manner from needle shaft 7 to actuator housing 31 .
[0027] Restoring spring 14 rests against shoulder 18 of valve needle 4 via its one end, and against actuator housing 31 by its other end.
[0028] Actuator 3 has a positive pole 38 and an earth pole 39 , which is the electrical negative pole. Provided on valve housing 1 , for instance on housing lid 1 . 2 , is a two-pole electrical plug 40 , for example, which has a positive terminal 41 and a ground terminal 42 for the contacting with an external voltage source 43 . Depending on the setting of a high-power switch 44 , either a high voltage of voltage source 43 or no voltage is applied at plug 40 . High-power switch 44 is connected to a positive pole of voltage source 43 . Voltage source 43 is a transformer, for example, which, for instance, raises a 12V on-board voltage of a vehicle to a high voltage.
[0029] According to the present invention, earth pole ( 39 ) of actuator ( 3 ) is electrically connected to ground terminal ( 42 ) of plug ( 40 ) in a cable-less manner, and positive pole ( 38 ) of actuator ( 3 ) is electrically connected to positive terminal ( 41 ) of plug 40 in a cable-less manner. Because of the cable-free connection, cable breaks, which would lead to malfunctioning of the fuel injector, are prevented.
[0030] According to an advantageous embodiment, earth pole 39 of actuator 3 is electrically connected to ground terminal 42 of plug 40 via actuator housing 31 and/or valve housing 1 . This reduces the electromagnetic interference radiation of actuator 3 .
[0031] Positive pole 38 of actuator 3 is electrically contacted by positive terminal 41 via hydraulic coupler 15 , for instance. According to this circuit arrangement, the current is fed from plug 40 to actuator 3 via hydraulic coupler 15 .
[0032] For example, earth pole 39 of actuator 3 is in electrical contact with actuator top 16 , actuator top 16 being connected to actuator base 17 by way of actuator sleeve 12 . Actuator base 17 in turn is electrically connected to actuator housing 31 via needle shaft 7 of valve needle 4 , shoulder 18 of valve needle 4 and restoring spring 14 resting against shoulder 18 .
[0033] Positive terminal 41 of plug 40 is electrically connected to head part 29 of hydraulic coupler 15 , for instance, and positive pole 38 of actuator 3 to a foot part 30 of hydraulic coupler 15 .
[0034] Head part 29 and foot part 30 of hydraulic coupler 15 are connected to one another in an electrically conducting manner by way of elastic sealing element 24 .
[0035] Provided between hydraulic coupler 15 and actuator 3 is a first electrical insulation 46 , and provided between hydraulic coupler 15 and valve housing 1 is a second electrical insulation 47 so as to prevent a short circuit between positive pole 38 and earth pole 39 of actuator 3 or between positive terminal 41 and ground terminal 42 of plug 40 . Insulations 46 , 47 are in the shape of disks, for example, and made of ceramic or some other electrically insulating material.
[0036] Positive pole 38 of actuator 3 extends, for instance, through a through hole 50 in actuator top 16 and projects through first electrical insulation 46 through a first opening 48 so as to provide contacting with foot part 30 of hydraulic coupler 15 . Positive terminal 41 of plug 40 runs through a connecting duct 51 in housing lid 1 . 2 and projects through second electrical insulation 47 , for instance through a second opening 49 , so as to provide contacting with head part 29 of hydraulic coupler 15 .
[0037] Second insulation 47 may also be embodied as piezo-ceramic for analyzing the power profile of actuator 3 and utilizing it to regulate the injection.
[0038] In valve housing 1 , the fuel is guided from input port 2 into pressure chamber 32 to valve-closure member 8 upstream from sealing seat 11 . When the fuel injector is opened, valve-closure member 8 lifts off from sealing seat 11 , thereby opening a connection to combustion chamber 10 of the internal combustion engine, so that fuel is flowing into combustion chamber 10 by way of an annular discharge gap 52 formed between valve-closure member 8 and valve seat 9 . The greater the lift of valve needle 4 in the opening direction, the larger discharge gap 52 becomes and the more fuel will be injected into combustion chamber 10 per time unit.
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Known fuel injectors have a valve housing in which an actuator and an hydraulic coupler are arranged, an electrical plug being provided on the valve housing for contact with a voltage source. The cables running from the plug to the actuator must be guided around the coupler to the actuator. It is disadvantageous that the compensating movements put heavy mechanical stress on the cables, so that a cable fracture as a result of material fatigue occurs after a predefined service life of the fuel injector, or that the solder or welding points of the cables tear. This leads to malfunctioning of the fuel injector. In the present fuel injector, the service life is increased by the provision of connections without cables. The earth pole of the actuator is electrically connected to the ground terminal of the plug in a cable-less manner, and the positive pole of the actuator is electrically connected to the positive terminal in a cable-less manner.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application is related to U.S. patent application Ser. No. ______ [Attorney Docket No. AT9-99-356], entitled “System and Method for Maintaining Device Name Consistency During Parallel Device Discovery Processes,” which is hereby incorporated by reference herein.
TECHNICAL FIELD
[0002] The present invention relates in general to displaying the status of an activity within a data processing system.
BACKGROUND INFORMATION
[0003] To enable problem determination and to provide indications of progress, many data processing systems display a status code or word that indicates what activity is currently taking place. As tasks are completed, the status code or word is changed to reflect the next activity that takes place. If a particular activity fails to complete, the user becomes aware because the status codes stop changing. Moreover, by observing the status code, the user can determine which activity failed to complete, and thus can focus problem diagnosis activities on the proper system component.
[0004] However, if there is only a single location for displaying a single status code or word, then there is a problem in determining what should be displayed when these activities are occurring in parallel. The prior method for changing the display each time a new activity is started does continue to provide information on the progress of activities. However, it is inadequate for problem determination, because if any activity fails to complete, the code or word displayed is for the activity that was the last to be started, rather than for the activity that has actually failed to complete. This leads to improper diagnosis of problems, laying blame on the wrong activity, and lengthening problem determination time.
[0005] More specifically, such a status code display is used on RS6000 systems implementing the AIX operating system, available from International Business Machines Corp. When the configuration manager is operating, the device being configured is displayed in the status display. A problem occurs when the AIX operating system is configuring several attached devices in parallel, because it is often not possible to determine which device is having problems being configured. This problem is magnified when there are several hundred devices that need to be configured, and are done so in parallel.
[0006] Therefore, there is a need in the art to provide a status display that provides information on the progress of parallel activities, but also ensures that if any parallel activity fails to complete, its code or word will eventually be displayed.
SUMMARY OF THE INVENTION
[0007] The present invention addresses the foregoing need by ensuring that the code or word displayed still provides information on the progress of parallel activities, but also ensures that if any parallel activity fails to complete, its code or word will eventually be displayed, thus ensuring that problem determination activities begin with the proper component.
[0008] The present invention implements the foregoing using an ordered list with three methods of access: insertion at the top, removal from anywhere, and read (not removal) of the top item. The items kept on this list are the status codes or words for the activities that are currently in progress. When a new activity begins, its status code or word is inserted at the top of the list. Whenever an activity completes, its code or word is removed from the list regardless of its location in the list, and in such a way as to preserve the order of the remaining entries in the list. Whenever the top entry in the list changes (whether through an insertion or removal), the single status display is updated to show the new top value.
[0009] The effect of this is that every newly-started activity will have its status code or word displayed for at least a short time, which gives the observer a sense of the progress of the activities. The code displayed will always be for the latest-started activity that has not yet completed. If any activity is never going to complete, eventually all the other activities will complete, and their status codes or words will be removed from the list. This leaves only the “hung” activity's code on the list, and since it is the only entry, it will be the one displayed. Thus, the observer will know which activity failed to complete.
[0010] The foregoing has outlined rather broadly the features and technical advantages of the present invention in order that the detailed description of the invention that follows may be better understood. Additional features and advantages of the invention will be described hereinafter which form the subject of the claims of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] For a more complete understanding of the present invention, and the advantages thereof, reference is now made to the following descriptions taken in conjunction with the accompanying drawings, in which:
[0012] [0012]FIG. 1 illustrates an exemplary diagram of devices connected within a data processing system;
[0013] [0013]FIG. 2 illustrates a data processing system configurable in accordance with the present invention;
[0014] [0014]FIG. 3 illustrates a method for implementing an embodiment of the present invention; and
[0015] [0015]FIG. 4 illustrates the status display of the present invention.
DETAILED DESCRIPTION
[0016] In the following description, numerous specific details are set forth such as specific word or byte lengths, etc. to provide a thorough understanding of the present invention. However, it will be obvious to those skilled in the art that the present invention may be practiced without such specific details. In other instances, well-known circuits have been shown in block diagram form in order not to obscure the present invention in unnecessary detail. For the most part, details concerning timing considerations and the like have been omitted inasmuch as such details are not necessary to obtain a complete understanding of the present invention and are within the skills of persons of ordinary skill in the relevant art.
[0017] Refer now to the drawings wherein depicted elements are not necessarily shown to scale and wherein like or similar elements are designated by the same reference numeral through the several views.
[0018] The following example is described with respect to the AIX operating system version 4.3, which is published at http:\\www.rs6000.ibm.com\doc_link\en_us\a_doc_lib\aixgen\topnav\topnav.htm, which is hereby incorporated by reference herein. However, the present invention is not limited in its applicability to the AIX operating system.
[0019] The present invention will be described below with respect to the configuration manager component of an AIX operating system. However, the concepts of the present invention may be expanded to other areas outside of this particular embodiment. The configuration manager is a rule-driven program that automatically configures devices in a data processing system during system boot and run time. When the configuration manager is invoked, it reads rules from the configuration rules object class and performs the indicated actions.
[0020] Devices are organized into a set of hierarchical tree structures. Individual entries in a tree are known as nodes and each represents a physical or logical device. Each tree represents a logical subsystem. For example, the tree containing the system node consists of all the physical devices in the system. Thus, the top node in the tree is the system node, which represents the system device, and has nodes connected below that represent individual pieces of the system. Below the system node is the system planar node, which represents the system planar in the system. Below the system planar node is one or more bus nodes, which represent the I/O buses in the system. Since adapter devices are connected to bus devices, adapter nodes fall below the bus nodes in the tree. The bottom of the hierarchy contains devices to which no other devices are connected. FIG. 1 illustrates an example of a connectivity and dependence diagram providing an example of the connections and dependencies of devices in a system.
[0021] Each rule in the configuration rules object class specifies a program name that the configuration manager must execute. These programs are typically the configuration programs for the devices at the top of the nodes. When these programs are invoked, the names of the next lower-level devices that need to be configured are returned. The configuration manager configures the next lower-level devices by invoking the configuration methods for those devices. In turn, those configuration methods return a list of to-be-configured device names. The process is repeated until no more device names are returned.
[0022] Referring next to FIG. 2, there is illustrated data processing system 213 , which may be configured to operate in accordance with the present invention. System 213 shows only a few of the devices that may be attached to the system, such as illustrated in FIG. 1. System 213 in accordance with the subject invention includes one or more central processing units (CPU) 210 , such as a conventional microprocessor, and a number of other units interconnected via a system bus 212 . System 213 includes a random access memory (RAM) 214 , a read only memory (ROM) 216 , and an input/output (I/O) adapter 218 for connecting peripheral devices such as disk units 220 and tape drives 240 to a bus 212 , a user interface adapter 222 for connecting a keyboard 224 , a mouse 226 , and/or other user interface devices such as a touch screen device (not shown) to the bus 212 , a communication adapter 234 for connecting system 213 to a data processing network, and a display adapter 236 for connecting the bus 212 to a display device 238 . CPU 210 may include other circuitry not shown herein, which will include circuitry commonly found within a microprocessor, e.g., execution unit, bus interface unit, arithmetic logic unit, etc. CPU 210 may also reside on a single integrated circuit.
[0023] [0023]FIG. 4 illustrates that on the chassis of system 213 , a status display 401 , which may be an LCD or LED display, is used to display the status of an activity operating within the system 213 .
[0024] The status display is used to show the status of the AIX boot processes, including the configuration manager. As the configuration manager discovers devices that are attached to the system, it invokes configuration methods (the “activities” described above) to configure each device. Currently, AIX displays a unique three-digit code for each method when it begins. When a method completes, AIX invokes the next such method, displaying a new code.
[0025] As noted previously, when the configuration method is run, the display identifies the type of device that is presently being configured. If there is any faulty hardware, such faulty hardware could cause the boot process to stop prematurely (i.e. “hang”). The display gives a clue as to where the problem resides. Since the present version of the AIX now runs the configuration methods in parallel, without the present invention, the display of the “hung” method might not occur.
[0026] Preferred implementations of the invention include implementations as a computer system programmed to execute the method or methods described herein, and as a computer program product. According to the computer system implementation, sets of instructions for executing the method or methods are resident in the random access memory 214 or ROM 216 of one or more computer systems configured generally as described above. Until required by the computer system 213 , the set of instructions may be stored as a computer program product in another computer memory, for example, in disk drive 220 (which may include a removable memory such as an optical disk or floppy disk for eventual use in the disk drive 220 ). Further, the computer program product can also be stored at another computer and transmitted when desired to the user's work station by a network or by an external network such as the Internet. One skilled in the art would appreciate that the physical storage of the sets of instructions physically changes the medium upon which it is stored so that the medium carries computer readable information. The change may be electrical, magnetic, chemical, biological, or some other physical change. While it is convenient to describe the invention in terms of instructions, symbols, characters, or the like, the reader should remember that all of these and similar terms should be associated with the appropriate physical elements.
[0027] Note that the invention may describe terms such as comparing, validating, selecting, identifying, or other terms that could be associated with a human operator. However, for at least a number of the operations described herein which form part of at least one of the embodiments, no action by a human operator is desirable. The operations described are, in large part, machine operations processing electrical signals to generate other electrical signals.
[0028] The software implementing the present invention is represented by the flow diagram illustrated in FIG. 3. In step 301 , the configuration method is begun. In step 302 , a determination is made whether a new activity has started, such as the configuration of a new device. If yes, the process proceeds to step 303 to display the identity of the new activity, and the process loops back to step 302 . The NO branch from step 302 proceeds to step 304 to determine if any activity has completed. If not, the process loops back to step 302 . However, if in step 304 , an activity has completed, then in step 305 , that activity is removed from the list of activities to be displayed on the status display 401 . Therefore, in step 306 , a determination is made whether the removed activity is currently being displayed. If not, the process loops back to step 302 . However, if in step 306 the removed activity is being displayed, the process proceeds to step 307 to display the activity previously displayed. The process then returns to step 304 .
[0029] An example of the foregoing is illustrated in the following table:
Display Contents with Display Contents Action List Contents this invention without this Invention Start Activity A aaa aaa aaa Start Activity B bbb, aaa bbb bbb Start Activity C ccc, bbb, aaa ccc ccc Activity B completes ccc, aaa ccc ccc Activity C ccc, aaa ccc ccc encounters an error and hangs Start Activity D ddd, ccc, aaa ddd ddd Start Activity E eee, ddd, ccc, aaa eee eee Start Activity F fff, eee, ddd, ccc, aaa fff fff Activity F completes eee, ddd, ccc, aaa eee fff Activity E completes ddd, ccc, aaa ddd fff Activity A completes ddd, ccc ddd fff Activity D completes ccc ccc fff
[0030] There are six activities, A-F, with status codes aaa through fff, respectively. The table shows the contents of the list and the display at each point in the evolution of a problem with Activity C that causes it to fail to complete. In the last column, the table shows what would be displayed if the process simply wrote out a new status code or word each time a new activity began. Notice that without the present invention, the observer loses any sense of progress once the last activity has begun (the display shows only “fff”), and there is no way for the user to know that Activity C has not completed. With the present invention, however, the display is much more useful. Longer-running activities (such as Activity D) will have their status codes or words eventually reappear on the display. Furthermore, it is seen that Activity C, which has become “hung,” eventually has its status code reappear on the display 401 , allowing the observer to determine which activity to investigate for problems after noting a lengthy period with no change in the contents of display 401 .
[0031] Although the present invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
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When activities are operated in parallel, and there is only one status display, an ordered list is implemented with three methods of access: insertion at the top, removal from anywhere, and read of the top item. Items kept on this list are the status codes or words for the activities that are currently in progress. When a new activity begins, its status code or word is inserted at the top of the list. Whenever an activity completes, its code or word is removed from the list regardless of its location in the list, and in such a way as to preserve the order of the remaining entries in the list. Whenever the top entry in the list changes (whether through an insertion or removal), the single status display is updated to show the new top value.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority of Chinese Patent Application No. 200910101642.X filed Aug. 20, 2009, which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] Exemplary embodiments of the invention generally relate to a light emitting diode (“LED”) circuit and, more particularly, to a pulse width modulation (“PWM”) dimming circuit for LED, and more particularly.
[0003] A high power LED lamp has such advantages as high luminous efficiency, long life, and environmental protection when compared to incandescent and/or fluorescent lighting. It is believed that using LED instead of incandescent, fluorescent, and other traditional lighting will be a new trend in the coming years. LED has simplicity of driving and controlling, and illumination intensity is easy to be adjusted flexibly. LED dimming modes usually comprise DC dimming, PWM dimming and other dimming. Compared with DC dimming, PWM dimming has advantages of a constant lighting color, and good stability at low brightness.
[0004] Typically, a constant-current LED driver with loop compensation methods as a current closed-loop has slow current loop dynamic response. It is difficult for the output current to fast-track to PWM dimming signal. Thus LED lamp current can not reach the desired chopping regulation with the variation PWM signal duty cycle.
BRIEF DESCRIPTION OF THE INVENTION
[0005] Exemplary embodiments of the present invention relate to a circuit for providing a PWM dimming circuit for LED.
[0006] In one exemplary embodiment, the circuit comprises a main LED drive circuit, a LED load connected to the main LED drive circuit, a current loop configured to measure output current from the LED load, a current loop regulation circuit connected to the current loop, a main control circuit configured to receive a signal from the current loop when the LED load produces an output current, and a PWM dimming controller configured to provide a signal to control the current loop regulation circuit and to make the current loop operate in a closed-loop mode when the LED load produces the output current and to provide a shutdown signal to the main control circuit when the LED load does not produce the output current. When the output current is detected, the main control circuit controls the main LED drive circuit to set its output current at a predetermined load current. When the output current is not detected, the main control circuit controls the LED driver main circuit to shut down.
[0007] In another exemplary embodiment, the circuit comprises a main LED drive circuit, a LED load connected to the main LED drive circuit, an output capacitor C connected in parallel to the main LED drive circuit and the LED load, a current loop configured to measure output current from the LED load, a current loop regulation circuit connected to the current loop, a main control circuit configured to receive a signal from the current loop when the LED load produces an output current, an output control switch connected between the LED load and the current loop, and a PWM dimming controller configured to controls the output control switch to let in a conduction state and to provide a signal to control the current loop regulation circuit and makes the current loop work in a closed-loop mode when the LED load produces the output current and to provide a shutdown signal to the main control circuit and the output control switch when the LED load does not produce the output current. When the output current is detected, the main control circuit controls the main LED drive circuit to set its output current at a predetermined load current. When the output current is not detected, the main control circuit controls the LED driver main circuit and the output control switch to shut down.
[0008] In yet another exemplary embodiment, the circuit comprises a main LED drive circuit, a LED load connected to the main LED drive circuit, an output capacitor connected in parallel to the main LED drive circuit and the LED load, a current loop configured to measure output current from the LED load, a current loop regulation circuit connected to the current loop, a main control circuit configured to receive a signal from the current loop when the LED load produces an output current, an output control switch connected between the LED load and the current loop, and a PWM dimming controller configured to control the output control switch to let in a conduction state and to provide a signal to control the current loop regulation circuit and make the current loop work in a closed-loop mode when the LED load produces the output current and to provide a shutdown signal to the output control switch when the LED load does not produce the output current. When the output current is detected, the main control circuit controls the main LED drive circuit to set its output current at a predetermined load current.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] A more particular description of the invention briefly described above will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. Understanding that these drawings depict only typical embodiments of the invention and are not therefore to be considered limiting of its scope, the invention will be described and explained with additional specificity and detail through the use of the accompanying drawings in which:
[0010] FIG. 1 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor;
[0011] FIG. 2 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration;
[0012] FIG. 3 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration;
[0013] FIG. 4 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor;
[0014] FIG. 5 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor;
[0015] FIG. 6 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration;
[0016] FIG. 7 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration;
[0017] FIG. 8 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration;
[0018] FIG. 9 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration; and
[0019] FIG. 10 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED further illustrating an exemplary LED driver main circuit.
DETAILED DESCRIPTION OF THE INVENTION
[0020] Reference will be made below in detail to exemplary embodiments of the invention, examples of which are illustrated in the accompanying drawings. Wherever possible, the same reference numerals used throughout the drawings refer to the same or like parts. Exemplary embodiments of the invention solve problems in the art by providing a pulse width modulation (PWM) dimming circuit for a LED lighting application.
[0021] For the sake of easy explain, the description of exemplary embodiments of the invention are provided under the following assumptions. It is supposed when a duty cycle of a PWM dimming control signal is maximum, LED lights are the brightest, and when minimum, LED lights are the darkest. At a time of a high PWM signal, the LED load has an output current, called the ‘Ton’ time. At a time of a low PWM signal, LED load (or simply LED) has no output current, called the ‘Toff’ time.
[0022] Exemplary embodiments of the present invention adopts a PWM dimming circuit for the LED load which is applicable to three different occasions: (1) an output of a LED driver main circuit does not include an output capacitor; (2) the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration; (3) the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration.
[0023] FIG. 1 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor. The PWM dimming circuit for the LED comprises a LED drive main circuit 10 , a main control circuit 12 , a PWM dimming controller 14 that provides a signal (throughout this document PWM dimming control signal is used interchangeably with the controller that provides the signal), a current loop regulation circuit 16 , a current loop 18 , a LED load 20 (one or more LED strings), and a shutdown signal 22 produced by the PWM dimming controller 14 . As further is illustrated an AC power source 24 is connected to the LED driver main circuit 10 .
[0024] During the ‘Ton’ time, the PWM dimming control signal 14 controls the current loop regulation circuit 16 and makes the current loop 18 work in a “normal” closed-loop mode where a current sampling signal compares with an internal current reference signal of the current loop 18 , and a output signal is adjusted through the closed-loop and feeds to the main control circuit 12 . The main control circuit 12 acts on the main LED drive circuit 10 to set its output current as the predetermined load current. The PWM dimming control signal 14 does not send a shutdown signal to the main control circuit 12 . During the ‘Toff’ time, the PWM dimming control signal 14 controls the current loop regulation circuit 16 . The current sampling signal of the current loop is forced to be equal to the current reference signal by the current loop regulation circuit output, so that the output of the current loop 18 remains unchanged. At the same time, the PWM dimming control signal 14 sends the shutdown signal 22 to the main control circuit 12 . The main control circuit 12 acts on the Main LED drive circuit 10 and shuts it down, and the output current turns zero.
[0025] The PWM dimming control signal 14 , or controller, regulates the current loop 18 through the current regulation circuit 16 in the ‘Toff’ time, so that the output of current loop 18 remains unchanged. The PWM dimming control signal 14 controls shutdown signal simultaneously to turn the LED driver main circuit 10 off in the Toff time and to reduce the output current to zero rapidly. Due to the current loop output remaining unchanged during the ‘Toff’ period of time, the load current tracks the current reference signal only in the ‘Ton’ period of time. Thus the LED load current can track the variation of the PWM dimming control signal duty cycle fast, or at a very high rate of speed.
[0026] FIG. 2 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor C, needs to turn a main control circuit off in ‘Toff’ duration. In this occasion, the PWM dimming circuit for the LED comprises an LED driver main circuit 10 , an output capacitor C, a main control circuit 12 , an output control switch 26 , a PWM dimming control signal (or controller) 14 , a current loop regulation circuit 16 , a current loop 18 , a LED load 20 (one or more LED strings), and a shutdown signal 22 .
[0027] During the ‘Ton’ time, the PWM dimming control signal 14 controls the output control switch 26 to let it operate in a conduction state. The PWM dimming control signal 14 further controls the current loop regulation circuit 16 and makes the current loop 18 work in the normal closed-loop mode where the current sampling signal compares with the internal current reference signal of the current loop 18 , and the output signal is adjusted through the closed-loop and feeds to the main control circuit 12 . The main control circuit 12 acts on the LED drive main circuit 10 to set its output current as the predetermined load current. The PWM dimming control signal 14 does not send a shutdown signal 22 to the main control circuit 12 . During the ‘Toff’ time, the PWM dimming control signal 14 controls the current loop regulation circuit 16 . The current sampling signal of the current loop 18 is forced to be equal to the current reference signal by the output of the current loop regulation circuit 16 , so that the output of current loop 18 remains unchanged. The PWM dimming control signal 14 sends the shutdown signal 22 to the main control circuit 12 to turn off the LED driver main circuit. At the same time, the PWM dimming control signal 14 controls the output control switch off and the LED load current turns zero.
[0028] The PWM dimming control signal 14 regulates the current loop through the current regulation circuit 16 in the ‘Toff’ time, so that the output of current loop 18 remains unchanged. Because of energy storage in the output capacitor C, the PWM dimming control signal 14 turns the output control switch 26 off to rapidly reduce the output current to zero in the ‘Toff’ time. Due to the current loop output remaining unchanged during the ‘Toff’ period of time, the load current tracks current reference signal only in the ‘Ton’ period of time. Thus the LED load current can track the variation of the PWM dimming control signal 14 duty cycle rather quickly, or rapidly.
[0029] The output capacitor C does not output energy to the load 20 any more in the ‘Toff’ time. When the ‘Toff’ is long (small duty cycle), the capacitor voltage may be increased, causing the load current amplitude increased (higher than the set value). In this case, the PWM dimming control signal 14 sends shutdown signal to the main control circuit 12 in the ‘Toff’ time. It stops the LED driver main circuit 10 from working, so that the voltage on the output capacitor C can be controlled without increasing and the load current amplitude will not change. As a result, the ideal variation of the output current of the LED driver main circuit 10 can be achieved and can also obtain a good LED lamp dimming effect.
[0030] FIG. 3 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration. The PWM dimming circuit for the LED comprises a LED driver main circuit 10 , an output capacitor C, a main control circuit 12 , an output control switch 26 , a PWM dimming control signal (or controller) 14 , a current loop regulation circuit 16 , a current loop 18 , and a LED load 20 (one or more LED strings).
[0031] During the ‘Ton’ time, the PWM dimming control signal 14 controls the output control switch 26 to let it operate in the conduction state; the PWM dimming control signal 14 controls the current loop regulation circuit 16 and makes the current loop 18 work in a closed-loop mode where a current sampling signal compares with an internal current reference signal of the current loop 18 , and the output signal feeds to the main control circuit 12 . The main control circuit 12 acts on the LED driver main circuit 10 to set its output current as the predetermined load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the current loop regulation circuit 16 . The current sampling signal of the current loop 18 is forced to be equal to the current reference signal by the output of the current loop regulation circuit 16 , so that the output of the current loop 18 remains unchanged. At the same time, the PWM dimming control signal 14 controls the output control switch 26 in the off state and the LED load current turns zero.
[0032] The PWM dimming control signal 14 regulates the current loop 18 through the current regulation circuit 16 in the ‘Toff’ time, so that the output of the current loop 18 remains unchanged. Because of energy storage of the output capacitor C, the PWM dimming control signal 16 turns the output control switch 26 off to reduce the output current to zero rapidly in the ‘Toff’ time. Due to the current loop output remaining unchanged during the ‘Toff’ period of time, the load current tracks current reference signal only in the ‘Ton’ period of time. Thus, the LED load current can track the variation of the PWM dimming control signal duty cycle fast.
[0033] The circuit structure is simpler in comparison with where the output of LED driver main circuit 10 , with an output capacitor C, needs to turn a main control circuit 12 off in ‘Toff’ duration, as illustrated in FIG. 2 . The capacity of the output capacitor C is required to be large enough in the main circuit design to ensure the output capacitor voltage will not rise in the longest ‘Toff’ case. As a result, constant amplitude of load current can be achieved to obtain a good dimming result.
[0034] In an exemplary embodiment, an output current waveform of LED driver main circuit 10 is a chopping square wave. The frequency and duty cycle of a square wave are the same as the PWM dimming control signal 14 and its amplitude remains unchanged. The average value of the output current is equal to the product of the output current amplitude and duty cycle. The output current duty cycle varies with the variation of the duty cycle of the PWM dimming control signal 14 , and always is consistent with it. In this way, the average output current varies with the duty cycle of the PWM dimming control signal 14 . Therefore, when the PWM signal duty cycle increases, the duty cycle of the output current is increased and the average output current is also increased, wherein the LED lamp is much brightened and/or vice versa.
[0035] FIG. 4 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor. The input of the LED driver main circuit 10 is an AC voltage Vin or 24 , and the positive output terminal connects the anode of the LED load 20 , while the cathode of the LED load 20 is connected with one end of a first resistor R 1 and one end of a second resistor R 2 . The current loop 18 comprises an integrated operational amplifier (op-amp) component or IC, a compensation network 28 , as well as the first resistor R 1 and the second resistor R 2 . A negative input terminal of the IC connects with the other end of the second resistor R 2 , and the other end of the first resistor R 1 is connected to the ground 30 . A positive input terminal of the IC is connected to a current-reference voltage Vref, and the compensation network 28 is in parallel with the negative input terminal and output terminal of the integrated op-amp IC. The output end of the IC connects with the main control circuit 12 . The current loop regulation circuit 16 consists of a first switch S 1 and its driving circuit 32 . The second terminal of the first switch S 1 is connected with the positive input terminal of the integrated op-amp IC and the current-reference voltage Vref, while the first terminal of the first switch S 1 is connected to ground 30 , and the third terminal of the first switch S 1 is connected with its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The PWM dimming control signal 14 controls the shutdown signal 22 , and the main control circuit 12 receives the shutdown signal 22 and the signal of the current loop 18 , and then output the signal to the LED driver main circuit 10 .
[0036] During the ‘Ton’ time, the PWM dimming control signal 14 does not output a shutdown signal 22 to the main control circuit 12 . The PWM dimming control signal 14 controls the output of the driving circuit 32 to be low, and the switch S 1 is turned off. The current loop 18 works in the normal closed-loop mode, namely that the current sampling signal is input to the negative input terminal of the integrated op-amp IC by resistor R 1 , then it compares with the current-reference signal Vref of the positive terminal of the integrated op-amp IC, and outputs the signal to the main control circuit 12 . The main control circuit 12 acts on the LED driver main circuit 10 to set its output current as the predetermination load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the output of the driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of the current loop 18 and the current-reference signal Vref are zero, and the current loop output remains unchanged. Meanwhile, the PWM dimming control signal 14 sends the shutdown signal 22 to the main control circuit 12 . The main control circuit 12 acts on the LED driver main circuit 10 and shuts it down, then the output current turns zero.
[0037] FIG. 5 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED with an output of the LED driver main circuit not including an output capacitor. The input of the LED driver main circuit 10 is the AC voltage Vin, and the positive output terminal connects an anode of the LED load 20 , while the cathode of the LED load is connected with one end of a first resistor R 1 and one end of a second resistor R 2 . The current loop 18 comprises an integrated operational amplifier IC, a compensation network 28 , as well as the first resistor R 1 and the second resistor R 2 . A negative input terminal of the IC connects with the other end of the second resistor R 2 , and then the other end of the first resistor R 1 is connected to the ground 30 . A positive input terminal of the IC is connected to one end of a third resistor R 3 , while the other end of the resistor R 3 connects to the current-reference voltage Vref. The compensation network 28 is connected in parallel with the negative input terminal and the output of the integrated op-amp IC. The IC output terminal connects with the main control circuit 12 . The current loop regulation circuit 16 consists of one switch S 1 and its driving circuit 32 . The second terminal of the switch 32 is connected to the negative input terminal of the integrated op-amp IC and the second resistor R 2 , while the first terminal of the switch S 1 is connected to the current-reference signal Vref and the third resistor R 3 , and the third terminal of the switch S 1 connects with its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The PWM dimming control signal 14 controls the shutdown signal 22 , and the main control circuit 12 receives the shutdown signal and the signal of the current loop 18 , then outputs the control signal to the LED driver main circuit 10 .
[0038] During the ‘Ton’ Time, the PWM dimming control signal 14 does not output a shutdown signal 22 to the main control circuit 12 . The PWM dimming control signal 14 controls the output of the switch driving circuit 32 to be low, and the switch S 1 is off. The current loop 18 works in a closed-loop mode, namely that a current sampling signal is input to the negative input terminal of the integrated op-amp IC by resistor R 1 , then it compares with the current-reference signal Vref of the positive terminal of the integrated op-amp IC, and outputs the signal to the main control circuit 12 . The main control circuit 12 acts on the LED driver main circuit 10 to set its output current as the predetermination load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the output of the switch driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of current loop 18 is forced to be equal to the current-reference signal Vref, and the current loop output remains unchanged. Meanwhile, the PWM dimming control signal 14 sends shutdown signal to the main control circuit 12 . The main control circuit 12 acts on the LED driver main circuit 10 and shuts it down, then the output current turns zero.
[0039] FIG. 6 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration. The input of LED driver main circuit 10 is the AC voltage Vin, and the output is in parallel with the capacitor C. The positive output terminal of LED driver main circuit connects with the anode of the LED load, while the cathode of LED load is connected with the second terminal of an output control switch S 2 , and the third terminal of it connects with a second driving circuit 34 which is controlled by the PWM dimming control signal 14 . The first terminal of the switch S 2 connects with one end of resistor R 1 and one end of resistor R 2 . The current loop 18 is composed of an integrated operational amplifier IC, an compensation network 28 , as well as resistor R 1 and resistor R 2 . The negative input terminal of the IC connects with the other end of resistor R 2 , and the other end of resistor R 1 is connected to ground 30 . The positive input terminal of the IC is connected to the current-reference voltage Vref. The compensation network 28 is in parallel with the negative input terminal and the output of the integrated op-amp IC. The IC output connects with the main control circuit 12 . The current loop regulation circuit 16 consists of the switch S 1 and its driving circuit 32 . The second terminal of switch S 1 is connected to the positive input terminal of the integrated op-amp IC and the current-reference signal Vref, while the first terminal of it is connected to ground 30 and the third terminal of it connects with its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The PWM dimming control signal 14 controls the shutdown signal 22 , while the main control circuit 12 receives the shutdown signal 22 and the current loop regulation, then outputs the control signal to the LED driver main circuit 10 .
[0040] During the ‘Ton’ Time, the PWM dimming control signal 14 controls the output of the second driving circuit 34 to be high, and the output control switch S 2 is on. The PWM dimming control signal 14 controls the output of the output switch S 2 driving circuit 34 to be low, and the output control switch S 2 is off. The current loop regulation circuit 16 does not work (no change on the original working state of the current loop). The current sampling signal compares with the current-reference signal Vref inside of the current loop 18 and then outputs the signal to the main control circuit 12 to set its output current as the predetermination load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of the current loop 18 and the current-reference signal are zero, and the current loop output remains unchanged. The current loop 18 outputs the signal to the main control circuit 12 . The PWM dimming control signal 14 controls the output control switch S 2 to be off and the LED load current turns zero. Meanwhile, the PWM dimming control signal 14 sends the shutdown signal 22 to the main control circuit 12 and shuts the LED driver main circuit 10 down, and the output current turns zero.
[0041] FIG. 7 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with an output capacitor, needs to turn a main control circuit off in ‘Toff’ duration. The input of LED driver main circuit 10 is the AC voltage Vin, and the output is in parallel with the capacitor C. The positive output terminal of the LED driver main circuit 10 connects with the anode of the LED load 20 , while the cathode of the LED load 20 is connected with the second terminal of the output control switch S 2 , and the third terminal of it connects with the driving circuit 34 which is controlled by the PWM dimming control signal 14 . The first terminal of the output control switch S 2 connects with one end of resistor R 1 and one end of resistor R 2 . The current loop 18 is comprised of an integrated operational amplifier IC, compensation network 28 , as well as resistor R 1 and resistor R 2 . The negative input terminal of the IC connects with the other end of resistor R 2 , and the other end of resistor R 1 is connected to the ground 30 . The positive input terminal of the IC is connected to one end of resistor R 3 , and the other end of resistor R 3 connects with the current-reference voltage Vref. The compensation network 28 is in parallel with the negative input terminal and the output of the integrated op-amp IC. The IC output connects with the main control circuit 12 . The current loop regulation circuit 16 consists of the switch S 1 and its driving circuit 32 . The second terminal of switch S 1 is connected to the negative input terminal of the integrated op-amp IC. Furthermore, the first terminal of switch S 1 is connected to the current-reference signal Vref and resistor R 3 . The third terminal of switch S 1 is connected to its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The PWM dimming control signal 14 controls the shutdown signal 22 , while the main control circuit 12 receives the shutdown signal 22 and the current loop regulation signal, then outputs a control signal to the LED driver main circuit 10 .
[0042] During the ‘Ton’ Time, the PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be high, and the switch S 1 is on. The PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be low, and the switch S 1 is off. The current loop regulation circuit 16 does not work (no change on the original working state of the current loop). The current sampling signal compares with the current-reference signal Vref inside of the current loop 18 and then outputs the signal to the main control circuit 12 to set its output current as the predetermination load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of the current loop 18 equals to the current-reference signal and the current loop 18 output remains unchanged. The current loop outputs the signal to the main control circuit 12 . The PWM dimming control signal 14 controls the switch S 2 to be off and the LED load current turns zero. Meanwhile, the PWM dimming control signal 14 sends the shutdown signal 22 to the main control circuit 12 and shuts the LED driver main circuit 10 down, and the output current turns zero.
[0043] FIG. 8 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration. The input of the LED driver main circuit 10 is the AC voltage Vin, and the output is in parallel with the capacitor C. The positive output terminal of the LED driver main circuit 10 is connected to the anode of the LED load 20 , while the cathode of the LED load 20 is connected with the second terminal of the output control switch S 2 , and the third terminal of it connects with its driving circuit 34 which is controlled by the PWM dimming control signal 14 . The first terminal of the switch S 2 connects with one end of resistor R 1 and one end of resistor R 2 . The current loop 18 comprises an integrated operational amplifier IC, a compensation network 28 , as well as resistor R 1 and resistor R 2 . The negative input terminal of the IC connects with the other end of resistor R 2 , and the other end of resistor R 1 is connected to ground 30 . The positive input terminal of the IC is connected to the current-reference voltage Vref. The compensation network is in parallel with the negative input terminal and output of the integrated op-amp IC. The IC output connects with the main control circuit 12 . The current loop regulation circuit 16 comprises the switch S 1 and its driving circuit 32 . The second terminal of switch S 1 is connected to the positive input terminal of the integrated op-amp IC and the current-reference signal Vref. The first terminal of switch S 1 is connected to ground 30 . The third terminal of switch S 1 is connected to its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The main control circuit 12 receives the current loop regulation, then outputs control signal to the LED driver main circuit.
[0044] During the ‘Ton’ Time, the PWM dimming control signal controls the output of the switch S 2 driving circuit 34 to be high, and the switch S 2 is on. The PWM dimming control signal 14 controls the output of the switch S 1 driving circuit to be low, and the switch S 1 is off. The current loop regulation circuit 16 does not work (no change on the original working state of the current loop). The current sampling signal compares with the current-reference signal Vref inside of the current loop and then outputs the signal to the main control circuit 12 to set its output current as the predetermination load current. During the ‘Toff time’, the PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of the current loop 18 and the current-reference signal turn zero, and the current loop output remains unchanged. The current loop outputs signal to the main control circuit 12 . The PWM dimming control signal controls the switch S 2 to be off and the LED load current turns zero.
[0045] FIG. 9 is an exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED where the output of LED driver main circuit, with the output capacitor, but does not need to turn the main control circuit off in ‘Toff’ duration. The LED driver output includes an output capacitor C and the main circuit is required to be shutdown during the ‘Toff’ time. The input of the LED driver main circuit is the AC voltage Vin, and the output is in parallel with the capacitor C. The positive output terminal of the LED driver main circuit 10 connects with the anode of LED light load, while the cathode of the LED light load is connected with the second terminal of the output control switch S 2 , and the third terminal of it connects with its driving circuit 34 which is controlled by the PWM dimming control signal 14 . The first terminal of the switch S 2 connects with one end of resistor R 1 and one end of resistor R 2 . The current loop 18 comprises an integrated operational amplifier IC, a compensation network 28 , as well as resistor R 1 and resistor R 2 . The negative input terminal of the IC is connected to the other end of resistor R 2 , and the other end of resistor R 1 is connected to ground 30 . The positive input terminal of the IC is connected to one end of a resistor R 3 , and the other end connects with the current-reference voltage Vref. The compensation network 28 is in parallel with the negative input terminal and output of the integrated op-amp IC. The IC output connects with the main control circuit 12 . The current loop regulation circuit 16 comprises the switch S 1 and its driving circuit 32 . The second terminal of switch 51 is connected with the negative input terminal of the integrated op-amp IC. And the first terminal of switch S 1 connects with the current-reference signal Vref and resistor R 3 . The third terminal of switch S 1 connects with its driving circuit 32 which is controlled by the PWM dimming control signal 14 . The main control circuit 12 receives the current loop regulation, then outputs a control signal to the LED driver main circuit 10 .
[0046] During the ‘Ton’ Time, the PWM dimming control signal 14 controls the output of the switch S 2 driving circuit 34 to be high, and the switch S 2 is on. The PWM dimming control signal 14 controls the output of the switch S 1 driving circuit to be low, and the switch S 1 is off. The current loop regulation circuit 16 does not work (no change on the original working state of the current loop). The current sampling signal compares with the current-reference signal Vref inside of the current loop 18 and then outputs signal to the main control circuit to set its output current as the predetermination load current. During the ‘Toff’ time, the PWM dimming control signal 14 controls the output of the switch S 1 driving circuit 32 to be high, and the switch S 1 is on. The current sample signal of the current loop 18 is equal to the current-reference signal, and the current loop output remains unchanged. The current loop 18 outputs the signal to the main control circuit 12 . The PWM dimming control signal 14 controls the switch S 2 to be off and the LED load current turns zero.
[0047] FIG. 10 is another exemplary embodiment of a circuit diagram of a PWM dimming circuit for a LED as disclosed in FIG. 8 , further illustrating an exemplary LED driver main circuit and an exemplary compensation network. As illustrated, the LED driver main circuit 10 comprises a transformer T 1 , such as but not limited to a dual pole transformer, a diode D 1 , a bridge rectifier BD 1 , and a switch S 1 . The switch S 1 may be a solid state switch. Also, as illustrated, the other switches S 2 , S 3 may also be solid state switches. As illustrated the third solid state switch S 2 has a first lead connected to the a second driving circuit, a second lead connected to the integrated op-amp IC, and a third lead connected to ground. The compensation network 28 comprises a second capacitor C 2 in series with a third resistor R 3 .
[0048] Thus, in an exemplary embodiment, the present invention provides for a PWM dimming circuit for LED lighting applications. The circuit includes a main LED drive circuit, a main control circuit, a PWM dimming control signal, a current loop regulating circuit, a current loop, and an LED load. The output current waveform of the LED drive circuit is chop square wave, the frequency and duty cycle of which are the same as that of the PWM dimming control signal, and its amplitude remains constant. The average output current equals a product of the output current amplitude and the duty cycle. The output current's duty cycle varies with the duty cycle of the PWM dimming control signal, and they always keep line with each other. In this way, the average output current varies with the duty cycle of the PWM dimming control signal. As a result, when the PWM dimming control signal's duty cycle increases, the duty cycle of the output current and the average output current increase, so the LED lamp gets brighter, and the vice versa. Furthermore, LED lamp current can change quickly with the PWM signal duty cycle to get a good dimming result.
[0049] It will be understood that examples are just the illumination of the present invention, but not limited to the invention. All extended solution or substitution based on the principle and content of this invention should be regarded as the inventors' claims to be protected. Furthermore, while the invention has been described with reference to various exemplary embodiments, it will be understood by those skilled in the art that various changes, omissions and/or additions may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed as the best mode contemplated for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated, any use of the terms first, second, etc., do not denote any order or importance, but rather the terms first, second, etc., are used to distinguish one element from another.
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A PWM dimming circuit for a LED load including a LED load connected to the main LED drive circuit, a current loop configured to measure output current from the LED load, a current loop regulation circuit connected to the current loop, a main control circuit configured to receive a signal from the current loop when the LED load produces an output current, and a PWM dimming controller configured to provide a signal to control the current loop regulation circuit and to make the current loop operate in a closed-loop mode when the LED load produces the output current and to provide a shutdown signal to the main control circuit when the LED load does not produce the output current. When the output current is detected, the main control circuit controls the main LED drive circuit to set its output current at a predetermined load current.
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BACKGROUND OF THE INVENTION
The present invention relates to a humidity detector using a humidity detecting element having a humidity sensing portion formed by sintering a metal oxide or metal oxides on a heat resistant wire coil.
There is well known a method for measuring the humidity in air, which utilizes the principle that the heat conductivity in a space varies depending upon the quantity of water vapor contained in the space, for example, as disclosed in U.S. Pat. No. 1,855,774.
The above method is realized by the construction made by the incorporation, in a bridge circuit, of a detecting element disposed in a measuring atmosphere in many cases and a reference element disposed in a space of the known humidity and having the same temperature-resistance characteristic as the detecting element.
A thermistor and a platinum wire are utilized as a detecting element.
A method as described in U.S. Pat. No. 4,419,888 is based on the aforementioned principle. This method involves supplying an electric current to a detecting element disposed in a measuring atmosphere and having a temperature characteristics found in a thermistor or the like to heat the detecting element to a temperature higher than that of such atmosphere. The resistance value of the detecting element is varied depending upon the quantity of water vapor contained in the above atmosphere, and this variation is detected. Then, the humidity in such atmosphere is detected from such variation.
There is also known a solid state thermal conductive gas detecting method which employs an element made by applying an n-type semiconductor such as SnO 2 and ZnO onto a platinum wire, as disclosed in Japanese Patent Publication No. 34640/79. In such a detecting device, when an electron donative gas such as a combustible gas has been adsorbed on a gas detecting portion made of a metal oxide semiconductor such as SnO 2 , the electron concentration in the detecting portion increases, and with the increase in electric conductivity, the increase in electron concentration promotes an increase in heat conductivity. As a result, the two actions reducing the temperature of the detecting portion cause the resistance of the platinum wire coil disposed at the center of the detecting portion to be reduced, thus detecting the concentration of the gas which is to be detected.
However, the conventional devices are accompanied by various problems. The output of the heat conduction type humidity detecting element with platinum employed as a detecting element is substantially smaller than that of the aforementioned thermistor heat conduction type humidity detecting element. Moreover, the platinum coil detecting element is very sensitive in thermal dissipation at an operating temperature of about 200° C. and is liable to be influenced by a slight mechanical vibration and wind.
In general, if an electric current is previously supplied so that the temperature of the detecting element may reach a level higher than the atmosphere temperature, the sensitivity can be improved. However, there is a problem that when the platinum coil detecting element is brought into a higher operating temperature, the output is unstable.
In the thermistor heat conduction type himidity detection, when the thermistor is heated to 200° C. or more, it may be broken by the self-heating.
The element made by applying an n-type semiconductor on the platinum wire has a relatively high sensitivity because of the purpose of detecting a gas, but has a lower sensitivity in humidity and hence, is not suitable for use as a humidity detecting element. Further, because the temperature at which the metal oxide semiconductor has been sintered is relatively low (at 800° C. to 900° C.), the operation in a hot and humid atmosphere (e.g., at 80° C. and 95% RH) causes the generation of a micro-crack which will grow into a large crack in a short time, resulting in a substantial variation in the resistance value. This is also a serious disadvantage.
SUMMARY OF THE INVENTION
It is an object of the present invention to povide a humidity detector wherein the drawbacks found in the conventional devices are overcome.
It is another object of the present invention to provide a humidity detector which uses an operating principle different from that of the foregoing heat conduction type humidity detecting element and enables the measurement in a wider range of a lower humidity to a higher humidity, and further, which is durable to the variations in surroundings such as a mechanical vibration.
According to the present invention, the above objects are accomplished by providing a humidity detector comprising a humidity sensing element consisting of a heating resistance wire coil and a humidity sensing portion of a metal oxide or metal oxides sintered on the coil with the opposite ends of the coil being exposed, heating means for energizing the coil to increase the temperature of the humidity sensing portion to a level higher than the temperature in an atmosphere whose humidity is to be measured, and resistance variation detecting means for detecting the variation in resistance between the opposite ends of the coil depending upon the humidity contained in the atmosphere.
With such an arrangement, the bulk resistance of the humidity sensing portion formed by the sintering is reduced by the adsorption of moisture in the atmosphere when the humidity detecting element is heated to a given temperature higher than the temperature in the atmosphere. As a result, the variation in resistance between the opposite ends of the coil is detected.
The reduction in resistance value causes each molecule of water to be adsorbed on the humidity sensing portion consisting essentially of Al 2 O 3 , so that a proton dissociated in the field of a crystal particle is supplied to form an electrolyte layer, thereby providing an increase in electric conductivity of the humidity sensing portion. In short, a carrier for a charge is a cation, and a mechanism for varying the resistance is different from that in the conventionally proposed element.
The metal oxide may be Al 2 O 3 or a mixture of Al 2 O 3 with at least one metal oxide selected from the group consisting of SnO 2 , ZnO, TiO 2 and MgO, and such metal oxide or mixed metal oxides may be sintered to the heating resistance wire coil. The operation of the humidity detector including the humidity detecting element having thus-formed humidity sensing portion may provide outputs equivalent to or over those in use of the platinum heat conduction type humidity detecting element.
Since the metal oxide or oxides is or are firmly sintered to the heating resistance wire coil at a high temperature, the stability in zero balance and output voltage against the influences of a mechanical vibration and wind is extremely good even during operation at a temperature as high as 400° C.
If the sintering has been conducted at an average temperature as extremely high as 1250° C., no micro-cracks can be produced in the metal oxide sintered portion even during operation in a hot and humid atmosphere, leading to an extremely high reliability.
In addition, bringing operating temperature of the humidity detecting element to a level of about 400° C. facilitates the adsorption and desorption of water vapor, an increase in response speed and a substantial reduction in hysteresis.
Further, from the fact that the operating temperature can be brought to a level of about 400° C. or more, any dirt may always be burned and hence, no particular cleaning is required, thus making it possible to conduct a repeated detection.
The above and other objects, features and advantages of the invention will become apparent from reading of the following description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional view of an embodiment of a humidity detecting element used in a humidity detector according to the present invention;
FIG. 2 is a circuit diagram illustrating an example of the humidity measurement by the humidity detecting element of the present invention and the heat resistance wire heat conduction type humidity detecting element;
FIG. 3 is a graph illustrating the output characteristics of the humidity detecting element of the present invention and the platinum heat conduction type humidity detecting element;
FIG. 4 is a graph illustrating the output characteristic of the humidity detecting element according to the present invention with respect to the operating temperature; and
FIG. 5 is a block diagram illustrating a second embodiment of a humidity detector according to the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will now be described by way of the preferred embodiments with reference to the accompanying drawings.
FIG. 1 is a view of an embodiment of a humidity detecting element used in a humidity detector according to the present invention. Terminal pins 4 and 5 are embedded in a stem 3 of an insulating structure to extend vertically upwardly and downwardly from the stem 3.
A platinum wire having a diameter of 0.05 mm is wound for 17 turns at a uniform pitche with a coil diameter of 0.5 mm (the coiled portion having a length of 2.5 mm) to form a heat resistance wire coil 1.
Five materials of Al 2 O 3 , SnO 2 , ZnO, TiO 2 , and MgO are prepared as materials for a humidity sensing portion, and one or more metal oxides of SnO 2 , ZnO, TiO 2 and MgO are incorporated in Al 2 O 3 at 12 kinds of weight ratios given in Table 1 which will be given hereinbelow, thereby giving samples. A sample of simple Al 2 O 3 is also prepared. The respective samples as a material for the humidity sensing portion are dissolved with pure water and each is directly applied on a respective platinum coil 1. The resulting materials are air dried and then fired at a temperature of about 1,000° C. to form respective humidity sensing portions.
The contour of each humidity sensing portion is cylindrical with a diameter of 1.2 mm and a length of 3.0 mm.
The terminal pins 4 and 5 are embedded in a stem 3 of an insulating structure to extend vertically upwardly and downwardly from the stem 3.
The opposite ends of each platinum coil 1 having the humidity sensing portion formed thereon are respectively secured to the upper ends of such a pair of terminals 4 and 5 embedded in a stem 3, by electric welding. Then, each platinum coil 1 is energized so that the average temperature thereof may be maintained at 1250° C., and the metal oxide 1 is further firmly sintered.
A respective perforated cap 6 is sealingly mounted on each stem 3 to form 13 types (Nos. 1 to 13) of humidity detecting elements 7. It is to be noted that in the sample No. 13, only Al 2 O 3 is sintered on the heat resistance coil. The sample No. 14 consists of only the heat resistance coil and prepared as corresponding to the conventional platinum wire humidity sensing element. The humidity sensing elements formed in the above manner are evaluated using a bridge circuit shown in FIG. 2.
It should be noted that this bridge circuit can be utilized as an actual humidity measuring circuit, and a device comprising a humidity detecting element according to the present invention being incorporated in such a bridge circuit forms a first embodiment of a humidity detector according to the present invention.
For this evaluation, 13 reference elements of the same kinds as those described above are likewise prepared which have been formed in the same process until the metal oxides 2 of the humidity detecting elements 7 have been firmly sintered. Each of thus formed elements is sealed by a sealing cap in dry air with a dew point of about -45° C. and the resulting element is referred to as a reference element 8.
Further, for comparison, a similar reference element is also prepared for the sample No. 14.
The humidity detecting element 7 and the reference element 18 are connected in series to a 2.0 V power source 11, and a series-circuit of resistances 9 and 10 each having a resistance value of approximately 1 KΩ and forming a bridge side is further connected. The resistances 9 and 10 are finely adjusted near 1 KΩ in accordance with the resistance value of the individual element.
An electric current of about 240 mA is supplied to the humidity detecting element and the reference element, so that each element is heated to about 400° C. At this time, the humidity detecting element 7 and the reference element 8 are thermally coupled by an heat evening plate to have the same temperature.
In the measuring circuit shown in FIG. 2, each reference element 8 is sealed in the dry air with a dew point of about -45° C. and with a saturated absolute humidity of about 0.1 g/m 3 which value is considered as a standard condition. When the humidity detecting element is in such a condition, the resistance side of the bridge is adjusted so that the bridge may be balanced (have an output of zero).
In FIG. 3, there is shown an output given when a humidity detecting element using the material of the sample No. 5 (Al 2 O 3 :SnO 2 :MgO=2:1:1) shown in Table 1 and the reference element are connected in the bridge circuit shown in FIG. 2, wherein curves (A), (B), and (C) indicate output voltages when the open air is at 20° C., 80° C. and 100° C., respectively.
It can be seen from FIG. 3 that the resistance value of the humidity detecting element 7 decreases with the increase in humidity. Indicated by a curve (D) in FIG. 3 is the result which has been obtained from the determination of the output characteristic, with the average temperature of the platinum coil (corresponding to the conventional humidity sensing element of platinum wire) of the sample No. 14 being increased up to about 400° C. In this case, the resistances 9 and 10 were at 1.000 KΩ and 1.051 KΩ, and the power source was at 1.7 V. The reference element 8 was sealed in the dry air with the dew point of about -45° C., and the temperature of the open air was 80° C.
As indicated by (D) in FIG. 3, if the self-heated temperature of platinum is increased to 400° C., the output is very large, and the higher humidity up to which the continuous measurement is available from the lower humidity is of about 250 g/m 3 . This is 1.7 times the value obtained upon the operation at 200° C. However, the platinum coil heated to the substantially high temperature of 400° C. is very sensitive in thermal dissipation, so that the condition of thermal dissipation is varied under the influence of a slight mechanical vibration and a wind, resulting in a lack of stability in zero balance and output voltage of the bridge. For this reason, it is necessary with the humidity sensing element to prepare a housing case extremely difficult to be influenced by the variation in surroundings, attendant with the difficulty in reduction in size and cost.
Given in Table 1 are the bridge outputs obtained for every sample given in Table 1 under the conditions of an open air temperature of 80° C., an absolute humidity of 240 g/m 3 kept constant, and an operating temperature of 400° C. of the humidity sensing portion in the measuring circuit shown in FIG. 2. The samples Nos. 5 and 6 exhibit a sensitivity larger than that of the sample No. 14. Some samples have an output lower than that of the simple platinum coil (the sample No. 14), regardless of the enlargement in surface area due to the metal oxide sinters. This indicates that the humidity detecting element of the present invention is not intended to detect only the deviation in heat conductivity between the dry air and the wet air and on the contrary, the proportion in contribution to the output of electric conductivity is larger.
An examination will now be made for the reaction of the sample No. 5 to a combustible gas.
With the use of the above-described bridge circuit, the output of -35.0 mV reverse to the humidity is provided at an isobutane concentration of 2%, wherein the operating temperature is 400° C. This means that the sample No. 5 obviously presents the action of a catalyst on the combustible gas, thereby causing the contact combustion to increase the temperature of the humidity sensing portion.
The action of the metal oxide semiconductors of SnO 2 and ZnO is ineffective on the combustible gas and effective on the humidity, which is the nature peculiar to the present invention.
After the resistances 9 and 10 are first finely adjusted in the measuring circuit shown in FIG. 2 to provide a zero balance, the drift of the zero balance due to the variation in humidity is on the order of 1 mV, thus making it possible to provide a significant temperature compensation effect.
It can be understood from the curves of the bridge outputs in FIG. 3 that the temperature dependence is also extremely small.
The measurement of the response speeds of the individual samples in the measuring circuit shown in FIG. 2 showed that the response speed is as high as 4 to 9 seconds for adsorption and 7 to 12 seconds for desorption, and the difference in output between the adsorption and desorption, i.e., a so-called hysteresis, is also extremely small.
Even in a resistance temperature detector or thermistor temperature detector having a consistent humidity coefficient and thermal dissipation constant, the temperature compensation is sufficiently available, if the reference element 8 is incorporated at a suitable point in the bridge circuit.
In FIG. 4, there is shown the result of the measurement for how the bridge output varies when the voltage of the power source 11 is varied and the operating temperatures of the humidity detecting element 7 and the reference element 8 are varied in the measuring circuit shown in FIG. 2. The conditions in the measuring atmosphere are at 80° C. and 240 g/m 3 which are kept constant, and use is made of the humidity detecting element 7 and the reference element 8 of the type defined in sample No. 5 in Table 1. It can be understood from FIG. 4 that if the operating temperature of the humidity detecting element 7 is on the order of 400° C., a sufficiently large output is provided.
The humidity detector can also be realized by the processing of information on the variation in resistance of the humidity detecting element and information on the atmospheric temperature rather than by use of the aforementioned bridge circuit.
FIG. 5 is a block diagram illustrating a second embodiment of a humidity detector according to the present invention. The humidity detecting element 7 and a temperature sensor 23 are contained in a measuring atmosphere, that is, the atmosphere whose humidity is to be measured. The information on the atmospheric temperature (t) take-in by the temperature sensor 23 is received into a microprocessor 24 where it is digitally converted. The humidity detecting element 7 and a resistance 22 are connected in series and supplied with a D.C. voltage from a power source. The resistance 22 does not have a temperature compensating function as the previously described reference element has. Therefore, the voltages at the opposite ends of the resistance 22 exhibit a temperature dependence. This temperature dependent portion can be approximated by the following general equation for the temperature resistance characteristic of a platinum temperature detector which will be described hereinbelow.
Rt=Ro(1+αt-βt.sup.2)
The constants Ro, α and β are previously stored in the memory of the microprocessor 24, and Rt is calculated from the atmosphere temperature (t) provided by the temperature sensor 23 and added or subtracted by a temperature dependent portion from the data taken-in from the resistance 22, thus giving the data of a humidity. The various calculations are made on the basis of the data on the temperature and the humidity to give indicating data of an absolute humidity, a relative humidity, a dew point, specific humidity, etc.
A humidity control device can be realized by the comparison of the above-described calculation results and a desired control value.
It can be understood by those skilled in the art that various modification for the embodiment which has been described in detail can be made within the scope of the present invention.
For the heat resistance wire coil of the humidity detecting element and the reference element, the example of the platinum wire has been given. In the present invention, such a coil is used not only as a resistance wire for maintaining the element at a constant temperature but also for detecting both of a heat conduction and an electric conduction and hence, a metal wire or noble metal alloy wire (e.g., platinum or platinum/iridium wire) having a temperature-resistance characteristic and which is difficult to oxidize at a higher temperature is required to provide a larger output.
In the measuring circuit shown in FIG. 2, the reference element 8 has been sealed in the dry air with a dew point of about -45° C. and with a saturated absolute humidity of about 0.1 g/m 3 which value is considered as a standard condition, and the deviation from such value has been measured, but the humidity in the atmosphere in which the reference element 8 is disposed may be set at any value, so that the deviation from such set value can be measured.
In addition, it is apparent that if the output from the bridge circuit shown in FIG. 2 is connected to a voltmeter or ammeter, the deviation in humidity can be measured, and an absolute humidity meter, a relative humidity meter, a dew-point meter, specific humidity meter and the like can be realized by the functional calculation of a signal from the temperature detector for detecting the open air temperature.
Further, if a voltage comparator is provided in the output of the bridge circuit or at a suitable point in the above meters, a humidity control device can readily be realized.
TABLE 1______________________________________Sample Weight Ratio OutputNo. Al.sub.2 O.sub.3 SnO.sub.2 ZnO TiO.sub.2 MgO (mV)______________________________________1 1 0 0 1 0 20.42 1 0 0 0 1 24.03 1 1 0 0 0 20.84 1 1 0 1 0 20.05 2 1 0 0 1 31.66 1 2 0 0 1 29.47 1 1 1 1 1 20.08 1 0 1 0 0 16.09 1 0 1 1 0 18.010 2 0 1 0 1 24.411 1 0 2 0 1 17.612 1 1 1 0 0 25.013* 1 0 0 0 0 22.0 14** 0 0 0 0 0 25.5______________________________________ *Sample No. 13 is produced by sintering only Al.sub.2 O.sub.3 to a heatin resistance wire coil. **Sample No. 14 is only a heating resistance wire coil and corresponds to the conventional platinum wire humidity sensing element.
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A humidity detector which is disclosed herein includes a humidity sensing element consisting of a heating resistance wire coil and a humidity sensing portion of a metal oxide or metal oxides sintered on the coil with the opposite ends of the coil being exposed, a heating circuit for energizing the coil to increase the temperature of the humidity sensing portion to a level higher than the temperature in a measuring atmosphere, and a resistance variation detecting circuit for detecting the variation in resistance between the opposite ends of the coil depending upon the humidity contained in the measuring atmosphere. The metal oxide may be Al2O3 or a mixture of Al2O3 with at least one selected from the group consisting of SnO2, ZnO, TiO2 and MgO.
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This application is a 35 U.S.C. 371 nationalization of PCT application PCT/EP2013/070619, filed Oct. 3, 2013, which claims priority to European patent application 12187519.9 filed Oct. 5, 2012, both of which are incorporated herein by reference.
This invention relates to acylaminopyrimidine derivatives, processes for their preparation, pharmaceutical compositions, and their use in therapy.
BACKGROUND OF THE INVENTION
The present invention relates to the use of acylaminopyrimidine derivatives in the treatment of viral infections, immune disorders, and cancer, or as a vaccine adjuvant, whereby the induction of interferon is desired. In the treatment of certain viral infections, regular injections of interferon (IFN-type 1) can be administered, as is the case for hepatitis C virus (HCV), For more information see reference Fried et. al. Peginterferon-alfa plus ribavirin for chronic hepatitis C virus infection, N Engl J Med 2002; 347: 975-82. Orally available small molecule IFN inducers offer the potential advantages of reduced immunogenicity and convenience of administration. Thus, novel IFN inducers are a potentially effective new class of drugs for treating virus infections. For an example in the literature of a small molecule IFN inducer having antiviral effect see De Clercq, E.; Descamps, J.; De Somer, P. Science 1978, 200, 563-565.
However there exists a strong need for novel interferon inducers having an improved safety profile compared to the compounds currently known.
BRIEF SUMMARY OF THE INVENTION
In accordance with the present invention a compound of formula (I) is provided
or a pharmaceutically acceptable salt, solvate or polymorph thereof, wherein
R 1A is selected from the group hydrogen, a substituted or unsubstituted acyl, or acyloxy group,
R 1B is selected from the group hydrogen, a substituted or unsubstituted acyl, or acyloxy group,
with the proviso that R 1A and R 1B are not both hydrogen,
R 2 is C 1-6 alkyl, C 1-6 alkoxy, arylalkyl or heteroarylalkyl, each of which is optionally substituted by one or more substituents independently selected from halogen, hydroxyl, amino, di-(C 1-6 )alkylamino, C 1-6 alkylamino, C 1-6 alkyl, C 1-6 alkoxy, C 3-6 cycloalkyl, carboxylic acid, carboxylic ester, carboxylic amide, heterocycle, bicyclic heterocycle, aryl, alkenyl, alkynyl, arylalkyl, heteroaryl, heteroarylalkyl, or nitrile and
R 3 is a C 1-8 alkyl, or arylalkyl each of which is optionally substituted by one or more substituents independently selected from halogen, hydroxyl, amino, C 1-6 alkyl, di-(C 1-6 )alkylamino, C 1-6 alkylamino, C 1-6 alkoxy, C 3-6 cycloalkyl, carboxylic acid, aromatic or aliphatic carboxylic ester, carboxylic amide, heterocycle, aryl, alkenyl, alkynyl, arylalkyl, heteroaryl, heteroarylalkyl, or nitrile.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A and 1B . Interferon levels measured in the liver ( FIG. 1A ) and in the plasma ( FIG. 1B ) after single oral administration of compound 1 at 15.5 mg/kg in mice.
FIGS. 2A and 2B . CXCL10 expression measured in the liver ( FIG. 2A )* and in the blood ( FIG. 2B ) after single oral administration of compound 1 at 15.5 mg/kg in mice. *one 4 h time point sample was removed due to high HPRT1 value
Induction of endogenous interferon and upregulation of CXCL10 was observed in the liver and blood/plasma in mice after oral administration of a single dose of compound 1.
DETAILED DESCRIPTION OF THE INVENTION
In a first embodiment the present invention provides compounds of formula (I) wherein R 1A and/or R 1B are substituted or unsubstituted acyl and wherein R 2 is C 1-6 alkyl preferably —CH 3 and R 3 is C 1-8 alkyl substituted with an alkylester.
In a second embodiment the present invention provides compounds of formula (I) wherein R 1A and/or R 1B are isobutyryl and wherein R 2 is —CH 3 , and R 3 is heptan-3-yl isobutyrate.
The compounds of formula (I) in any stereochemical form and their pharmaceutically acceptable salt, solvate or polymorph thereof have activity as pharmaceuticals, in particular as inducers of interferon.
So, in a further aspect the present invention provides a pharmaceutical composition comprising a compound of formula (I) or a pharmaceutically acceptable salt, solvate or polymorph thereof together with one or more pharmaceutically acceptable excipients, diluents or carriers.
Furthermore a compound of formula (I) or a pharmaceutically acceptable salt, solvate or polymorph thereof according to the current invention, or a pharmaceutical composition comprising said compound of formula (I) or a pharmaceutically acceptable salt, solvate or polymorph thereof can be used as a medicament.
Another aspect of the invention is that a compound of formula (I) or a pharmaceutically acceptable salt, solvate or polymorph thereof, or said pharmaceutical composition comprising said compound of formula (I) or a pharmaceutically acceptable salt, solvate or polymorph thereof can be used accordingly in the treatment of a disorder in which the induction of interferon is involved.
The term “alkyl” refers to a straight-chain or branched-chain saturated aliphatic hydrocarbon containing the specified number of carbon atoms.
The term “halogen” refers to fluorine, chlorine, bromine or iodine.
The term “acyl” refers to the group defined as —(C═O)R, where R is a substituted or unsubstituted alkyl, cycloalkyl, aryl, heteroaryl.
The term “acyloxy” refers to the group defined as —(C═O)OR, where R is a substituted or unsubstituted alkyl, cycloalkyl, aryl, heteroaryl.
The term “alkenyl” refers to an alkyl as defined above consisting of at least two carbon atoms and at least one carbon-carbon double bond.
The term “alkynyl” refers to an alkyl as defined above consisting of at least two carbon atoms and at least one carbon-carbon triple bond.
The term “cycloalkyl” refers to a carbocyclic ring containing the specified number of carbon atoms.
The term “alkoxy” refers to an alkyl (carbon and hydrogen chain) group singular bonded to oxygen (e.g. methoxy group or ethoxy group).
The term “aryl” means an aromatic ring structure optionally comprising one or two heteroatoms selected from N, O and S, in particular from N and O. Said aromatic ring structure may have 5, 6 or 7 ring atoms. In particular, said aromatic ring structure may have 5 or 6 ring atoms.
The term “bicyclic heterocycle” means an aromatic ring structure, as defined for the term “aryl” comprised of two fused aromatic rings. Each ring is optionally comprised of heteroatoms selected from N, O and S, in particular from N and O.
The term “arylalkyl” means an aromatic ring structure as defined for the term “aryl” optionally substituted with an alkyl group.
The term “heteroarylalkyl” means an aromatic ring structure as defined for the term “heteroaryl” optionally substituted by an alkyl group.
“Heterocycle” refers to molecules that are saturated or partially saturated and include ethyloxide, tetrahydrofuran, dioxane or other cyclic ethers. Heterocycles containing nitrogen include, for example azetidine, morpholine, piperidine, piperazine, pyrrolidine, and the like. Other heterocycles include, for example, thiomorpholine, dioxolinyl, and cyclic sulfones.
“Heteroaryl” groups are heterocyclic groups which are aromatic in nature. These are monocyclic, bicyclic, or polycyclic containing one or more heteroatoms selected from N, O or S. Heteroaryl groups can be, for example, imidazolyl, isoxazolyl, furyl, oxazolyl, pyrrolyl, pyridonyl, pyridyl, pyridazinyl, pyrazinyl . . . .
Pharmaceutically acceptable salts of the compounds of formula (I) include the acid addition and base salts thereof. Suitable acid addition salts are formed from acids which form non-toxic salts. Suitable base salts are formed from bases which form non-toxic salts.
The compounds of the invention may also exist in unsolvated and solvated forms. The term “solvate” is used herein to describe a molecular complex comprising the compound of the invention and one or more pharmaceutically acceptable solvent molecules, for example, ethanol.
The term “polymorph” refers to the ability of the compound of the invention to exist in more than one form or crystal structure.
The compounds of the present invention may be administered as crystalline or amorphous products. They may be obtained for example as solid plugs, powders, or films by methods such as precipitation, crystallization, freeze drying, spray drying, or evaporative drying. They may be administered alone or in combination with one or more other compounds of the invention or in combination with one or more other drugs. Generally, they will be administered as a formulation in association with one or more pharmaceutically acceptable excipients. The term “excipient” is used herein to describe any ingredient other than the compound(s) of the invention. The choice of excipient depends largely on factors such as the particular mode of administration, the effect of the excipient on solubility and stability, and the nature of the dosage form. The compounds of the present invention or any subgroup thereof may be formulated into various pharmaceutical forms for administration purposes. As appropriate compositions there may be cited all compositions usually employed for systemically administering drugs. To prepare the pharmaceutical compositions of this invention, an effective amount of the particular compound, optionally in addition salt form, as the active ingredient is combined in intimate admixture with a pharmaceutically acceptable carrier, which carrier may take a wide variety of forms depending on the form of preparation desired for administration. These pharmaceutical compositions are desirably in unitary dosage form suitable, for example, for oral, rectal, or percutaneous administration. For example, in preparing the compositions in oral dosage form, any of the usual pharmaceutical media may be employed such as, for example, water, glycols, oils, alcohols and the like in the case of oral liquid preparations such as suspensions, syrups, elixirs, emulsions, and solutions; or solid carriers such as starches, sugars, kaolin, diluents, lubricants, binders, disintegrating agents and the like in the case of powders, pills, capsules, and tablets. Because of their ease in administration, tablets and capsules represent the most advantageous oral dosage unit forms, in which case solid pharmaceutical carriers are obviously employed. Also included are solid form preparations that can be converted, shortly before use, to liquid forms. In the compositions suitable for percutaneous administration, the carrier optionally comprises a penetration enhancing agent and/or a suitable wetting agent, optionally combined with suitable additives of any nature in minor proportions, which additives do not introduce a significant deleterious effect on the skin. Said additives may facilitate the administration to the skin and/or may be helpful for preparing the desired compositions. These compositions may be administered in various ways, e.g., as a transdermal patch, as a spot-on, as an ointment. The compounds of the present invention may also be administered via inhalation or insufflation by means of methods and formulations employed in the art for administration via this way. Thus, in general the compounds of the present invention may be administered to the lungs in the form of a solution, a suspension or a dry powder.
It is especially advantageous to formulate the aforementioned pharmaceutical compositions in unit dosage form for ease of administration and uniformity of dosage. Unit dosage form as used herein refers to physically discrete units suitable as unitary dosages, each unit containing a predetermined quantity of active ingredient calculated to produce the desired therapeutic effect in association with the required pharmaceutical carrier. Examples of such unit dosage forms are tablets (including scored or coated tablets), capsules, pills, powder packets, wafers, suppositories, injectable solutions or suspensions and the like, and segregated multiples thereof. Those of skill in the treatment of infectious diseases will be able to determine the effective amount from the test results presented hereinafter. In general it is contemplated that an effective daily amount would be from 0.01 mg/kg to 50 mg/kg body weight, more preferably from 0.1 mg/kg to 10 mg/kg body weight. It may be appropriate to administer the required dose as two, three, four or more sub-doses at appropriate intervals throughout the day. Said sub-doses may be formulated as unit dosage forms, for example, containing 1 to 1000 mg, and in particular 5 to 200 mg of active ingredient per unit dosage form.
The exact dosage and frequency of administration depends on the particular compound of formula (I) used, the particular condition being treated, the severity of the condition being treated, the age, weight and general physical condition of the particular patient as well as other medication the individual may be taking, as is well known to those skilled in the art. Furthermore, it is evident that the effective amount may be lowered or increased depending on the response of the treated subject and/or depending on the evaluation of the physician prescribing the compounds of the instant invention. The effective amount ranges mentioned above are therefore only guidelines and are not intended to limit the scope or use of the invention to any extent.
EXPERIMENTAL SECTION
Preparation of Compound 1
Into a 50 mL vial equipped with a magnetic stir bar was placed 2,4-dichloro-5-methoxypyrimidine (2.0 g, 11.7 mmol), and acetonitrile (20 mL), diisopropylethylamine (3.02 g, 23.4 mmol) and (S)-3-aminoheptanol (4.59 g, 35.1 mmol). The reaction mixture was allowed to stir 15 hours at room temperature. The solvents were removed under reduced pressure. The crude was purified via silica gel column chromatography using a dichloromethane to 10% methanol in dichloromethane gradient. The best fractions were pooled and the solvents were removed under reduced pressure to afford a white solid, B.
To a thick wall glass vial equipped with a magnetic stir bar was added B (1 g, 3.66 mmol), NH 3 (10 mL, aq.), ammonium bicarbonate (3.34 g, 42.3 mmol) and copper(I) oxide (121 mg, 0.85 mmol). The vial was sealed and placed into an oil bath and heated to 150° C. for 15 hours. The reaction mixture was extracted with dichloromethane (3×25 mL), the organic layers were pooled and dried over magnesium sulfate. The solids were removed by filtration and the solvents of the filtrate were removed under reduced pressure. Crude C was purified via HPLC.
C (463 mg, 1.82 mmol) was dissolved in THF (13 mL) and cooled to −78° C. NaH (145 mg, 3.64 mmol, a 60% dispersion in mineral oil) was added in one portion and stirred at −78° C. for 30 minutes. Isobutyryl chloride (389 μL, 3.64 mmol) was added dropwise at −78° C. and stirred for 10 minutes. The cooling bath was removed and the mixture was allowed to reach room temperature. The mixture was stirred at room temperature for 30 minutes. The mixture was quenched with water and concentrated in vacuo. The residue was purified by HPLC (RP Vydac Denali C18 10 μm, 200 g, 5 cm, mobile phase 0.25% NH 4 HCO 3 solution in water, acetonitrile), the desired fractions were collected, and the solvents were removed under reduced pressure to afford the pure product.
LC-MS m/z=395 (M+H), Retention time 1.1 minutes, LC method A.
1 H NMR (400 MHz, DMSO-d 6 ) δ ppm 0.83 (t, J=6.90 Hz, 3H) 0.98-1.07 (m, 12H) 1.16-1.35 (m, 4H) 1.44-1.62 (m, 2H) 1.84 (q, J=6.78 Hz, 2H) 2.45 (spt, J=7.00 Hz, 1H) 2.96 (br. s., 1H) 3.80 (s, 3H) 3.92-4.07 (m, 2H) 4.18-4.31 (m, 1H) 6.69 (d, J=9.03 Hz, 1H) 7.60 (s, 1H) 9.49 (s, 1H).
Synthetic Scheme for the Preparation of A
Preparation of A2
To a solution of valeraldehyde (43 g, 500 mmol) in THF (1 L) was added A1 (200 g, 532 mmol) and the reaction mixture was stirred for 16 hours at room temperature. The solvents were evaporated and the residue was diluted in petroleum ether and filtered. The solvents of the filtrate were removed under reduced pressure and the residue was purified by silica chromatography using a petroleum ether to 3% ethyl acetate in petroleum ether gradient to give A2 (90 g) as a colorless oil.
1 H NMR (400 MHz, CDCl 3 ): δ ppm 6.81-6.77 (m, 1H), 5.68-5.64 (td, J=1.2 Hz, 15.6 Hz, 1H), 2.11-2.09 (m, 2H), 1.41 (s, 9H), 1.38-1.26 (m, 4H), 0.85-0.81 (t, J=7.2 Hz, 3H).
Preparation of Compound A4
n-butyl lithium (290 mL, 725 mmol) was added to a stirred solution of A3 (165 g, 781 mmol) in THF (800 mL) at −78° C. The reaction mixture was stirred for 30 minutes then A2 (90 g, 488.4 mmol) in THE (400 mL) was added and the reaction was stirred for 2 hours at −78° C. The mixture was quenched with sat., aq. NH 4 Cl solution and warmed to room temperature. The product was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried and evaporated. The residue was purified by column chromatography eluting with 5% ethyl acetate in petroleum ether to afford a colorless oil, A4 (132 g).
1 H NMR (400 MHz, CDCl 3 ): δ ppm 7.36-7.16 (m, 10H), 3.75-3.70 (m, 2H), 3.43-3.39 (d, J=15.2 Hz, 1H), 3.33-3.15 (m, 1H), 1.86-1.80 (m, 2H), 1.47-1.37 (m, 2H), 1.32 (s, 9H), 1.26-1.17 (m, 7H), 0.83-0.79 (t, J=7.2 Hz, 3H).
Preparation of A5
A4 (130 g, 328 mmol) was dissolved in THF (1.5 L) and LAH (20 g, 526 mmol) was added at 0° C. in small portions. The resulting mixture was stirred at the same temperature for 2 hours and then allowed to warm to room temperature. The mixture was quenched with a sat. aq. NH 4 Cl solution. The product was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried and evaporated. The combined organic layers were dried over sodium sulfate, the solids were removed via filtration and concentrated to afford crude A5 (100 g), which was used in the next step without further purification.
1 H NMR (400 MHz, CDCl 3 ): δ ppm 7.33-7.14 (m, 10H), 3.91-3.86 (m, 1H), 3.80-3.77 (d, J=13.6 Hz, 1H), 3.63-3.60 (d, J=13.6 Hz, 1H), 3.43-3.42 (m, 1H), 3.15-3.10 (m, 1H), 2.70-2.63 (m, 2H), 1.65-1.28 (m, 10H), 0.89-0.81 (m, 3H).
Preparation of A
A solution of A5 (38 g, 116.75 mmol) and 10% Pd/C in methanol (200 mL) was hydrogenated under 50 PSI hydrogen at 50° C. for 24 hours. The reaction mixture was filtered and the solvent was evaporated to give A.
1 H NMR (400 MHz, DMSO-d 6 ): δ ppm 8.04 (s, 3H), 3.60-3.49 (m, 2H), 3.16-3.15 (m, 1H), 1.71-1.67 (m, 2H), 1.60-1.55 (m, 2H), 1.33-1.26 (m, 4H), 0.90-0.87 (t, J=6.8 Hz, 3H).
Analytical Method.
Compounds 1-8 in the table below were characterized by LC-MS according to the following LC-MS method.
Reverse phase UPLC (Ultra Performance Liquid Chromatography) was carried out on a bridged ethylsiloxane/silica hybrid (BEH) C18 column (1.7 μm, 2.1×50 mm; Waters Acquity) with a flow rate of 0.8 ml/min. Two mobile phases (10 mM ammonium acetate in H 2 O/acetonitrile 95/5; mobile phase B: acetonitrile) were used to run a gradient condition from 95% A and 5% B to 5% A and 95% B in 1.3 minutes and hold for 0.7 minutes. An injection volume of 0.75 μL was used. Cone voltage was 30 V for positive ionization mode and 30 V for negative ionization mode.
LC-MS Mass Ret Exact Found Time STRUCTURE Mass [M + H] (min) 1 394.5 395 1.1 2 324.2 325 0.83 3 358.2 359 0.88 4 372.2 373 0.94 5 314.2 315 1.2 6 373.2 374 0.7 7 419.2 420 0.73 8 358.2 359 0.89
Production of IFN-α and Up-Regulation of CXCL10 mRNA In Vivo
The potential of compounds to induce IFN-α production and CXCL10 mRNA up-regulation in vivo was evaluated after oral administration to C57BL/6 mice. The quantity of IFN-α in systemic circulation was followed over time, using a murine pan-IFN-α ELISA (PBL InterferonSource, ref. 42120). This ELISA recognizes all murine IFN-α subtypes. CXCL10 is an interferon-stimulated gene (ISG) whose expression is highly induced upon binding of IFN-I to the receptor IFNAR (interferon alpha receptor). CXCL10 mRNA expression levels were followed by RT-qPCR.
For each compound and dose tested, 3 female C57BL/6J mice, from 6-10 weeks of age, 20-22 g of body weight were tested. Animals were given compound 1 as a single oral dose of 15.5 mg/kg as a 1.55 mg/mL solution in 20% aqueous hydroxypropyl β-cyclodextrin vehicle using a feeding tube. 0.5, 1, 2, 4 and 7 hours after dosing, systemic blood was drawn from the tail vein into K-EDTA containing tubes. Plasma was separated from blood cells by centrifugation at 1500 g, 10 min, 4° C. and stored at −80° C. prior to ELISA analysis. At each time point, the median and standard deviation over the 3 animals was calculated to evaluate the potency of the compound.
Blood was also drawn from the tail vein into micronic tubes containing 500 μl of PAXgene solution (PAXgene blood RNA tubes from PreAnalytix). After overnight incubation at room temperature, the tubes were stored at −20° C. before total RNA extraction with the PAXgene 96 Blood RNA kit (PreAnalytix). Purified RNA was reverse transcribed using random 6-mer primers (High-Capacity cDNA Archive kit, Applied Biosystems). CXCL10 mRNA levels were by Taqman qPCR technology (Taqman universal PCR master mix, no UNG AmpErase and Taqman Gene Expression assay Mm00445235_m1 from Applied Biosystems) on a 7900HT Fast Real-time PCR system (Applied Biosystems). HPRT1 (hypoxanthine phosphoribosyltransferase 1) mRNA levels were used as endogenous control (Mm01545399_m1). The ΔΔCt method (for relative quantification) was used to evaluate regulation of CXCL10 expression by the compound compared to the vehicle control. At each time point, the median and standard deviation over the 3 animals was calculated to evaluate the potency of the compounds.
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This invention relates to acylaminopyrimidine derivatives, processes for their preparation, pharmaceutical compositions, and their use in therapy.
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This application is the national phase of PCT/US 93/04063, filed May 5, 1993.
BACKGROUND OF THE INVENTION
The present invention relates to novel substituted benzylamino nitrogen containing non-aromatic heterocycles, pharmaceutical compositions comprising such compounds and the use of such compounds in the treatment and prevention of inflammatory and central nervous system disorders, as well as several other disorders. The pharmaceutically active compounds of this invention are substance P receptor antagonists. This invention also relates to novel intermediates used in the synthesis of such substance P receptor antagonists.
Substance P is a naturally occurring undecapeptide belonging to the tachykinin family of peptides, the latter being named because of their prompt stimulatory action on smooth muscle tissue. More specifically, substance P is a pharmacologically active neuropeptide that is produced in mammals and possesses a characteristic amino acid sequence that is illustrated by D. F. Veber et al. in U.S. Pat. No. 4,680,283. The wide involvement of substance P and other tachykinins in the pathophysiology of numerous diseases has been amply demonstrated in the art. For instance, substance P has been shown to be involved in the transmission of pain or migraine (see B. E. B. Sandberg et al., Journal of Medicinal Chemistry, 25, 1009 (1982)), as well as in central nervous system disorders such as anxiety and schizophrenia, in respiratory and inflammatory diseases such as asthma and rheumatoid arthritis, respectively, in rheumatic diseases such as fibrositis, and in gastrointestinal disorders and diseases of the GI tract such as ulcerative colitis and Crohn's disease, etc. (see D. Regoli in "Trends in Cluster Headache," edited by F. Sicuteri et al., Elsevier Scientific Publishers, Amsterdam, pp. 85-95 (1987)).
Quinuclidine, piperidine, and azanorbornane derivatives and related compounds that exhibit activity as substance P receptor antagonists are referred to in U.S. patent application Ser. No. 566,338 filed Nov. 20, 1989, U.S. patent application Ser. No. 724,268, filed Jul. 1, 1991, PCT patent application PCT/US 91/02853, filed Apr. 25, 1991, PCT patent application PCT/US 91/03369, filed May 14, 1991, PCT patent application PCT/US 91/05776, filed Aug. 20, 1991, PCT patent application PCT/US 92/00113, filed Jan. 17, 1992, PCT patent application PCT/US 92/03571, filed May 5, 1992, PCT patent application PCT/US 92/03317, filed Apr. 28, 1992, PCT patent application PCT/US 92/04697, filed Jun. 11, 1992, U.S. patent application 766,488, filed Sep. 26, 1991, U.S. patent application 790,934, filed Nov. 12, 1991, PCT patent application PCT/US 92/04002, filed May 19, 1992, and Japanese Patent Application No. 065337/92, filed Mar. 23, 1992.
SUMMARY OF THE INVENTION
The present invention relates to compounds of the formula ##STR2## wherein ring A is an aryl group selected from phenyl, naphthyl, thienyl, dihydroquinolinyl and indolinyl, and wherein the side chain containing NR 2 R 3 is attached to a carbon atom of ring A;
W is hydrogen, (C 1 -C 6 )alkyl, S--(C 1 -C 3 )alkyl, halo or (C 1 -C 6 )alkoxy optionally substituted with from one to three fluorine atoms;
R 1 is selected from amino, (C 1 -C 6 )alkylamino, di-(C 1 -C 6 )alkylamino, --S(O) v --(C 1 -C 10 )-alkyl wherein v is zero, one or two, --S(O) v -aryl wherein v is zero, one or two, --O-aryl, --SO 2 NR 4 R 5 wherein each of R 4 and R 5 is, independently, (C 1 -C 6 )alkyl, or R 4 and R 5 , together with the nitrogen to which they are attached, form a saturated ring containing one nitrogen and from 3 to 6 carbons, ##STR3## wherein one or both of the alkyl moieties may optionally be substituted with from one to three fluorine atoms, --N(SO 2 --(C 1 -C 10 )alkyl) 2 and ##STR4## and wherein the aryl moieties of said --S(O) v -aryl, --O-aryl and ##STR5## are independently selected from phenyl and benzyl and may optionally be substituted with from one to three substituents independently selected from (C 1 -C 4 )alkyl, (C 1 -C 4 )alkoxy and halo;
or R 1 is a group having the formula ##STR6## wherein a is 0, 1 or 2 and the asterisk represents a position meta to the R 2 R 3 NCH 2 side chain;
R 2 is hydrogen or --CO 2 (C 1 -C 10 )alkyl;
R 3 is selected from ##STR7## wherein R 6 and R 10 are independently selected from furyl, thienyl, pyridyl, indolyl, biphenyl and phenyl, wherein said phenyl may optionally be substituted with one or two substituents independently selected from halo, (C 1 -C 10 ) alkyl optionally substituted with from one to three fluorine atoms, (C 1 -C 10 ) alkoxy optionally substituted with from one to three fluorine atoms, carboxy, benzyloxycarbonyl and (C 1 -C 3 ) alkoxy-carbonyl;
R 7 is selected from (C 3 -C 4 ) branched alkyl, (C 5 -C 6 ) branched alkenyl, (C 5 -C 7 ) cycloalkyl, and the radicals named in the definition of R 6 ;
R 8 is hydrogen or (C 1 -C 6 ) alkyl;
R 9 and R 19 are independently selected from phenyl, biphenyl, naphthyl, pyridyl, benzhydryl, thienyl or furyl, and R 9 and R 19 may optionally be substituted with from one to three substituents independently selected from halo, (C 1 -C 10 ) alkyl optionally substituted with from one to three fluorine atoms and (C 1 -C 10 ) alkoxy optionally substituted with from one to three fluorine atoms;
Y is (CH 2 ) 1 wherein 1 is an integer from one to three, or Y is a group of the formula ##STR8## Z is oxygen, sulfur, amino, (C 1 -C 3 )alkylamino or (CH 2 ) n wherein n is zero, one or two;
x is zero, one or two;
y is zero, one or two;
z is three, four or five;
o is two or three;
p is zero or one;
r is one, two or three;
the ring containing (CH 2 ) z may contain from zero to three double bonds, and one of the carbon atoms of (CH 2 ) z may optionally be replaced by oxygen, sulfur or nitrogen;
R 11 is thienyl, biphenyl or phenyl optionally substituted with one or two substituents independently selected from halo, (C 1 -C 10 ) alkyl optionally substituted with from one to three fluorine atoms and (C 1 -C 10 ) alkoxy optionally substituted with from one to three fluorine atoms;
X is (CH 2 ) q wherein q is an integer from 1 to 6, and wherein any one of the carbon-carbon single bonds in said (CH 2 ) q may optionally be replaced by a carbon-carbon double bond, and wherein any one of the carbon atoms of said (CH 2 ) q may optionally be substituted with R 14 , and wherein any one of the carbon atoms of said (CH 2 ) q may optionally be substituted with R 15 ;
m is an integer from 0 to 8, and any one of the carbon-carbon single bonds of (CH 2 ) m , wherein both carbon atoms of such bond are bonded to each other and to another carbon atom of the (CH 2 ) m chain, may optionally be replaced by a carbon-carbon double bond or a carbon-carbon triple bond, and any one of the carbon atoms of said (CH 2 ) m may optionally be substituted with R 17 ;
R 12 is a radical selected from hydrogen, (C 1 -C 6 ) straight or branched alkyl, (C 3 -C 7 ) cycloalkyl wherein one of the carbon atoms may optionally be replaced by nitrogen, oxygen or sulfur; aryl selected from biphenyl, phenyl, indanyl and naphthyl; heteroaryl selected from thienyl, furyl, pyridyl, thiazolyl, isothiazolyl, oxazolyl, isoxazolyl, triazolyl, tetrazolyl and quinolyl; phenyl-(C 2 -C 6 ) alkyl, benzhydryl and benzyl, wherein the point of attachment on R 12 is a carbon atom unless R 12 is hydrogen, and wherein each of said aryl and heteroaryl groups and the phenyl moieties of said benzyl, phenyl-(C 2 -C 6 ) alkyl and benzhydryl may optionally be substituted with one or more substituents independently selected from halo, nitro, (C 1 -C 10 ) alkyl optionally substituted with from one to three fluorine atoms, (C 1 -C 10 ) alkoxy optionally substituted with from one to three fluorine atoms, amino, hydroxy-(C 1 -C 6 )alkyl, (C 1 -C 6 )alkoxy-(C 1 -C 6 )alkyl, (C 1 -C 6 )-alkylamino, ##STR9## and wherein one of the phenyl moieties of said benzhydryl may optionally be replaced by naphthyl, thienyl, furyl or pyridyl;
R 13 is hydrogen, phenyl or (C 1 -C 6 )alkyl;
or R 12 and R 13 , together with the carbon to which they are attached, form a saturated carbocyclic ring having from 3 to 7 carbon atoms wherein one of said carbon atoms that is neither the point of attachment of the spiro ring nor adjacent to such point of attachment may optionally be replaced by oxygen, nitrogen or sulfur;
R 14 and R 15 are each independently selected from hydrogen, hydroxy, halo, amino, oxo (═O), cyano, hydroxy-(C 1 -C 6 )alkyl, (C 1 -C 6 )alkoxy-(C 1 -C 6 )alkyl, (C 1 -C 6 )alkylamino, ##STR10## and the radicals set forth in the definition of R 12 ; ##STR11## NHCH 2 R 18 , SO 2 R 18 , CO 2 H or one of the radicals set forth in any of the definitions of R 12 , R 14 and R 15 ;
R 17 is oximino (═NOH) or one of the radicals set forth in any of the definitions of R 12 , R 14 and R 15 ; and
R 18 is (C 1 -C 6 )alkyl, hydrogen, phenyl or phenyl (C 1 -C 6 )alkyl;
with the proviso that (a) when m is 0, one of R 16 and R 17 is absent and the other is hydrogen, (b) when R 3 is a group of the formula VIII, R 14 and R 15 cannot be attached to the same carbon atom, (c) when R 14 and R 15 are attached to the same carbon atom, then either each of R 14 and R 15 is independently selected from hydrogen, fluoro, (C 1 -C 6 )alkyl, hydroxy-(C 1 -C 6 )alkyl and (C 1 -C 6 )alkoxy-(C 1 -C 6 )alkyl, or R 14 and R 15 , together with the carbon to which they are attached, form a (C 3 -C 6 ) saturated carbocyclic ring that forms a spiro compound with the nitrogen-containing ring to which they are attached; (d) when R 1 is amino, (C 1 -C 6 )alkylamino, di-(C 1 -C 6 )alkylamino or ##STR12## R 3 is a group of the formula II, III, IV, V or VI, and (e) when R 14 or R 15 is attached to a carbon atom of X or (CH 2 ) y that is adjacent to the ring nitrogen, then R 14 or R 15 , respectively, must be a substituent wherein the point of attachment is a carbon atom.
The present invention also relates to the pharmaceutically acceptable acid addition and base salts of compounds of the formula I. The acids which are used to prepare the pharmaceutically acceptable acid addition salts of the aforementioned base compounds of this invention are those which form non-toxic acid addition salts, i.e., salts containing pharmacologically acceptable anions, such as the hydrochloride, hydrobromide, hydroiodide, nitrate, sulfate, bisulfate, phosphate, acid phosphate, acetate, lactate, citrate, acid citrate, tartrate, bitartrate, succinate, maleate, fumarate, gluconate, saccharate, benzoate, methanesulfonate, ethanesulfonate, benzenesulfonate, p-toluenesulfonate and pamoate i.e., 1,1'-methylene-bis-(2-hydroxy-3-naphthoate)!salts. The chemical bases which are used as reagents to prepare the pharmaceutically acceptable base salts of this invention are those which form non-toxic base salts with the acidic compounds of formula I. Such non-toxic base salts include those derived from such pharmacologically acceptable cations as sodium, potassium calcium and magnesium, etc.
The term "halo", as used herein, unless otherwise indicated, includes chloro, fluoro, bromo and iodo.
The term "alkyl", as used herein, unless otherwise indicated, includes saturated monovalent hydrocarbon radicals having straight, branched or cyclic moieties or combinations thereof.
The term "alkoxy", as used herein, includes O-alkyl groups wherein "alkyl" is defined as above.
The term "one or more substituents," as used herein, includes from one to the maximum number of substituents possible based on the number of available bonding sites.
Preferred compounds of the formula I include those wherein the substituents at positions "2" and "3" of the nitrogen containing ring of R 3 are in a cis configuration. When R 3 is a group of the formula VII or VIII, "a cis configuration," as used herein, means that the non-hydrogen substituent at position "3" is cis to R 12 .
Other preferred compounds of the formula I are those wherein R 3 is a group of the formula II, III, VII or IX; R 2 is hydrogen; ring A is phenyl or indolinyl; W is (C 1 -C 3 )alkoxy optionally substituted with from one to five fluorine atoms; and R 1 is S(O) v --(C 1 -C 10 )alkyl wherein v is zero, one or two, S(O) v -aryl wherein v is zero, one or two, O-aryl, ##STR13## wherein one or both of the alkyl moieties may optionally be substituted with from one to three fluorine atoms, --N(SO 2 -(C 1 -C 10 )alkyl) 2 or ##STR14## wherein said aryl is phenyl or benzyl and may optionally be substituted with from one to three substituents independently selected from (C 1 -C 4 )alkyl, (C 1 -C 4 )alkoxy and halo.
More preferred compounds of the formula I are the foregoing preferred compounds wherein: (a) R 3 is a group of the formula III and R 9 is benzhydryl; (b) R 3 is a group of the formula VII, each of R 13 , R 14 , R 15 and R 16 is hydrogen, m is zero and X is --(CH 2 ) 3 --; or (c) R 3 is a group of the formula IX, r is two and R 19 is benzhydryl.
Other more preferred compounds of the formula I are those wherein: (a) R 3 is a group of the formula III wherein the substituents at positions "2" and "3" of the nitrogen containing ring are in the cis configuration, R 9 is benzhydryl and ring A is phenyl; (b) R 3 is a group of the formula VII wherein R 12 and the substituent at position "3" of the nitrogen containing ring are in the cis configuration, ring A is phenyl, R 12 is phenyl, each of R 2 , R 13 , R 14 , R 15 and R 16 is hydrogen, m is zero, W is methoxy or isopropoxy, X is --(CH 2 ) 3 -- and R 1 is S(O) v --(C 1 -C 10 )alkyl wherein v is zero, one or two, or ##STR15## or (c) R 3 is a group of the formula IX wherein the substituents at positions "2" and "3" of the nitrogen containing ring are in the cis configuration, R 19 is benzhydryl, r is two and ring A is phenyl.
Especially preferred compounds of the formula I are those wherein R 3 is a group of the formula III, R 9 is benzhydryl, ring A is phenyl, W is selected from OCF 3 , isopropoxy, OCH 3 , OCHF 2 and OCH 2 CF 3 , and R 1 is selected from amino, (C 1 -C 6 )alkylamino, di-(C 1 -C 6 )alkylamino, and --S(O) v --(C 1 -C 10 )alkyl wherein v is zero, one or two.
Other especially preferred compounds of this invention are those wherein R 3 is a group of the formula VII, each of R 13 , R 14 , R 15 and R 16 is hydrogen, m is zero, X is --(CH 2 ) 3 --, ring A is phenyl, W is selected from OCF 3 , OCH 3 , isopropoxy, OCHF 2 and OCH 2 CF 3 , and R 1 is selected from --S(O) v --(C 1 -C 10 )alkyl wherein v is zero, one or two, and ##STR16##
Specific preferred compounds of the formula I include the following:
(2S,3S)-3- 2-methoxy-5-(N-acetyl-N-methylamino)benzylamino!-2-diphenylmethyl-1-azabicyclo 2.2.2!octane;
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(N-methyl-N-trifluoromethane-sulfonylamino)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane;
(1SR,2SR,3SR,4RS)-3- 2-methoxy-5-(N-thiazolidine-S,S-dioxide)benzyl!amino-2-benzhydryl- 2.2.1!-1-azanorbornane;
(1SR,2SR,3SR,4RS)-3- (2,3-dihydro-5-methoxy-1-methanesulfonyl-6-indolyl)methylamino!-2-benzhydryl- 2.2.1!-1-azanorbornane;
(2S,3S)-3-(2-methoxy-5-methylthiobenzyl)amino-2-phenylpiperidine;
(2S,3S)-3-(2-methoxy-5-methylsulfonylbenzyl)amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-methyl-N-methanesulfonylamino)-benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-trifluoromethoxy-5-(N-methyl-N-methane-sulfonylamino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-isopropoxy-5-(N-methyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-isopropyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-isopropoxy-5-(N-isopropyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-isopropoxy-5-(N-isopropyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-cyclopentyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-methyl-N-trifluoromethane-sulfonylamino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-isopropoxy-5-(N-methyl-N-trifluoromethane-sulfonylamino)benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-methyl-N-isopropylsulfonylamino)-benzyl!amino-2-phenylpiperidine;
(2S,3S)-3- 2-methoxy-5-(N-thiazolidine-S,S-dioxide)-benzyl!amino-2-phenyl-piperidine;
(2S,3S)-3- (2,3-dihydro-5-methoxy-1-methanesulfonyl-6-indolyl)methylamino!-2-phenylpiperidine;
(2S,3S)-3- (2,3-dihydro-5-methoxy-2-methyl-1-methane-sulfonyl-6-indolyl)methylamino!-2-phenylpiperidine;
(2SR,3SR,4RS)-2-benzhydryl-4-(2-hydroxyethyl)-3-(2-methoxy-5-methylthiobenzyl)aminopyrrolidine;
(2SR,3SR,4RS)-2-benzhydryl-4-(2-hydroxyethyl)-3-(2-methoxy-5-(N-methyl-N-methanesulfonylamino)benzyl)aminopyrrolidine;
(2SR,3SR,4RS)-2-benzhydryl-4-(2-hydroxyethyl)-3-(2-methoxy-5-(N,thiazolidine-S,S-dioxide)benzyl)aminopyrrolidine;
(2S,3S)-N-(2-methoxy-5-methylthiophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine;
(2S,3S)-N-(2-methoxy-5-dimethylaminophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine;
(2S,3S)-N-(5-ethylthio-2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine;
(2S,3S)-N-(5-trifluoroacetylamino-2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine;
(2S,3S)-N-(5-amino-2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine;
(2S,3S)-N-(2-methoxy-5-methylsulfinylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine; and
(2S,3S)-N-(2-methoxy-5-methylsulfonylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine.
Other compounds of the formula I include:
4-(2-methylthiophenyl)methylamino-3-phenyl-2-azabicyclo 3.3.0!octane;
4-benzhydryl-5-(2-methylthiophenyl)methylamino-3-azabicyclo 4.1.0!heptane;
4-(2-methylthiophenyl)methylamino-3-phenyl-2-azabicyclo 4.4.0!decane;
8-benzhydryl-7-(2-methylthio-5-trifluoromethoxyphenyl)methylamino-9-azatricyclo 4.3.1.0 4 ,9 !decane;
9-benzhydryl-8-(2-methylthio-5-trifluoromethoxyphenyl)methylamino-10-azatricyclo 4.4.1.0 5 ,10 !undecane;
9-benzhydryl-8-(2-methylthio-5-trifluoromethoxyphenyl)methylamino-3-thia-10-azatricyclo 4.4.1.0 5 ,10 !undecane;
2-benzhydryl-3-(2-methylthiophenyl)methylamino-5,6-pentamethylene-quinuclidine;
2-benzhydryl-3-(2-methylthiophenyl)methylamino-5,6-trimethylene-quinuclidine;
cis-3-(2-phenoxyphenyl)methylamino-2-benzhydrylquinuclidine;
8-benzhydryl-9-(2-methylthiophenyl)methylamino-7-azatricyclo 4.4.1.0 5 ,10 !undecane;
2-benzhydryl-3-(2-methylthiophenyl)methylamino-1-azabicyclo 3.2.2!nonane;
2-benzhydryl-3-(2-methylthiophenyl)methylamino-1-azabicyclo 2.2.1!heptane;
3-(2-methylthiophenyl)methylamino-2-phenyl-1-azabicyclo 2.2.1!heptane;
N- 3-(4-benzhydryl-1-azabicyclo 2.2.1!hept-3-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-isopropylsulfonamide;
N- 3-(7-benzhydryl-1-azabicyclo 3.2.2!non-6-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(7-benzhydryl-1-azabicyclo 3.2.2!non-6-ylaminomethyl)-4-trifluoromethoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(8-benzhydryl-1-azabicyclo 4.2.2!dec-7-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(8-benzhydryl-1-azabicyclo 4.2.2!dec-7-ylaminomethyl)-4-trifluoromethoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(4-benzhydryl-1-azabicyclo 2.2.1!hept-3-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(4-benzhydryl-1-azabicyclo 2.2.1!hept-3-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-trifluoromethanesulfonamide;
N- 3-(4-benzhydryl-1-azabicyclo 2.2.1!hept-3-ylaminomethyl)-4-methoxyphenyl!-isopropylsulfone;
N- 3-(4-benzhydryl-1-azabicyclo 2.2.1!hept-3-ylaminomethyl)-4-methoxyphenyl!-methylsulfone;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-isopropoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-trifluoromethoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-methoxyphenyl!-N-methyl-trifluoromethanesulfonamide;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-methoxyphenyl!-methanesulfone;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-trifluoromethoxyphenyl!-methanesulfone;
N- 3-(2-benzhydryl-1-azabicyclo 2.2.2!oct-3-ylaminomethyl)-4-methoxyphenyl!-isopropylsulfone;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-isopropoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-trifluoromethoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(10-benzhydryl-octahydro-1,4-ethano-quinolin-9-ylaminomethyl)-4-isopropoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-methoxyphenyl!-methanesulfone;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-trifluoromethoxyphenyl!-methanesulfone;
N- 3-(9-benzhydryl-1-azatricyclo 5.2.2.0 2 ,6 !undec-8-ylaminomethyl)-4-methoxyphenyl!-isopropylsulfone;
N- 3-(9-benzhydryl-8-azatricyclo 5.3.1.0 3 ,8 !undec-10-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(10-benzhydryl-9-azatricyclo 6.3.1.0 3 ,9 !dodec-11-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(9-benzhydryl-8-azatricyclo 5.3.1.0 3 ,8 !undec-10-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(10-benzhydryl-9-azatricyclo 6.3.1.0 3 ,9 !dodec-11-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(10-benzhydryl-9-azatricyclo 6.3.1.0 3 ,9 !dodec-11-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(11-benzhydryl-1-azatricyclo 6.3.1.0 3 ,9 !dodec-10-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(11-benzhydryl-1-azatricyclo 6.3.1.0 3 ,9 !dodec-10-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(11-benzhydryl-1-azatricyclo 6.3.1.0 3 ,9 !dodec-10-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(11-benzhydryl-1-azatricyclo 6.3.1.0 3 ,9 !dodec-10-ylaminomethyl)-4-methoxyphenyl!-N-methyl-trifluoromethanesulfonamide;
N- 3-(3-benzhydryl-octahydro-2,5-methano-isoquinolin-4-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(3-benzhydryl-octahydro-2,5-methano-isoquinolin-4-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
(2-trifluoromethoxy-5-methylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
(2-difluoromethoxy-5-methylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
(2-cyclopropoxy-5-methylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
(2-cyclopentyloxy-5-methylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
(2-isopropoxy-5-methylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
(2-methoxy-5-isopropylsulfonylbenzyl)-(2-phenylpiperidin-3-yl)-amine;
N- 4-methoxy-3-(3-phenyl-decahydro-isoquinolin-4-ylaminomethyl)-phenyl!-N-methyl-methanesulfonamide;
N- 4-trifluoromethoxy-3-(3-phenyl-decahydroisoquinolin-4-ylaminomethyl)-phenyl!-N-methyl-methanesulfonamide;
N- 4-methoxy-3-(3-phenyl-decahydro-isoquinolin-4-ylaminomethyl)-phenyl!-N-isopropyl-methanesulfonamide;
N- 4-methoxy-3-(2-phenyl-decahydro-quinolin-3-ylaminomethyl)-phenyl!-N-methyl-methanesulfonamide;
N- 4-methoxy-3-(2-phenyl-decahydro-quinolin-3-ylaminomethyl)-phenyl!-N-isopropyl-methanesulfonamide;
N- 4-methoxy-3-(2-phenyl-decahydro-quinolin-3-ylaminomethyl)-phenyl!-N-methyl-isopropylsulfonamide;
N- 4-methoxy-3-(2-phenyl-octahydro- 1!pyrindin-3-ylaminomethyl)-phenyl!-N-methyl-methanesulfonamide;
N- 4-methoxy-3-(2-phenyl-octahydro- 1!pyrindin-3-ylaminomethyl)-phenyl!-N-isopropyl-methanesulfonamide;
N- 4-methoxy-3-(2-phenyl-octahydro- 1!pyrindin-3-ylaminomethyl)-phenyl!-N-methyl-trifluoromethanesulfonamide;
N- 4-methoxy-3-(2-phenyl-decahydro-cyclohepta- b!pyridin-3-ylaminomethyl)-phenyl!-N-methyl-methanesulfonate;
N- 4-methoxy-3-(2-phenyl-octahydro-indol-3-ylaminomethyl)-phenyl!-N-methyl-methanesulfonate;
N- -3-(2-benzhydryl-decahydro-cyclohepta b!pyridin-3-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonate;
N- 3-(7-benzhydryl-1-aza-bicyclo 3.2.1!oct-6-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(7-benzhydryl-1-aza-bicyclo 3.2.1!oct-6-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(7-benzhydryl-1-aza-bicyclo 3.2.1!oct-6-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(7-benzhydryl-1-aza-bicyclo 3.2.1!oct-6-ylaminomethyl)-4-methoxyphenyl!-N-methyl-trifluoromethane-sulfonamide;
N- 3-(8-benzhydryl-1-aza-bicyclo 4.2.1!non-7-ylaminomethyl)-4-methoxyphenyl!-N-methyl-methanesulfonamide;
N- 3-(8-benzhydryl-1-aza-bicyclo 4.2.1!non-7-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-aza-bicyclo 5.2.1!dec-8-ylaminomethyl)-4-methoxyphenyl!-N-isopropyl-methanesulfonamide;
N- 3-(9-benzhydryl-1-aza-bicyclo 5.2.1!dec-8-ylaminomethyl)-4-methoxyphenyl!-N-methyl-isopropylsulfonamide;
N- 3-(9-benzhydryl-1-aza-bicyclo 5.2.1!dec-8-ylaminomethyl)-4-methoxyphenyl!-methanesulfone; and
N- 3-(9-benzhydryl-1-aza-bicyclo 5.2.1!dec-8-ylaminomethyl)-4-trifluoromethoxyphenyl!-methanesulfone.
The present invention also relates to compounds of the formulae ##STR17## wherein ring A, R 1 , R 3 and W are defined as above. These compounds are intermediate in the synthesis of compounds of the formula I.
The present invention also relates to a pharmaceutical composition for treating or preventing a condition selected from the group consisting of inflammatory diseases (e.g., arthritis, psoriasis, asthma and inflammatory bowel disease), anxiety, depression or dysthymic disorders, colitis, psychosis, pain, allergies such as eczema and rhinitis, chronic obstructive airways disease, hypersensitivity disorders such as poison ivy, vasospastic diseases such as angina, migraine and Reynaud's disease, fibrosing and collagen diseases such as scleroderma and eosinophilic fascioliasis, reflex sympathetic dystrophy such as shoulder/hand syndrome, addiction disorders such as alcoholism, stress related somatic disorders, peripheral neuropathy, neuralgia, neuropathological disorders such as Alzheimer's disease, AIDS related dementia, diabetic neuropathy and multiple sclerosis, disorders related to immune enhancement or suppression such as systemic lupus erythematosus, and rheumatic diseases such as fibrositis in a mammal, including a human, comprising an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in treating or preventing such condition, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of treating or preventing a condition selected from the group consisting of inflammatory diseases (e.g., arthritis, psoriasis, asthma and inflammatory bowel disease), anxiety, depression or dysthymic disorders, colitis, psychosis, pain, allergies such as eczema and rhinitis, chronic obstructive airways disease, hypersensitivity disorders such as poison ivy, vasospastic diseases such as angina, migraine and Reynaud's disease, fibrosing and collagen diseases such as scleroderma and eosinophilic fascioliasis, reflex sympathetic dystrophy such as shoulder/hand syndrome, addiction disorders such as alcoholism, stress related somatic disorders, peripheral neuropathy, neuralgia, neuropathological disorders such as Alzheimer's disease, AIDS related dementia, diabetic neuropathy and multiple sclerosis, disorders related to immune enhancement or suppression such as systemic lupus erythematosus, and rheumatic diseases such as fibrositis in a mammal, including a human, comprising administering to said mammal an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in treating or preventing such condition.
The present invention also relates to a pharmaceutical composition for antagonizing the effects of substance P in a mammal, including a human, comprising a substance P antagonizing amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of antagonizing the effects of substance P in a mammal, including a human, comprising administering to said mammal a substance P antagonizing amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof.
The present invention also relates to a pharmaceutical composition for treating or preventing a disorder in a mammal, including a human, resulting from an excess of substance P, comprising a substance P antagonizing amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of treating or preventing a disorder in a mammal, including a human, resulting from an excess of substance P, comprising administering to said mammal a substance P antagonizing amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof.
The present invention also relates to a pharmaceutical composition for treating or preventing a condition selected from the group consisting of inflammatory diseases (e.g., arthritis, psoriasis, asthma and inflammatory bowel disease), anxiety, depression or dysthymic disorders, colitis, psychosis, pain, allergies such as eczema and rhinitis, chronic obstructive airways disease, hypersensitivity disorders such as poison ivy, vasospastic diseases such as angina, migraine and Reynaud's disease, fibrosing and collagen diseases such as scleroderma and eosinophilic fascioliasis, reflex sympathetic dystrophy such as shoulder/hand syndrome, addiction disorders such as alcoholism, stress related somatic disorders, peripheral neuropathy, neuralgia, neuropathological disorders such as Alzheimer's disease, AIDS related dementia, diabetic neuropathy and multiple sclerosis, disorders related to immune enhancement or suppression such as systemic lupus erythematosus, and rheumatic diseases such as fibrositis in a mammal, including a human, comprising an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in antagonizing the effect of substance P at its receptor site, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of treating or preventing a condition selected from the group consisting of inflammatory diseases (e.g., arthritis, psoriasis, asthma and inflammatory bowel disease), anxiety, depression or dysthymic disorders, colitis, psychosis, pain, allergies such as eczema and rhinitis, chronic obstructive airways disease, hypersensitivity disorders such as poison ivy, vasospastic diseases such as angina, migraine and Reynaud's disease, fibrosing and collagen diseases such as scleroderma and eosinophilic fascioliasis, reflex sympathetic dystrophy such as shoulder/hand syndrome, addiction disorders such as alcoholism, stress related somatic disorders, peripheral neuropathy, neuralgia, neuropathological disorders such as Alzheimer's disease, AIDS related dementia, diabetic neuropathy and multiple sclerosis, disorders related to immune enhancement or suppression such as systemic lupus erythematosus, and rheumatic diseases such as fibrositis in a mammal, including a human, comprising administering to said mammal an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in antagonizing the effect of substance P at its receptor site.
The present invention also relates to a pharmaceutical composition for treating or preventing a disorder in a mammal, including a human, the treatment or prevention of which is effected or facilitated by a decrease in substance P mediated neurotransmission, comprising an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in antagonizing the effect of substance P at its receptor site, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of treating or preventing a disorder in mammal, including a human, the treatment or prevention of which is effected or facilitated by a decrease in substance P mediated neurotransmission, comprising administering to said mammal an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in antagonizing the effect of substance P at its receptor site.
The present invention also relates to a pharmaceutical composition for treating or preventing a disorder in a mammal, including a human, the treatment or prevention of which is effected or facilitated by a decrease in substance P mediated neurotransmission, comprising an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in treating or preventing such disorder, and a pharmaceutically acceptable carrier.
The present invention also relates to a method of treating or preventing a disorder in mammal, including a human, the treatment or prevention of which is effected or facilitated by a decrease in substance P mediated neurotransmission, comprising administering to said mammal an amount of a compound of the formula I, or a pharmaceutically acceptable salt thereof, effective in treating or preventing such disorder.
The compounds of the formula I have chiral centers and therefore exist in different enantiomeric forms. This invention relates to all optical isomers and all stereoisomers of compounds of the formula I, and mixtures thereof.
DETAILED DESCRIPTION OF THE INVENTION
The compounds of the formula I may be prepared as described in the following reaction schemes and discussion. Unless otherwise indicated, ring A, W, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , R 15 , R 16 , R 17 , R 18 , R 19 , X, Z, Y, m, n, o, p, q, r, x, y, and z, and structural formulas I, II, III, IV, V, VI, VII, VIII, IX, XI and XII in the reaction schemes and discussion that follow are defined as above. ##STR18##
Scheme 1 illustrates the preparation of compounds of the formula I from starting materials of the formula X wherein G is hydrogen, hydroxy, chloro, bromo or (C 1 -C 6 )alkoxy.
Referring to scheme 1, a compound of the formula X wherein G is hydrogen may be converted directly into the corresponding compound of the formula I by reacting it with a compound of the formula NH 2 R 3 in the presence of a reducing agent. Reducing agents that may be used include sodium cyanoborohydride, sodium triacetoxyborohydride, sodium borohydride, hydrogen and a metal catalyst, zinc and hydrochloric acid, and formic acid. This reaction is typically conducted in a reaction inert solvent at a temperature from about 0° C. to about 150° C. Suitable reaction inert solvents include lower alcohols (e.g., methanol, ethanol and isopropanol), 1,2-dichloroethane, acetic acid and tetrahydrofuran (THF). Preferably, the solvent is acetic acid, the temperature is about 25° C., the reducing agent is sodium triacetoxyborohydride, and the reaction is conducted in the presence of a dehydrating agent such as molecular sieves.
Alternatively, the reaction of a compound of the formula X with a compound of the formula NH 2 R 3 may be carried out in the presence of a dehydrating agent or using an apparatus designed to remove azeotropically the water generated, to produce an imine of the formula ##STR19## which is then reacted with a reducing agent as described above, preferably with sodium triacetoxyborohydride in an acetic acid or 1,2-dichloroethane solvent at about room temperature. The preparation of the imine is generally carried out in a reaction inert solvent such as benzene, xylene or toluene, preferably toluene, at a temperature from about 25° C. to about 110° C., preferably at about the reflux temperature of the solvent. Suitable dehydrating agents/solvent systems include titanium tetrachloride/dichloromethane titanium isopropoxide/dichloromethane and molecular sieves/THF. Titanium tetrachloride/dichloromethane is preferred.
Compounds of the formula X wherein G is hydroxy, chloro, bromo or (C 1 -C 6 )alkoxy may be converted into the corresponding compounds of formula XII having the desired R 3 group by reacting them with the appropriate compound of the formula NH 2 R 3 under conditions that will be obvious to those skilled in the art, and then reducing the resulting amides to yield the desired compounds having formula I wherein R 2 is hydrogen. When G is hydroxy, the compound of formula X is reacted with NH 2 R 3 in the presence of an activating agent. Appropriate activating agents include carbonyldiimidazole, diethylphosphoryl cyanide and dicyclohexylcarbodiimide. Carbonyldiimidazole is preferred. This reaction is generally conducted at a temperature from about 0° C. to about 50° C., preferably at about 25° C., in an inert solvent such as chloroform, diethyl ether, THF or dimethylformamide (DMF).
When G is chloro or bromo, the reaction of the compound of formula X with the appropriate compound of formula NH 2 R 3 is typically carried out in the presence of an acid scavenger in an aprotic solvent at a temperature from about 0° C. to about 100° C. Suitable acid scavengers include triethylamine (TEA), pyridine and inorganic salts such as sodium and potassium carbonate. Suitable solvents include methylene chloride (CH 2 Cl 2 ), chloroform (CHCl 3 ), benzene, toluene and tetrahydrofuran (THF). Preferably, the reaction is conducted in CH 2 Cl 2 at room temperature using TEA as the acid scavenger.
When G is O--(C 1 -C 6 )alkyl, the reaction of the compound of formula NH 2 R 3 is usually conducted in an aprotic solvent such as benzene, toluene, chlorobenzene or xylenes, at a temperature from about 25° C. to about 100° C., preferably at about the reflux temperature of the solvent.
Reduction of the compound of formula XII so formed yields the corresponding compound of the formula I wherein R 2 is hydrogen. This is generally accomplished using a reducing agent such as lithium aluminum hydride, borane dimethylsulfide complex or diborane, in an aprotic solvent such as THF, dioxane or diethyl ether, at a temperature from about 0° C. to about 70° C. Preferably, the reducing agent is borane dimethylsulfide complex and the reaction is carried out at about room temperature in an ethereal solvent such as THF.
Compounds of the formula I wherein R 2 is hydrogen may be converted into the corresponding compounds wherein R 2 is --CO 2 (C 1 -C 10 )alkyl by reacting them with a (C 1 -C 10 )alkyl halo carbonate such as methyl or ethyl chloroformate in the presence of an acid scavenger. Typically, this reaction is conducted in an polar solvent such as chloroform, methylene chloride, water or a water/acetone mixture, at a temperature from about 0° C. to about 100° C., preferably at about room temperature. Suitable acid scavengers include triethylamine, pyridine and potassium and sodium carbonate or bicarbonate.
When R 3 is a group of the formula II, the starting materials of the formula NH 2 R 3 may be prepared as described in U.S. patent application Ser. No. 556,338, filed Jul. 20. 1990, which issued as U.S. Pat. No. 5,162.339, issued Nov. 10, 1992. This application is incorporated herein in its entirety.
When R 3 is a group of the formula III, the starting materials of the formula NH 2 R 3 may be prepared as described in U.S. patent application Ser. No. 532,525, filed Jun. 1, 1990, which was filed as PCT patent application PCT/US 91/02853, filed Apr. 25, 1991, which was filed as U.S. National patent application Ser. No. 07/955,733, filed Dec. 1, 1992, which issued as U.S. Pat. No. 5,451,586, issued Sep. 19, 1995. Both these applications are incorporated herein in their entirety.
When R 3 is a group of the formula IV, V or VI, the starting materials of the formula NH 2 R 3 may be prepared as described in U.S. patent application Ser. No. 557,442, filed Jul. 23, 1990, which was filed as PCT patent application PCT/US 91/03369, filed May 14, 1991, which was filed as U.S. National application Ser. No. 07/988,125, filed Feb. 1, 1993, which issued as U.S. Pat. No. 5,422,354, issued Jun. 6, 1995. Both these applications are incorporated herein in their entirety.
When R 3 is a group of the formula VII, the starting materials of the formula NH 2 R 3 may be prepared as described in U.S. patent application Ser. No. 724,268, filed Jul. 1, 1991, which issued as U.S. Pat. No. 5,232,929, issued Aug. 3, 1993; U.S. patent application Ser. No. 800,667, filed Nov. 27, 1991, which issued as U.S. Pat. No. 5,364,943, issued Nov. 15, 1994; and PCT patent application PCT/US 92/00065, filed Jan. 14, 1992, which published as WO 92/17449, published Oct. 15, 1992, and which was filed as pending U.S. National application Ser. No. 08/119,149, filed Sep. 20, 1993. These applications are incorporated herein in their entirety.
When R 3 is a group of the formula VIII, the starting materials of the formula NH 2 R 3 may be prepared as described in PCT patent application PCT/US 91/05776, filed Aug. 20, 1991, which published as WO 92/06079, published Apr. 16, 1992; U.S. patent application Ser. No. 800,667, filed Nov. 27, 1991, which issued as U.S. Pat. No. 5,364,943, issued Nov. 15, 1994; and PCT patent application PCT/US 92/00065, filed Jan. 14, 1992, which published as WO 92/17449, published Oct. 15, 1992 and which was filed as pending U.S. National application Ser. No. 08/119,149, filed Sep. 20, 1993. These applications are incorporated herein in their entirety.
When R 3 is a group of the formula IX, the starting materials of the formula NH 2 R 3 may be prepared as described in U.S. patent application Ser. No. 719,884, filed Jun. 21, 1991, which was filed as International patent application PCT/US92/04697, filed Jun. 11, 1992, and published as WO 93/00330, published Jan. 7, 1993, and was filed as U.S. National patent application Ser. No. 08/167,851, filed Dec. 14, 1994, which issued as U.S. Pat. No. 5,604,252, issued Feb. 18, 1997. This application is incorporated herein in its entirety.
Scheme 2 illustrates the preparation of the starting materials of formula X wherein G is hydrogen and R 1 is other than ##STR20## Once formed, these compounds can be converted into the corresponding compounds of the formula I or XI according to the procedures described above.
Referring to scheme 2, a compound of the formula XIII
wherein R 1 is other than ##STR21## or --SO 2 NR 4 R 5 is reacted with titanium tetrachloride (TiCl 4 ) and dichloromethyl methyl ether (CHCl 2 --O--CH 3 ) at a temperature from about 0° C. to about room temperature in a methylene chloride solvent to yield the corresponding aldehyde of formula X wherein G is hydrogen. Alternatively, the compound of the formula XIII may be reacted with hexamethylene tetraamine and trifluoroacetic acid at about 70° C. to yield the same product.
Those compounds of the formula XIII wherein R 1 is --SO--(C 1 -C 10 )alkyl, --SO 2 --(C 1 -C 10 )alkyl, --SO-aryl or --SO 2 -aryl may be obtained from their deoxygenated counterparts of the formula XIII wherein R 1 is --S--(C 1 -C 10 )alkyl or --S-aryl by reacting them with an oxidizing agent. For example, such oxidation may be carried out using metachloroperbenzoic acid in methylene chloride at about room temperature. It may also be carried out using peroxyphthalic acid magnesium hydrate in aqueous ethanol at a temperature from about 70° C. to about 100° C. The foregoing oxidation reactions produce mixtures of the oxy and dioxy products (--SO-- and --SO 2 --) which can be separated by ordinary means.
Compounds of the formula X wherein G is hydrogen and R 1 is --NHCOCF 3 may be obtained using procedures known to those skilled in the art. Scheme 3 illustrates one method of preparing such compounds. Referring to scheme 3, the --CHO group of a nitro benzaldehyde of the formula XIV is protected by conversion to the corresponding 1,3-dioxolane of formula XV. This reaction is generally carried out by heating a mixture of the nitrobenzaldehyde and ethylene glycol in an inert solvent such as benzene or toluene, preferably in the presence of an acid such as p-toluenesulfonic acid, and preferably at the reflux temperature of the solvent to remove the water formed in the reaction. The resulting compound of formula XV is then treated with hydrogen gas and a metal catalyst such as palladium on carbon in a reaction inert solvent such as ethyl acetate or a lower alcohol to convert the NO 2 group to an NH 2 group and produce the corresponding compound of formula XVI.
The resulting intermediate of formula XVI is then acylated with a reagent such as ethyl trifluoroacetate in methanol or trifluoroacetic anhydride in methylene chloride at a temperature from about 0° C. to about 50° C., preferably at about room temperature, to produce the corresponding trifluoroacetamide of the formula XVII. Treatment of this amide with a mixture of aqueous hydrochloric acid in acetone at a temperature from about 0° C. to about 50° C., preferably at room temperature, will convert the dioxolane to the desired compound of formula X wherein R 1 is NHCOCF 3 and G is hydrogen.
Scheme 4 illustrates the preparation of the starting materials of the formula X wherein G is hydrogen and R 1 is --SO 2 NR 4 R 5 . Referring to scheme 4, a compound of formula X wherein R 1 is --SO 2 NR 4 R 5 and G is (C 1 -C 3 )alkoxy is reacted with a reducing agent in a reaction inert solvent, for example lithium borohydride (LiBH 4 ) in tetrahydrofuran (THF). The reduction, which yields an alcohol of the formula XVIII, is usually conducted at a temperature from about 0° C. to about 100° C., preferably by heating the reaction mixture to the reflux temperature of the solvent. The alcohol of formula XVIII may then be oxidized using methods known to those skilled in the art. For example, treatment of a solution of such alcohol in a solvent such as methylene chloride with an oxidizing agent such as pyridinium dichromate at a temperature from about 0° C. to about 50° C., preferably at room temperature, will yield the corresponding compounds of formula X wherein G is hydrogen and R 1 is --SO 2 NR 4 R 5 . Other oxidizing agents/solvent systems such as manganese dioxide/acetone and chromium trioxide/acetic anhydride/acetic acid are also capable of producing this conversion.
The preparation of other compounds of the formula I not specifically described in the foregoing experimental section can be accomplished using combinations of the reactions described above that will be apparent to those skilled in the art.
In each of the reactions discussed or illustrated in schemes 1 to 4 above, pressure is not critical unless otherwise indicated. Pressures from about 0.5 atmospheres to about 5 atmospheres are generally acceptable, and ambient pressure, i.e. about 1 atmosphere, is preferred as a matter of convenience.
The novel compounds of the formula I and the pharmaceutically acceptable salts thereof are useful as substance P antagonists, i.e., they possess the ability to antagonize the effects of substance P at its receptor site in mammals, and therefore they are able to function as therapeutic agents in the treatment of the aforementioned disorders and diseases in an afflicted mammal.
The compounds of the formula I which are basic in nature are capable of forming a wide variety of different salts with various inorganic and organic acids. Although such salts must be pharmaceutically acceptable for administration to animals, it is often desirable in practice to initially isolate a compound of the Formula I from the reaction mixture as a pharmaceutically unacceptable salt and then simply convert the latter back to the free base compound by treatment with an alkaline reagent and subsequently convert the latter free base to a pharmaceutically acceptable acid addition salt. The acid addition salts of the base compounds of this invention are readily prepared by treating the base compound with a substantially equivalent amount of the chosen mineral or organic acid in an aqueous solvent medium or in a suitable organic solvent, such as methanol or ethanol. Upon careful evaporation of the solvent, the desired solid salt is readily obtained.
Those compounds of the formula I which are also acidic in nature, e.g., where R 6 or R 10 is carboxyphenyl, are capable of forming base salts with various pharmacologically acceptable cations. Examples of such salts include the alkali metal or alkaline-earth metal salts and particularly, the sodium and potassium salts. These salts are all prepared by conventional techniques. The chemical bases which are used as reagents to prepare the pharmaceutically acceptable base salts of this invention are those which form non-toxic base salts with the acidic compounds of formula I. Such non-toxic base salts include those derived from such pharmacologically acceptable cations as sodium, potassium, calcium and magnesium, etc. These salts can easily be prepared by treating the corresponding acidic compounds with an aqueous solution containing the desired pharmacologically acceptable cations, and then evaporating the resulting solution to dryness, preferably under reduced pressure. Alternatively, they may also be prepared by mixing lower alkanolic solutions of the acidic compounds and the desired alkali metal alkoxide together, and then evaporating the resulting solution to dryness in the same manner as before. In either case, stoichiometric quantities of reagents are preferably employed in order to ensure completeness of reaction and maximum yields of the desired final product.
The compounds of formula I and their pharmaceutically acceptable salts exhibit substance P receptor-binding activity and therefore are of value in the treatment and prevention of a wide variety of clinical conditions the treatment or prevention of which are effected or facilitated by a decrease in substance P mediated neurotransmission. Such conditions include inflammatory diseases (e.g., arthritis, psoriasis, asthma and inflammatory bowel disease), anxiety, depression or dysthymic disorders, colitis, psychosis, pain, allergies such as eczema and rhinitis, chronic obstructive airways disease, hypersensitivity disorders such as poison ivy, vasospastic diseases such as angina, migraine and Reynaud's disease, fibrosing and collagen diseases such as scleroderma and eosinophilic fascioliasis, reflex sympathetic dystrophy such as shoulder/hand syndrome, addiction disorders such as alcoholism, stress related somatic disorders, peripheral neuropathy, neuralgia, neuropathological disorders such as Alzheimer's disease, AIDS related dementia, diabetic neuropathy and multiple sclerosis, disorders related to immune enhancement or suppression such as systemic lupus erythematosus, and rheumatic diseases such as fibrositis. Hence, these compounds are readily adapted to therapeutic use as substance P antagonists for the control and/or treatment of any of the aforesaid clinical conditions in mammals, including humans.
The compounds of the formula I and the pharmaceutically acceptable salts thereof can be administered via either the oral, parenteral or topical routes. In general, these compounds are most desirably administered in dosages ranging from about 5.0 mg up to about 1500 mg per day, although variations will necessarily occur depending upon the weight and condition of the subject being treated and the particular route of administration chosen. However, a dosage level that is in the range of about 0.07 mg to about 21 mg per kg of body weight per day is most desirably employed. Variations may nevertheless occur depending upon the species of animal being treated and its individual response to said medicament, as well as on the type of pharmaceutical formulation chosen and the time period and interval at which such administration is carried out. In some instances, dosage levels below the lower limit of the aforesaid range may be more than adequate, while in other cases still larger doses may be employed without causing any harmful side effect, provided that such larger doses are first divided into several small doses for administration throughout the day.
The compounds of the formula I and their pharmaceutically acceptable salts ("the therapeutic compounds") may be administered alone or in combination with pharmaceutically acceptable carriers or diluents by either of the three routes previously indicated, and such administration may be carried out in single or multiple doses. More particularly, the novel therapeutic agents of this invention can be administered in a wide variety of different dosage forms, i.e., they may be combined with various pharmaceutically acceptable inert carriers in the form of tablets, capsules, lozenges, troches, hard candies, powders, sprays, creams, salves, suppositories, jellies, gels, pastes, lotions, ointments, aqueous suspensions, injectable solutions, elixirs, syrups, and the like. Such carriers include solid diluents or fillers, sterile aqueousmedia and various non-toxic organic solvents, etc. Moreover, oral pharmaceutical compositions can be suitably sweetened and/or flavored. In general, the therapeutically-effective compounds of this invention are present in such dosage forms at concentration levels ranging from about 5.0% to about 70% by weight.
For oral administration, tablets containing various excipients such as microcrystalline cellulose, sodium citrate, calcium carbonate, dicalcium phosphate and glycine may be employed along with various disintegrants such as starch (and preferably corn, potato or tapioca starch), alginic acid and certain complex silicates, together with granulation binders like polyvinylpyrrolidone, sucrose, gelatin and acacia. Additionally, lubricating agents such as magnesium stearate, sodium lauryl sulfate and talc are often very useful for tabletting purposes. Solid compositions of a similar type may also be employed as fillers in gelatin capsules; preferred materials in this connection also include lactose or milk sugar as well as high molecular weight polyethylene glycols. When aqueous suspensions and/or elixirs are desired for oral administration, the active ingredient may be combined with various sweetening or flavoring agents, coloring matter or dyes, and, if so desired, emulsifying and/or suspending agents as well, together with such diluents as water, ethanol, propylene glycol, glycerin and various like combinations thereof.
For parenteral administration, solutions of a therapeutic compound of the present invention in either sesame or peanut oil or in aqueous propylene glycol may be employed. The aqueous solutions should be suitably buffered if necessary and the liquid diluent first rendered isotonic. These aqueous solutions are suitable for intravenous injection purposes. The oily solutions are suitable for intraarticular, intramuscular and subcutaneous injection purposes. The preparation of all these solutions under sterile conditions is readily accomplished by standard pharmaceutical techniques well known to those skilled in the art.
Additionally, it is also possible to administer the compounds of the present invention topically when treating inflammatory conditions of the skin and this may preferably be done by way of creams, jellies, gels, pastes, ointments and the like, in accordance with standard pharmaceutical practice.
The activity of the therapeutic compounds of the present invention as substance P receptor antagonists may be determined by their ability to inhibit the binding of substance P at its receptor sites in bovine caudate tissue, employing radioactive ligands to visualize the tachykinin receptors by means of autoradiography. The substance P antagonizing activity of the herein described compounds may be evaluated by using the standard assay procedure described by M. A. Cascieri et al., as reported in the Journal of Biological Chemistry, Vol. 258, p. 5158 (1983). This method essentially involves determining the concentration of the individual compound required to reduce by 50% the amount of radiolabelled substance P ligands at their receptor sites in said isolated cow tissues, thereby affording characteristic IC 50 values for each compound tested.
In this procedure, bovine caudate tissue is removed from a -70° C. freezer and homogenized in 50 volumes (w./v.) of an ice-cold 50 mM Tris (i.e., trimethamine which is 2-amino-2-hydroxymethyl-1,3-propanediol) hydrochloride buffer having a pH of 7.7. The homogenate is centrifuged at 30,000×G for a period of 20 minutes. The pellet is resuspended in 50 volumes of Tris buffer, rehomogenized and then recentrifuged at 30,000×G for another twenty-minute period. The pellet is then resuspended in 40 volumes of ice-cold 50 mM Tris buffer (pH 7.7) containing 2 mM of calcium chloride, 2 mM of magnesium chloride, 4 μg/ml of bacitracin, 4μg/ml of leupeptin, 2μg of chymostatin and 200 g/ml of bovine serum albumin. This step completes the production of the tissue preparation.
The radioligand binding procedure is then carried out in the following manner, viz., by initiating the reaction via the addition of 100 μl of the test compound made up to a concentration of 1 μM, followed by the addition of 100 μl of radioactive ligand made up to a final concentration 0.5 mM and then finally by the addition of 800 μl of the tissue preparation produced as described above. The final volume is thus 1.0 ml, and the reaction mixture is next vortexed and incubated at room temperature (ca. 20° C.) for a period of 20 minutes. The tubes are then filtered using a cell harvester, and the glass fiber filters (Whatman GF/B) are washed four times with 50 mM of Tris buffer (pH 7.7), with the filters having previously been presoaked for a period of two hours prior to the filtering procedure. Radioactivity is then determined in a Beta counter at 53% counting efficiency, and the IC 50 values are calculated by using standard statistical methods.
The ability of the therapeutic compounds of this invention to inhibit substance P induced effects in vivo may be determined by the following procedures "a" through "d". (Procedures "a" through "c" are described in Nagahisa et al., European Journal of Pharmacology, 217, 191-5 (1992), which is incorporated herein by reference in its entirety.)
a. Plasma extravasation in the skin
Plasma extravasation is induced by intradermal administration of substance P (50 μl, 0.01% BSA-saline solution) in dorsal skin of pentobarbital (25 mg/kg i.p.) anesthetized male Hartley guinea pigs weighing 450-500 g. The compound to be tested is dissolved in 0.1% methyl cellulose-water (MC) and dosed p.o. 1 hour before substance P challenge (3 pmol/site). Evans blue dye (30 mg/kg) is administered intravenously 5 minutes before challenge. After 10 minutes, the animals are sacrificed, the dorsal skin is removed, and the blue spots are punched out using a cork borer (11.5 mm oral dose (o.d.)). Tissue dye content is quantitated after overnight formamide extraction at 600 nm absorbance.
b. Capsaicin-induced plasma extravasation
Plasma extravasation is induced by intraperitoneal injection of capsaicin (10 ml of 30 μM solution in 0.1% BSA/saline) into pentobarbital anesthetized (25 mg/kg i.p.) guinea pigs. The compound to be tested is dissolved in 0.1% MC and dosed p.o. 1 hour before capsaicin challenge. Evans blue dye (30 mg/kg) is administered i.v. 5 minutes before challenge. After 10 minutes, the animals are sacrificed, and both right and left ureters are removed. Tissue dye content is quantitated as in "a" above.
c. Acetic acid-induced abdominal stretching
Male ddY mice (SLC, Japan), weighing 14-18 g, were fasted overnight. The compound to be tested is dissolved in 0.1% MC and dosed p.o. 0.5 hour before acetic acid (AA) injection (0.7%, 0.16 ml/10 g body weight). The animals are placed in clear beakers (1 per beaker) and the stretching response is counted 10 to 20 minutes after the AA injection (10 minute interval).
d. Substance p-induced hyperlocomotor paradigm
The anti-psychotic activity of the therapeutic compounds of the present invention as neuroleptic agents for the control of various psychotic disorders may be determined by a study of their ability to suppress substance P-induced or substance P agonist induced hypermotility in guinea pigs. This study is carried out by first dosing the guinea pigs with a control compound or with an appropriate test compound of the present invention, then injecting the guinea pigs with substance P or a substance P agonist by intracerebral administration via canula and thereafter measuring their individual locomotor response to said stimulus.
The present invention is illustrated by the following examples. It will be understood, however, that the invention is not limited to the specific details of these examples.
PREPARATION 1
2-Cyclopentyloxy-5-(N-methyl-N-methanesulfonylamino)-benzaldehyde
A. 4-Cyclopentyloxy-N-methanesulfonylaniline
Under N 2 in a flame-dried flask, a mixture of 4-cyclopentyloxyaniline (1.0 g, 5.64 mmol) in 25 mL of dry CH 2 Cl 2 was treated with triethylamine (1.3 mL, 9.38 mmol) and cooled to 0° C. A solution of recrystallized methanesulfonic anhydride (1.5 g, 8.62 mmol) in 10 mL of dry CH 2 Cl 2 was added dropwise and the reaction was stirred for 1.5 hours. The reaction mixture was then poured into 100 mL of saturated aqueous NaHCO 3 and extracted with CH 2 Cl 2 (3×50 mL). The combined organics were dried over MgSO 4 , evaporated in vacuo to a dark grey solid and flash chromatographed on silica gel, eluting with hexanes:EtOAc (80:20), to produce the pure intermediate compound, 0.8 g (56%), m.p. 140°-142° C.
B. 4-Cyclopentyloxy-N-methyl-N-methanesulfonylaniline
Under N 2 in a flame-dried flask, the preceding intermediate (0.5 g, 1.96 mmol) in 25 mL of acetone was treated with K 2 CO 3 (0.54 g, 3.91 mmol), stirred for 5 minutes at 25° C. and treated with methyl iodide (0.33 g, 2.32 mmol). After 18 hours, the suspension was filtered through a pad of diatomaeous earth (d.e.), concentrated in vacuo, redissolved in 100 mL of ethyl acetate (EtOAc), refiltered and concentrated to an off-white solid, 300 mg (57%), m.p. 120°-122° C.
C. 2-Cyclopentyloxy-5-(N-methyl-N-methanesulfonylamino)benzaldehyde
Under N 2 in a flame-dried flask, the above intermediate from part "B" (300 mg, 1.11 mmol) in 15 mL of CH 2 Cl 2 was cooled to 0° C. and treated with titanium tetrachloride (0.46 g, 0.27 mL, 2.42 mmol). After 20 minutes at 0° C. α,α-dichloromethyl methyl ether (0.15 g, 0.12 mL, 1.33 mmol) was added and the reaction was left to slowly warm to room temperature overnight. The reaction was quenched in 100 mL of saturated aqueous NaHCO 3 , extraced with CH 2 Cl 2 (3×75 mL) and dried over MgSO 4 . Concentration in vacuo gave a light brown solid which was filtered through a pad of d.e. to obtain the purified title aldehyde, 155 mg (47%).
Mass Spectrum (MS): m/e 297 (p+), 229, 150 (100%).
1 H NMR (CDCl 3 ) δ1.6-2.05 (m, 10H), 2.85 (s, 3H), 3.3 (s, 3H), 4.95 (m, 1H), 7.0 (d, 1H), 7.2-7.75 (m, 3H), 10.5 (s, 1H).
The following intermediate aldehydes of the general formula X were prepared by a procedure similar to that of Preparation 1.
2-Methoxy-5-(trifluoromethylthio)benzaldehyde, m.p. 61°-64° C., 30% yield.
5-Tert-butyl-2-methylthiobenzaldehyde, oil, 54% yield, MS: m/e 208 (p+), 193 (100%), 165, 117.
1 H NMR (CDCl 3 ) δ1.30 (s, 9H), 2.45 (s, 3H), 7.28 (d, 1H), 7.55 (dd, 1H), 7.82 (d, 1H), 10.3 (s, 1H).
5-Chloro-2-methylthiobenzaldehyde, m.p. 51°-54° C., 52% yield.
2-Methoxy-5-(N-methyl-N-methanesulfonylamino)-benzaldehyde, 89%, 1 H NMR (CDCl 3 ) δ2.9 (s, 3H), 3.4 (s, 3H), 4.0 (s, 3H), 7.1 (d, 1H), 7.7-7.85 (m, 2H), 10.5 (s, 1H).
2-Methoxy-5-(N-isopropyl-N-methanesulfonylamino)-benzaldehyde, m.p. 114°-116° C., 81% yield.
2-Methoxy-5-(1,1-dioxo-2-thiazolidinyl)benzaldehyde, m.p. 99°-101° C., 82% yield.
2-Isopropoxy-5-(N-methyl-N-methanesulfonylamino)-benzaldehyde, m.p. 107°-110° C., 60% yield.
2-Isopropoxy-5-(N-methyl-N-trifluoromethanesulfonylamino)benzaldehyde, m.p. 42°-45° C., 83% yield.
2-Methoxy-5-(N-methyl-N-trifluoromethanesulfonylamino)-benzaldehyde, 55% yield, 1 H NMR (CDCl 3 ) δ3.46 (s, 3H), 3.98 (s, 3H), 7.04 (d, 1H), 7.57 (dd, 1H), 7.81 (d, 1H), 10.4 (s, 1H). MS: m/e 297 (p+).
2-Methoxy-5-(N-methyl-N-isopropylsulfonylamino)-benzaldehyde, 39% yield.
2-Methoxy-5-(N-methyl-N-(4-methylphenylsulfonyl)amino)-benzaldehyde, oil, 88% yield.
2-Isopropoxy-5-(N-methyl-N-(4-methylphenylsulfonyl)amino)benzaldehyde, 28% yield, 1 H NMR (CDCl 3 ) δ1.45 (d, 6H0, 2.42 (s, 3H), 3.10 (s, 3H), 4.70 (m, 1H), 7.0 (m, 3H), 7.25 (m, 3H), 7.42 (d, 2H), 7.58 (dd, 1H), 10.4 (s, 1H). MS: m/e 347 (p+), 305, 150 (100%).
2-Methoxy-5-(N-methyl-N-benzylsulfonylamino)benzaldehyde, 51% yield, 1 H NMR (CDCl 3 ) δ3.14 (s, 3H), 3.94 (s, 3H), 4.27 (s, 2H), 6.95 (d, 1H), 7.35-7.58 (m, 7H), 10.4 (s, 1H). MS: m/e 319 (p+), 255, 164, 91 (100%).
5-Methoxy-1-methanesulfonyl-2,3-dihydroindol-6-carboxaldehyde, 49% yield, 1 H NMR (CDCl 3 ) δ2.85 (s, 3H), 3.19 (t, 2H), 3.90 (s, 3H), 3.98 (t, 2H), 6.90 (s, 1H), 7.73 (s, 1H), 10.3 (s, 1H).
5-Methoxy-3-methyl-1-methanesulfonyl-2,3-dihydroindol-6-carboxaldehyde, m.p. 147°-150° C., 49% yield, 1 H NMR (CDCl 3 ) δ1.45 (d, 3H), 2.75 (dd, 1H), 2.85 (s, 3H), 3.5 (dd, 1H), 3.95 (s, 3H), 4.5 (m, 1H), 6.9 (s, 1H), 7.8 (s, 1H), 10.4 (S,1H).
2-Methoxy-5-(N-cyclopentyl-N-(4-methanesulfonylamino)-benzaldehyde, m.p. 95°-98° C., 62% yield.
2-Methoxy-5-(2-methyl-4-thiazolyl)benzaldehyde, 56% yield, 1 H NMR (CDCl 3 ) δ2.72 (s, 3H), 3.95 (s, 3H), 7.05 (d, 1H), 7.25 (s, 1H), 8.15 (dd, 1H), 8.25 (d, 1H), 10.5 (s, 1H).
2-Methoxy-5-(N-(3,4-dichlorobenzyl)-N-methanesulfonyl-amino)benzaldehyde, gum, 86% yield, 1 H NMR (CDCl 3 ) δ2.97 (s, 3H), 3.95 (s, 3H), 4.75 (s, 2H), 6.95 (d, 1H), 7.10 (d, 1H), 7.35 (m, 3H), 7.77 (d, 1H), 10.4 (s, 1H).
2-Methoxy-5-(N-cyclohexylmethyl-N-methanesulfonyl-amino)benzaldehyde, oil, 73% yield, 1 H NMR (CDCl 3 ) δ0.9-1.8 (m, 11H), 2.85 (s, 3H), 3.48 (d, 2H), 3.98 (s, 3H), 7.05 (d, 1H), 7.60 (dd, 1H), 7.75 (d, 1H), 10.5 (s, 1H).
5-(Isopropylsulfonyl)-2-methoxybenzaldehyde, m.p. 105°-107° C., 57% yield, MS: m/e 242 (M + , 27%), 200 (78%), 136 (100%), 1 H NMR (CDCl 3 ) δ1.3 (d, 6H), 3.15 (m, 1H), 4.05 (s, 3H), 7.15 (d, 1H), 8.05 (dd, 1H), 8.3 (d, 1H), 10.5 (s, 1H).
5-(N-cyclopentyl-N-methanesulfonyl)amino-2-methoxybenzaldehyde, m.p. 95°-98° C., 62% yield, MS: m/e 297 (M + , 20%), 229, 218 (100%), 150 (95%), 1 H NMR (CDCl 3 ) δ1.25-1.6 (m, 6H), 1.95 (m, 2H), 2.95 (s, 3H), 3.95 (s, 3H), 4.5 (m, 1H), 7.05 (d, 1H), 7.5 (dd, 1H), 7.7 (d, 1H), 10.45 (s, 1).
5-(N-cyclohexylmethyl-N-methanesulfonyl)amino-2-methoxybenzaldehyde, oil, 74% yield, 1 H NMR (CDCl 3 ) δ0.9-1.8 (m, 11H), 2.85 (s, 3H), 3.45 (d, 2H), 4.0 (s, 3H), 7.05 (d, 1H), 7.65 (dd, 1H), 7.75 (d, 1H), 10.45 (s, 1H).
2,3-Dihydro-N-methanesulfonyl-5-methoxy-2-methylindole-6-carboxaldehyde, m.p. 147°-150° C., 48% yield, 1 H NMR (CDCl 3 ) δ1.45 (d, 3H), 2.75 (m, 1H), 2.85 (s, 3H), 3.5 (dd, 1H), 3.9 (s, 3H), 4.5 (m, 1H), 6.9 (s, 1H), 7.83 (s, 1H), 10.4 (s, 1H).
2-Methoxy-5-(N-methyl-N-(2,4-dimethyl-5-thiazolesulfonyl))aminobenzaldehyde, oil, 29% yield, MS: m/e 340 (M + , 10%), 164 (100%), 1 H NMR (CDCl 3 ) δ2.1 (s, 3H), 2.5 (s, 3H), 3.1 (s, 3H), 3.9 (s, 3H), 7.0 (d, 1H), 7.5 (m, 1H), 7.6 (q, 1H), 10.4 (s, 1H).
2-Methoxy-5-(N-(4,5-dimethyl-2-thiazolyl)-N-methanesulfonyl)aminobenzaldehyde, waxy solid, 39% yield, MS: m/e (340 (M + , 20%), 261 (65%), 1 H NMR (CDCl 3 ) δ2.3 (d, 6H), 3.4 (s, 3H), 4.0 (s, 3H), 7.0 (s, 3H), 7.0 (d, 1H), 7.7 (q, 1H), 10.5 (s, 1H).
2-Methoxy-5-(N-(4,5-dimethyl-2-thiazolyl)-N-methyl)aminobenzaldehyde, oil, 7% yield, MS: m/e 277 (M +1 , 20%), 276 (100%), 126 (30), 1 H NMR (CDCl 3 ) δ2.1 (d, 6H), 3.4 (s, 3H), 4.0 (s, 3H), 7.0 (d, 1H), 7.6 (q, 1H), 7.8 (d, 1H), 10.5 (s, 1H).
2-Methoxy-5-(N-(4,5-dimethyl-2-thiazolyl))aminobenzaldehyde, m.p. 137°-139° C., 20% yield, MS: m/e 262 (M + , 100%), 1 H NMR (CDCl 3 ) δ2.15 (s, 3H), 2.25 (s, 3H), 3.9 (s, 3H), 7.0 (d, 1H), 7.6 (dd, 1H), 7.7 (dd, 1H), 10.5 (s, 1H).
2-Methoxy-5-(N-(ethoxycarbonylmethanesulfonyl)-N-methyl)aminobenzaldehyde, oil, 81% yield, 1 H NMR (CDCl 3 ) δ1.3 (t, 3H), 2.05 (s, 2H), 3.35 (s, 3H), 3.9 (s, 3H), 4.25 (q, 2H), 7.05 (d, 1H), 7.7 (dd, 1H), 7.9 (d, 1H), 10.5 (s, 1H).
2-Methoxy-5-(N-(3,4-dichlorobenzyl)-N-methanesulfonyl)aminobenzaldehyde, 86% yield, 1 H NMR (CDCl 3 ) δ3.0 (s, 3H), 3.95 (s, 3H), 4.8 (s, 2H), 6.95 (d, 1H), 7.15 (dd, 1H), 7.35 (m, 3H), 7.75 (d, 1H), 10.4 (s, 1H).
PREPARATION 2
2-Methoxy-5-methylthiobenzaldehyde
Under N 2 in a flame-dried flask, fitted with a condensor and stirrer, was placed a solution of 1-methoxy-4-methylthiobenzene (2.0 g, 13 mmol) in 75 mL of trifluoroacetic acid (TFA). Hexamethylenetetramine (1.2 g, 13 mmol) was added while stirring the reaction at 25° C. After heating for 2 hours to reflux, the reaction was cooled and concentrated in vacuo and the residue was partitioned between CH 2 Cl 2 and 2N sodium hydroxide (NaOH). The organic layer was dried over MgSO 4 , concentrated in vacuo to a yellow oil and flash chromatographed on silica gel eluting with hexanes:EtOAc (85:15) to give the pure title compound as a yellow oil, 0.99 g, 42% yield. 1 H NMR (CDCl 3 ) δ2.5 (s, 3H), 3.95 (s, 3H), 6.97 (d, 1H), 7.5 (dd, 1H), 7.78 (d, 1H), 10.5 (s, 1H).
Using a procedure similar to that of Preparation 2,4-methoxyphenyl cyclohexyl sulfide was converted to 2-methoxy-5-(cyclohexylthio)benzaldehyde, oil. 1 H NMR (CDCl 3 ) δ1.1-2.0 (m, 10H), 3.0 (m, 1H), 3.95 (s, 3H), 6.95 (d, 1H), 7.62 (dd, 1H), 7.90 (d, 1H), 10.45 (s, 1H).
PREPARATION 3
2-Phenoxybenzaldehyde
A mixture of 2-phenoxybenzyl alcohol (4.0 g, 20.2 mmol, prepared by the reduction of commercially available 2-phenoxybenzoic acid with LiAlH 4 /THF) and 150 mL CH 2 Cl 2 was treated with pyridinium dichromate (11.39 g, 30.3 mmol) at 25° C. and stirred for another 36 hours. The mixture was filtered through d.e. and then through a pad of silica gel to produce 3.11 g (78%) of title compound as a yellow oil. 1 H NMR (CDCl 3 ) δ6.8 (d, 1H), 6.9 (d, 1H), 7.0 (m, 2H), 7.1 (m, 2H), 7.2 (m, 1H), 8.9 (m, 1H), 10.2 (s, 1H).
Using a procedure similar to that of Preparation 3, the following benzaldehydes of formula X were prepared from the corresponding compounds of formula XVIII:
5-Diethylaminosulfonyl-2-methoxybenzaldehyde, 76%, 1 H NMR (CDCl 3 ) δ1.1 (t, 6H), 3.2 (q, 4H), 4.0 (s, 3H), 7.1 (d, 1H), 7.9 (dd, 1H), 8.2 (d, 1H), 10.4 (s, 1H).
5-Diethylaminosulfonyl-2-isopropoxybenzaldehyde, oil, 36%, 1 H NMR (CDCl 3 ) δ1.2 (t, 6H), 1.4 (d, 6H), 3.2 (q, 4H), 4.8 (m, 1H), 7.1 (d, 1H), 8.0 (dd, 1H), 8.2 (d, 1H), 10.4 (s, 1H).
PREPARATION 4
2-Trifluoromethoxy-5-(N-methyl-N-methanesulfonyl)benzaldehyde
A. To a mixture of concentrated sulfuric acid (81 mL) and concentrated nitric acid (15.5 mL), cooled to 0° C., was added 2-trifluoromethoxybenzaldehyde (25 g, 0.13 mol) portionwise while maintaining the temperature of the reaction below 0° C. After 1.5 hours, the reaction mixture was poured cautiously over 1000 mL of ice in a large beaker and left to stand for 0.5 hours. The resulting suspension was filtered, washed well with H 2 O and air dried to give crude 5-nitro-2-trifluoromethoxybenzaldehyde, m.p. 32°-34° C.
B. The preceding compound and ethylene glycol (35 mL, 0.62 mol) in 1000 mL of toluene was treated with paratoluenesulfonic acid (0.72 g, 4 mmol) and heated to reflux under N 2 for 24 hours, using a Dean-Stark trap to collect the water formed. The solvent was then removed in vacuo and the residue was dissolved in CH 2 Cl 2 , washed with saturated aqueous NaHCO 3 and dried over MgSO 4 . Removal of the solvent in vacuo gave crude 2-(5-nitro-2-trifluoromethoxyphenyl)-1,3-dioxolane as a pale orange oil.
C. The dioxolane from part B (5.09 g) in 100 mL of EtOAc was hydrogenated with 0.29 g of 5% palladium on carbon at 45 p.s.i. for 18 hours. After filtration through d.e., the solvent was removed in vacuo to give 2-(5-amino-2-trifluoromethoxyphenyl)-1,3-dioxolane as an orange oil, 4.6 g.
D. The above oil from part C and triethylamine (2.53 mL, 39 mmol) in 200 mL of dry THF was treated with methanesulfonic anhydride (4.9 g, 28 mmol) in 26 mL of THF at 25° C. After 72 hours, 200 mL of H 2 O was added and the mixture was stirred for another 30 minutes. The aqueous layer was extracted with CH 2 Cl 2 and the organics were combined, washed with 1N HCl, 2N NaOH and H 2 O, and finally dried over MgSO 4 . Removal of the solvent in vacuo gave an orange oil which was flash chromatographed on silica gel using hexanes:EtOAc (40:60). Pure 2-(5-methanesulfonylamino-2-trifluoromethoxyphenyl)-1,3-dioxolane was obtained as an oil, 1.64 g.
E. A suspension of sodium hydride (60% oil dispersion, 0.19 g, 4.75 mmol) in 10 mL of dry DMF was treated with the compound from part D (1.5 g, 4.58 mmol) in 20 mL of dry DMF and stirred at 25° C. for 30 minutes. Methyl iodide (0.28 mL, 4.5 mmol) was added and the mixture was stirred for an additional 15 hours. After dilution with 100 mL of water, the mixture was extracted with Et 2 O (3×100 mL) and the combined organics were dried over MgSO 4 and evaporated to give 2-(5-N-methyl-N-methanesulfonylamino)-2-trifluoromethoxyphenyl)-1,3-dioxolane as an orange oil, 1.63 g.
F. The preceding dioxolane from part E (1.63 g) in 30 mL of acetone was treated with 6N HCl at 25° C. for 72 hours. The acetone was then evaporated and the resulting solution was extracted with Et 2 O and the organics were washed with H 2 O, dried over MgSO 4 and concentrated to an oil. Flash chromatography on silica gel using hexanes:EtOAc (65:35) gave pure 5-(N-methyl-N-methanesulfonylamino)-2-trifluoromethoxy-benzaldehyde as an oil, 0.63 g (42%). 1 H NMR (CDCl 3 ) δ2.9 (s, 3H), 3.4 (s, 3H), 7.4 (dd, 1H), 7.8 (dd, 1H), 7.9 (d, 1H), 10.4 (s, 1H). MS: m/e 297 (p+), 218, 162.
PREPARATION 5
2-Methoxy-5-methanesulfonylbenzaldehyde
Under N 2 in a round-bottomed flask fitted with a condensor, 2-methoxy-5-methylthiobenzaldehyde (0.89 g, 4.9 mmol) was added to 0.6 mL of EtOH. To this, a solution of monoperoxyphthalic acid magnesium salt hexahydrate (2.41 g, 4.9 mmol) in 10.4 mL of H 2 O was added and the mixture was heated at 95° C. for 18 hours. The reaction was then quenched with 10 mL of H 2 O, extracted with CH 2 Cl 2 (4×10 mL) and the combined organics were dried over MgSO 4 and concentrated in vacuo to an oil, 0.34 g. Flash chromatography on silica gel, eluting with EtOAc:hexanes (2.98) gave the pure title compound as a white solid, 0.36 g, m.p. 140°-143° C. 1 H NMR (CDCl 3 ) δ3.05 (s, 3H), 4.05 (s, 3H), 7.2 (d, 1H), 8.15 (dd, 1H), 8.40 (d, 1H), 10.5 (s, 1H).
EXAMPLE 1
Cis-3-(5-fluoro-2methylthiobenzyl)amino-2-phenylpiperidine dihydrochloride
A. 5-Fluoro-2-methylthiobenzaldehyde
Under N 2 a solution of 8.81 g (62 mmole) of p-fluorothioanisole in 50 mL of dichloromethane was stirred, cooled to 0° C. and treated dropwise with 15 mL (136 mmole) of titanium tetrachloride (TiCl 4 ). After stirring approximately 30 minutes at this temperature, the red solution was treated with 6.73 mL (74.4 mmole) of a α,α-dichloromethyl methyl ether (Aldrich Chem Co.), stirred an additional 2 hours at 0° C. and allowed to warm to room temperature while stirring for another 18 hours. After pouring the reaction mixture into a mixture of 250 mL of saturated aqueous sodium bicarbonate and 250 mL of dichloromethane, the aqueous layer was extracted with three 50 mL portions of dichloromethane and the organic layers were combined and dried over magnesium sulfate (MgSO 4 ). Evaporation of the solvent produced a solid which was recrystallized from hexane; 0.72 g, M.P. 45°-47° C. Mass spectrum (m/e, %); 172 (17), 171 (33), 170 (100, M+), 155 (49), 142 (53), 127 (28).
B. Cis-3-(5-fluoro-2-methylthiobenzyl)amino-6-oxo-2-phenylpiperidine
A mixture of 0.67 g (3.52 mmole) of cis-3-amino-6-oxo-2-phenylpiperidine, 0.72 g (4.23 mmole) of the above aldehyde and 1 g of 3A molecular sieves (Aldrich) in 15 mL of acetic acid was stirred at 25° C. for approximately 1.5 hours, then treated with 1.71 g (8.1 mmole) of sodium triacetoxyborohydride. After stirring for another 18 hours, the mixture was filtered and the filtrate concentrated to a yellow oil. Chromatography on silica gel using dichoromethane:ethanol:concentrated ammonium hydroxide (98:1:1) produced the pure product as an oil which crystallized on standing; 0.51 g (42%), M.P. 125°-130° C. Mass spectrum (m/e, %): 345 (45, M +1 ) 344 (100 M + ), 210 (92), 155 (91), 106 (99).
C. Cis-3-(5-fluoro-2-methylthiobenzyl)amino-2-phenylpiperidine dihydrochloride
In a flame-dried flask 0.69 g (2 mmole) of the previous compound in 5 mL of tetrahydrofuran was treated with 3.0 mL of 1.0M borane-tetrahydrofuran complex (Aldrich), refluxed for 1 hour and stirred at 25° C. for 18 hours. After acidifying the crude mixture with 2N hydrochloric acid (HCl), it was extracted with dichloromethane and the aqueous layer was made basic with 2N sodium hydroxide (NaOH). This alkaline layer was finally extracted with dichloromethane which was dried over (MgSO 4 ) and concentrated to an oil; on standing it crystallized to an off-white solid, mp 60°-64° C. This free base was redissolved in dichloromethane and treated with hydrogen chloride (HCl) gas to form the dihydrochloride salt, recrystallized from methanol:diethyl ether as a white crystalline solid, M.P. 270°-273° C. Mass spectrum (m/e, %): 330 (15, M + ), 211 (100), 210 (65), 155 (98).
Anal. calc'd for C 19 H 23 FN 2 S.0.5 H 2 O: C, 55.34; H, 6.35; N, 6.79. Found: C, 55.08; H, 6.51; N, 6.59.
The title compounds of Examples 2-8 were prepared by a procedure similar to that of Example 1.
EXAMPLE 2
Cis-3-2-methlthiophenyl)methylamino-2-phenylpiperidine dihydrochloride
M.P. 256°-259° C. (MeOH:Et 2 O)
MS (m/e, %): 312 (M + ), 193, 192, 175, 160, 137 (100)
Anal. calc'd for C 19 H 24 N 2 S.2HCl: C, 59.21; H, 6.80; N, 7.27. Found: C, 59.08; H, 6.92; N, 7.18
EXAMPLE 3
Cis-3-(5-tert-butyl-2-methylthiophenyl)methylamino-2-phenylpiperidine dihydrochloride
M.P. 237°-240° C. (MeOH:Et 2 O)
MS (m/e, %): 368 (3, M + ), 367, 264, 210, 175, 155.
Anal. calc'd for C 23 H 32 N 2 S.2HCl.0.5 CH 2 Cl 2 : C, 59.65; H, 7.44; N, 6.79. Found: C, 59.37; H, 7.38; N, 6.12.
EXAMPLE 4
Cis-3-(5-chloro-2-methylthiophenyl)methylamino-2-phenylpiperidine dihydrochloride
M.P. 260°-265° C. (MeOH:Et 2 O)
MS (m/e, %): 348, 346 (M + ), 227, 180, 171, 120, 106.
Anal. calc'd for C 19 H 23 ClN 2 S.2HCl: C, 54.35; H, 6.00; N, 6.67. Found: C, 54.04; H, 6.08; N, 6.66.
EXAMPLE 5
Cis-3-(2-tert-butylthiophenyl)methylamino-2-phenylpiperidine dihydrochloride
M.P. 243°-245° C. dec. (MeOH:Et 2 O)
MS (m/e, %): 354 (6, M + ), 297, 235, 234, 178, 160, 123, 70(100).
Anal. calc'd for C 22 H 30 N 2 S.2HCl: C, 61.81; H, 7.55; N, 6.55. Found: C, 61.46; H, 7.26; N, 6.52.
EXAMPLE 6
Cis-3-(2-(4-chlorophenylthio(phenylmethylamino-2-phenylpiperidine dihydrochloride
M.P. 245°-249° C. dec. (MeOH:Et 2 O)
MS (m/e, %): 408 (M + ), 289, 231, 197 (100), 165, 146, 120.
Anal. calc'd for C 24 H 25 ClN 2 S.2HCl.1/3 H 2 O: C, 59.08; H, 5.72; N, 5.74. Found: C, 59.08; H, 5.61; N, 5.84.
EXAMPLE 7
Cis-3-(2-methoxy5-(trifluoromethylthio)phenyl)methylamino-2-phenylpiperidine dihydrochloride
M.P. 257°-259° C. (MeOH:Et 2 O)
Anal. calc'd for C 20 H 23 F 3 N 2 OS.2HCl.1/2H 2 O: C, 50.21; H, 5.48; N, 5.86. Found: C, 50.60; H, 5.42; N, 6.09.
EXAMPLE 8
Cis-3-(2-phenoxyphenyl)methylamino-2-phenylpiperidine hydrochloride
M.P. 210°-212° C. (MeOH:Et 2 O)
MS (m/e, %): 358 (M + ), 239, 198, 183 (100), 175, 160, 146.
Anal. calc'd for C 24 H 26 N 2 O.HCl.1/4H 2 O; C, 71.97; H, 6.79; N, 6.91. Found: C, 72.16; H, 6.94; N, 7.01.
EXAMPLE 9
(+)-(2S,3S)-3- 2-methoxy-5-(N-isopropyl-N-methane-sulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
A. (+)-(2S,3S)-3-Amino-2-phenylpiperidine
In a bottle were placed 9 g of 10% palladium-carbon, 180 ml of methanol, 275 ml of ethanol, 6.5 ml of concentrated hydrochloric acid and 9 g of the hydrochloride salt of (2S,3S)-3-(2-methoxybenzylamino)-2-phenylpiperidine. The mixture was shaken under hydrogen (40 p.s.i.) overnight, after which 9 g of additional catalyst were added to the system and the mixture was shaken under hydrogen for 1 day. The mixture was diluted with water (250 mL), filtered through diatomaceous earth (Celite (trademark)) and the Celite was rinsed well with water. The filtrate was concentrated to a volume of ca. 600-700 mL, made basic with concentrated aqueous sodium hydroxide and extracted with chloroform. The chloroform extracts were dried (sodium sulfate) and concentrated to obtain 4.4 g of the title compound as a colorless oil.
α! D (HCl salt)=+62.8° (c=0.46, methanol (CH 3 OH)).
1 H NMR (CDCl 3 ) δ1.68 (m, 4H), 2.72 (m, 1H), 2.94 (broad s, 1H), 3.16 (m, 1H), 3.80 (d, 1H, J=3), 7.24 (m, 5H).
HRMS calc'd for C 11 H 16 N 2 : 176.1310. Found: 176.1309.
Anal. calc'd for C 11 H 16 N 2 .2HCl.1/3H 2 O: C, 51.78; H, 7.36; N, 10.98. Found: C, 51.46; H, 7.27; N, 10.77.
B. (+)-(2S,3S)-3- 2-methoxy-5-(N-isopropyl-N-methane-sulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
Under a nitrogen atmosphere in a round-bottom flask were placed 80 mg (0.46 mmol) of (+)-(2S,3S)-3-amino-2-phenylpiperidine, 5 ml of acetic acid and 150 mg (0.55 mmol) of 2-methoxy-5-(N-isopropyl-N-methanesulfonylamino)benzaldehyde, and the mixture was stirred for 60 minutes. To the system were added 0.21 g (1.0 mmol) of sodium triacetoxyborohydride, and the mixture was stirred at room temperature overnight. The mixture was concentrated, basified with 1M aqueous sodium hydroxide and extracted with methylene chloride. The methylene chloride extracts were washed with water and extracted with 1M aqueous hydrochloric acid. The hydrochloric acid extracts were basified with 1M aqueous sodium hydroxide and extracted with methylene chloride. The methylene chloride extracts were dried (sodium sulfate) and concentrated to obtain 528 mg of colorless oil. The oil was dissolved in methylene chloride, and ether saturated with hydrogen chloride was added to the solution. The resulting white solid was collected by filtration and stirred in isopropanol at 60° C. for 2 hours. Filtration afforded 128 mg of the title compound as its hydrochloride.
M.P. 268°-270° C.
1 H NMR (CDCl 3 ; free base) δ1.0 (d, 6H), 1.38-2.20 (m, 6H), 2.80 (m, 2H), 2.85 (s, 3H), 3.2 (t, 1H), 3.35 (d, 1H), 3.50 (s, 3H), 3.70 (d, 1H), 3.90 (d, 1H), 4.50 (m, 1H), 6.65 (d, 1H), 6.90 (d, 1H), 7.05 (dd, 1H), 7.25 (m, 5H).
Mass spectrum: m/z 431 (parent), 312 (100%).
Anal. calc'd for C 23 H 33 N 3 O 3 S.2HCl: C, 54.75; H, 6.99; N, 8.32. Found: C, 54.75; H, 6.99; N, 8.29.
The title compounds of Examples 10-37 were prepared from either (+)-(2S,3S)-3-amino-2-phenylpiperidine or the corresponding racemate by employing the appropriate aldehyde and using a procedure similar to that of Example 9B.
EXAMPLE 10
(2S,3S)-3-(2-Methoxy-5-methylmercaptobenzylamino)-2-phenylpiperidine hydrochloride
M.P. 257°-259° C. (dec.)
1 H NMR (free base; CDCl 3 ) δ1.32 (m, 1H), 1.50 (m, 1H), 1.82 (m, 1H), 2.04 (m, 1H), 2.30 (s, 3H), 2.72 (m, 2H), 3.18 (m, 1H), 3.26 (d, 1H, J=15), 3.36 (s, 3H), 3.54 (d, 1H, J=15), 3.80 (d, 1H, J=3), 6.52 (d, 1H, J=10), 6.90 (d, 1H, J=3), 7.04 (dd, 1H, J=3, 10), 7.2 (m, 5H).
HRMS calc'd for C 20 H 26 N 2 OS: 342.1760. Found: 342.1770.
Anal. calc'd for C 20 H 26 N 2 OS.2HCl.0.25H 2 O: C, 57.20; H, 6.84; N, 6.67. Found: C, 57.35; H, 6,76; N, 6.61.
EXAMPLE 11
(2S,3S)-3-(2-Methoxy-5-methylsulfoxybenzylamino)-2-phenylpiperidine hydrochloride
M.P. 209° C. (dec).
1 H NMR (free base; CDCl 3 ) δ1.40 (m, 1H), 1.56 (m, 1H), 1.90 (m, 1H), 2.10 (m, 1H), 2.59, 2.62 (2S,3H), 2.76 (m, 2H), 3.22 (m, 1H), 3.42 (m, 1H), 3.49, 3.52 (2S,3H), 3.66 (m, 1H), 3.86 (d, 1H, J=3), 6.76 (m, 1H), 7.24 (m, 6H), 7.46 (m, 1H).
HRMS calc'd for C 20 H 27 N 2 O 2 S(M+1): 359.1787. Found: 359.1763.
EXAMPLE 12
(2S,3S)-3-(2-Methoxy-5-methylsulfonylbenzylamino)-2-phenylpiperidine hydrochloride
M.P.>260° C.
1 H NMR (free base; CDCl 3 ) δ1.40 (m, 1H), 1.58 (m, 1H), 1.88 (m, 1H), 2.10 (m, 1H), 2.78 (m, 2H), 2.96 (s, 3H), 3.24 (m, 1H), 3.38 (d, 1H, J=15), 3.54 (s, 3H), 3.66 (d, 1H, J=15), 3.90 (d, 1H, J=3), 6.74 (d, 1H, J=10), 7.26 (m, 5H), 7.58 (d, 1H, J=3), 7.72 (d, 1H, J=10).
HRMS calc'd for C 20 H 26 N 2 O 3 S: 374.1658. Found: 374.1622.
EXAMPLE 13
(2S,3S )-3-(2-Methoxy-5-phenoxybenzylamino)-2-phenylpiperidine hydrochloride
M.P.>250° C.
1 H NMR (free base; CDCl 3 ) δ1.34 (m, 1H), 1.74 (m, 2H), 2.06 (m, 1H), 2.76 (m, 2H), 3.22 (m, 1H), 3.32 (d, 1H, J=15), 3.44 (s, 3H), 3.60 (d, 1H, J=15), 3.85 (d, 1H, J=3), 6.60 (d, 1H, J=9), 6.67 (d, 1H, J=3), 6.78 (dd, 1H, J=6,9), 6.86 (d, 2H), 7.00 (t, 1H, J=6), 7.22 (m, 7H).
HRMS calc'd for C 25 H 28 N 2 O 2 : 388.2151. Found: 388.2137.
EXAMPLE 14
(2S,3S)-3-(2-Methoxy-5-N-methylmethanesulfonylamino-benzylamino)-2-phenylpiperidine hydrochloride
M.P. 281°-283° C.
1 H NMR (free base; CDCl 3 ) δ1.42 (m, 1H), 1.74 (m, 2H), 2.12 (m, 1H), 2.78 (m, 5H), 3.20 (s, 3H), 3.24 (m, 1H), 3.36 (d, 1H, J=15), 3.52 (s, 3H), 3.64 (d, 1H, J=15), 3.89 (d, 1H, J=3), 6.64 (d, 1H, J=9), 6.98 (d, 1H, J=3), 7.14 (dd, 1H, J=3, 9), 7.26 (m, 5H).
HRMS calc'd for C 21 H 29 N 3 O 3 S: 403.1992. Found: 403.1923.
Anal. calc'd for C 21 H 29 N 3 O 3 S.2HCl. 1/3H 2 O: C, 52.28; H, 6.61; N, 8.71. Found: C, 52.09; H, 6.63; N, 8.68.
EXAMPLE 15
Cis-3- 2-isopropoxy-5-(N-methyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 278°-280° C., 39% yield.
Anal. calc'd for C 23 H 33 N 3 O 3 S.2HCl: C, 54.75; H, 6.99; N, 8.32. Found: C, 54.83, H, 7.16, N, 8.16.
1 H NMR (free base, CDCl 3 ) δ1.10 (dd, 6H), 1.15-2.1 (m, 6H), 2.65-2.90 (m+s, 5H), 3.05-3.25 (m+s, 4H), 3.35 (d, 1H), 3.55 (d, 1H), 3.90 (d, 1H), 4.30 (m, 1H), 6.65 (d, 1H), 6.95 (d, 1H), 7.05-7.4 (m, 6H).
EXAMPLE 16
Cis-3- 2-methoxy-5-(N-isopropyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 268°-270° C., 65% yield.
Anal. calc'd for C 23 H 33 N 3 O 3 S.2HCl: C, 54.75; H, 6.99; N, 8.32. Found: C, 54.75, H, 6.99, N, 8.29.
1 H NMR (free base, CDCl 3 ) δ1.10 (dd, 6H), 1.45 (d, 1H), 1.60 (tt, 1H), 1.7-1.95 (m, 3H), 2.12 (d, 1H), 2.80 (m, 2H), 2.90 (s, 3H), 3.25 (d, 1H), 3.35 (d, 1H), 3.50 (s, 3H), 3.70 (d, 1H), 3.90 (d, 1H), 4.50 (m, 1H), 6.65 (d, 1H), 6.90 (d, 1H), 7.05 (dd, 1H), 7.30 (m, 5H).
EXAMPLE 17
Cis-3- 2-methoxy-5-(N-methyl-N-trifluoromethane-sulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 245°-250° C., 24% yield.
Anal. calc'd for C 21 H 26 F 3 N 3 O 3 S.2HCl: C, 47.55; H, 5.32; N, 7.92. Found: C, 47.55, H, 5.32, N, 7.86.
1 H NMR (free base, CDCl 3 ) δ1.50 (d, 1H), 1.60 (tt, 1H), 1.8-2.00 (m, 3H), 2.15 (d, 1H), 2.85 (m, 2H), 3.25 (d, 1H), 3.35 (s, 3H), 3.40 (d, 1H), 3.50 (s, 3H), 3.65 (d, 1H), 3.90 (d, 1H), 6.65 (d, 1H), 6.98 (d, 1H), 7.10 (dd, 1H), 7.25 (m, 5H).
EXAMPLE 18
Cis-3- 2-methoxy-5-(N-thiazolidine-S,S-dioxide)-benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 263°-265° C., 36% yield.
Anal. calc'd for C 22 H 29 N 3 O 3 S.2HCl: C, 54.09; H, 6.40; N, 8.60. Found: C, 53.87, H, 6.43, N, 8.45.
1 H NMR (free base, CDCl 3 ) δ1.40 (d, 1H), 1.60 (tt, 1H), 1.75 (m, 2H), 1.90 (m, 1H), 2.15 (d, 1H), 2.50 (m, 2H), 2.80 (m, 2H), 3.2-3.50 (m, 7H), 3.55-3.70 (m, 3H), 3.90 (d, 1H), 6.65 (d, 1H), 6.95 (d, 1H), 7.1-7.40 (m, 6H).
EXAMPLE 19
Cis-3- 2-trifluoromethoxy-5-(N,N-bis(methanesulfonyl)-amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 256°-257° C., 29% yield.
Anal. calc'd for C 21 H 26 F 3 N 3 O 5 S 2 .2HCl: C, 42.43; H, 4.75; N, 7.07. Found: C, 42.38, H, 4.77, N, 6.94.
1 H NMR (free base, CDCl 3 ) δ1.50 (d, 1H), 1.6-1.90 (m, 4H), 2.10 (d, 1H), 2.75-2.95 (m, 2H), 3.2-3.40 (m+s, 7H), 3.50 (d, 1H), 3.65 (d, 1H), 3.95 (d, 1H), 7.15-7.45 (m, 8H).
EXAMPLE 20
Cis-3- 2-methoxy-5-(N,N-diethylaminosulfonyl)-benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 267°-269° C., 29% yield.
Anal. calc'd for C 23 H 33 N 3 O 3 S 2 .2HCl: C, 54.75; H, 6.99; N, 8.32. Found: C, 54.98; H, 7.34; N, 8.18.
1 H NMR (free base, CDCl 3 ) δ1.15 (t, 6H), 1.50 (d, 1H), 1.6-2.00 (m, 4H), 2.10 (d, 1H), 2.80 (m, 2H), 3.15 (q, 4H), 3.30 (d, 1H), 3.55 (s+d, 4H), 3.70 (d, 1H), 3.95 (d, 1H), 6.70 (d, 1H), 7.30 (m, 5H), 7.65 (dd, 1H).
EXAMPLE 21
Cis-3- 2-trifluoromethoxy-5-(N-methyl-N-methane-sulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 247°-248° C., 43% yield.
Anal. calc'd for C 21 H 26 F 3 N 3 O 3 S 2 .2HCl: C, 47.55; H, 5.32; N, 7.92. Found: C, 47.51, H, 5.47, N, 7.60.
1 H NMR (free base, CDCl 3 ) δ1.50 (d, 1H), 1.6-1.95 (m, 4H), 2.10 (d, 1H), 2.75 (s, 3H), 2.85 (m, 2H), 3.15 (s, 3H), 3.30 (d, 1H), 3.50 (d, 1H), 3.65 (d, 1H), 3.95 (d, 1H), 7.1-7.45 (m, 8H).
EXAMPLE 22
Cis-3- 2-isopropoxy-5-(N-methyl-N-trifluoromethane-sulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 267°-273° C., 7% yield.
Anal. calc'd for C 23 H 30 F 3 N 3 O 3 S 2 .2HCl: C, 49.46; H, 5.41; N, 7.52. Found: C, 49.71, H, 5.72, N, 7.30.
1 H NMR (free base, CDCl 3 ) δ1.15 (dd, 6H), 1.4-1.95 (m, 5H), 2.15 (d, 1H), 2.30 (m, 2H), 3.15-3.4 (m+s, 5H), 3.55 (d, 1H), 3.90 (d, 1H), 4.35 (m, 1H), 6.65 (d, 1H), 6.95 (d, 1H), 7.10 (dd, 1H), 7.30 (m, 5H).
EXAMPLE 23
Cis-3- 2-methoxy-5-(N-methyl-N-isopropylsulfonyl-amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 264°-266° C., 22% yield.
Anal. calc'd for C 23 H 33 N 3 O 3 S.2HCl: C, 54.75; H, 6.99; N, 8.32. Found: C, 54.91, H, 7.04, N, 8.23.
1 H NMR (free base, CDCl 3 , δ) 1.35 (d, 6H), 1.45 (d, 1H), 1.55-1.95 (m, 4H), 2.15 (d, 1H), 2.85 (m, 2H), 3.25 (m+s, 5H), 3.35 (d, 1H), 3.50 (s, 3H), 3.65 (d, 1H), 3.90 (d, 1H), 6.65 (d, 1H), 7.05 (d, 1H), 7.15-7.35 (m, 6H).
EXAMPLE 24
Cis-3- 2-cyclopentyloxy-5-(N-methyl-N-methanesulfonyl-amino)benzyl!amino-2-phenylpiperidine dihydrochloride hemihydrate
M.P. 252°-255° C., 37% yield.
Anal. calc'd for C 25 H 35 N 3 O 3 S.2HCl.1/2H 2 O: C, 55.65, H, 7.10, N, 7.79. Found: C, 55.51, H, 6.95, N, 7.73.
1 H NMR (free base, CDCl 3 ) δ1.4-1.95 (m, 13H), 2.10 (d, 1H), 2.7-2.90 (m+s, 5H), 3.20 (s, 3), 3.25 (d, 1H), 3.35 (d, 1H), 3.55 (d, 1H), 3.85 (d, 1H), 4.55 (m, 1H), 6.65 (d, 1H), 6.95 (d, 1H), 7.10 (dd, 1H), 7.25 (m, 5H).
EXAMPLE 25
Cis-3- 2-methoxy-5-(N-methyl-N-(4-methylphenylsulfonyl)amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 215°-220° C., 42% yield.
Anal. calc'd for C 27 H 33 N 3 O 3 S.2HCl: C, 58.69, H, 6.38, N, 7.60. Found: C, 58.46, H, 6.30, N, 7.41. 1 H NMR (free base, CDCl 3 , δ) 1.30-2.04 (m, 7H), 2.40 (s, 3H), 2.74 (m, 2H), 3.05 (s, 3H), 3.25 (d, 1H), 3.40 (s, 3H), 3.52 (d, 1H), 3.80 (d, 1H), 6.52 (d, 1H), 6.62 (d, 1H), 6.85 (dd, 1H), 7.10-7.42 (m, 9H).
EXAMPLE 26
Cis-3- 2-isopropoxy-5-(N-methyl-N-(4-methylphenylsulfonyl)amino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 215°-219° C., 3.2% yield.
Anal. calc'd for C 29 H 37 N 3 O 3 S.2HCl: C, 59.99, H, 6.77, N, 7.23. Found: C, 59.98, H, 6.83, N, 7.19.
1 H NMR (free base, CDCl 3 , δ) 1.04 (dd, 6H), 1.30-2.05 (m, 7H), 2.40 (s, 3H), 2.75 (m, 2H), 3.04 (s, 3H), 3.24 (d, 1H), 3.44 (d, 1H), 3.80 (d, 1H), 4.26 (m, 1H), 6.55 (d, 1H), 6.63 (d, 1H), 6.85 (dd, 1H), 7.10-7.42 (m, 9H).
EXAMPLE 27
Cis-3- 2-isopropoxy-5-(N-isopropyl-N-methanesulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 243°-246° C., 23% yield.
Anal. calc'd for C 25 H 37 N 3 O 3 S.2HCl: C, 56.38, H, 7.38, N, 7.89. Found: C, 56.52, H, 7.03, N, 7.70.
1 H NMR (free base, CDCl 3 , δ) 1.10-1.5 (dd+dd, 12H), 1.40-2.20 (m, 6H), 2.60 (m, 2H), 2.80 (s, 3H), 3.30 (m, 1H), 3.35 (d, 1H), 3.65 (d, 1H), 3.80 (d, 1H), 4.35 (m, 1H), 4.50 (m, 1H), 6.95 (d, 1H), 7.05 (dd, 1H), 7.30 (m, 5H).
EXAMPLE 28
Cis-3- 2-isopropoxy-5-(N,N-diethylaminosulfonyl)-benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 246°-248° C. (dec.), 98% yield.
Anal. calc'd for C 25 H 37 N 3 O 3 S.2HCl: C, 56.39, H, 7.38, N, 7.89. Found: C, 56.29, H, 7.29, N, 7.82.
1 H NMR (free base, CDCl 3 , δ) 1.11 (m, 12H), 1.37-2.15 (m, 6H), 2.72-2.83 (m, 2H), 3.12-3.28 (q+m, 5H), 3.33 (d, 1H), 3.60 (d, 1H), 3.85 (d, J=2.2 Hz, 1H), 4.38 (m, 1H), 6.71 (d, 1H), 7.25 (m, 5H), 7.48 (d, 1H), 7.57 (dd, 1H).
EXAMPLE 29
Cis-3- 2-methoxy-5-(N-methyl-N-phenylmethylsulfonylamino)benzyl!amino-2-phenylpiperidine dihydrochloride
M.P. 266°-269° C. (dec.), 23% yield.
Anal. calc'd for C 27 H 33 N 3 O 3 S.2HCl: C, 58.69, H, 6.39, N, 7.60. Found: C, 58.70, H, 6.54, N, 7.41.
1 H NMR (free base, CDCl 3 , δ) 1.40-2.30 (m, 6H), 2.80 (m, 2H), 3.07 (s, 3H), 3.30 (m, 1H), 3.35 (d, 1H), 3.50 (s, 3H), 3.65 (d, 1H), 3.90 (d, 1H), 4.20 (s, 2H), 6.62 (d, 1H), 6.90 (d, 1H), 7.08 (dd, 1H), 7.20-7.45 (m, 10H).
EXAMPLE 30
Cis-3- (2,3-dihydro-5-methoxy-1-methanesulfonyl-6-indolyl)methylamino!-2-phenylpiperidine dihydrochloride
M.P. 255°-258° C., 27% yield.
Anal. calc'd for C 22 H 29 N 3 O 3 S.2HCl: C, 54.09, H, 6.40, N, 8.60. Found: C 54.10, H, 6.21, N, 8.52.
1 H NMR (free base, CDCl 3 , δ) 1.35-2.20 (m, 7H), 2.75 (m, 1H), 2.80 (s, 3H), 3.05 (t, 2H), 3.25 (m, 1H), 3.35 (d, 1H), 3.40 (s, 3H), 3.60 (d, 1H), 3.95 (m, 3H), 6.55 (s, 1H), 7.15 (s, 1H), 7.30 (m, 5H).
EXAMPLE 31
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(N-methyl-N-methanesulfonylamino)benzyl)-amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride monohydrate
M.P. 196°-200° C.
Anal. calc'd for C 29 H 35 N 3 O 3 S.2HCl.H 2 O: C, 58.38, H, 6.59; N, 7.04. Found: C, 58.71; H, 6.52; N, 6.93.
1 H NMR (D 2 O, δ) 1.85 (m, 1H), 2.35 (m, 1H), 3.06 (s, 3H), 3.27-3.63 (m+s+s, 10H), 3.85 (d, 1H), 3.96 (d+d, 2H), 4.26 (d, 1H), 4.39 (d, 1H), 4.8 (s, D 2 O), 5.16 (m, 1H), 6.97 (d, 1H), 7.21 (d, 1H), 7.31-7.50 (m, 1H).
EXAMPLE 32
(1SR,2SR,3SR,4RS)-3-(2-isopropoxy-5-(N-methyl-N-methanesulfonylamino)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride monohydrate
M.P. 182°-183° C.
Anal. calc'd for C 31 H 39 N 3 O 3 S.2HCl.H 2 O: C, 53.54; H, 5.58; N, 6.46. Found: C, 53.36; H, 5.71; N, 6.40.
1H NMR (D 2 O, δ) 1.20 (t, 6H), 1.90 (m, 1H), 2.35 (m, 1H), 3.06 (s, 3H), 3.26 (s, 3H), 3.29-3.47 (m, 4H), 3.84 (m, 3H), 4.14 (d, 1H), 4.36 (d, 1H), 4.45 (m, 1H), 4.80 (s, D 2 O), 5.08 (m, 1H), 6.96-7.04 (m, 2H), 7.26-7.47 (m, 11H).
EXAMPLE 33
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(N-methyl-N-trifluoromethanesulfonylamino)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride
M.P. 186° C.
HRMS calc'd for C 29 H 32 F 3 N 3 O 3 S: 559.2116. Found: 559.2197.
1 H NMR (D 2 O, δ) 1.85 (m, 1H), 2.34 (m, 1H), 3.36-3.55 (m+s, 10H), 3.72-3.85 (d+d, 4H), 4.14 (d, 1H), 4.37 (d, 1H), 4.80 (s, D 2 O), 5.03 (m, 1H), 6.97 (d, 1H), 7.24 (d, 1H), 7.32-7.53 (m, 11H).
EXAMPLE 34
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(N-methyl-N-phenylmethanesulfonylamino)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride hydrate
M.P. 178° C.
Anal. calc'd for C 35 H 39 N 3 O 3 S.2HCl.1.5H 2 O: C, 58.76; H, 7.00; N, 6.63. Found: C, 59.15; H, 6.60; N, 6.40.
1 H NMR (D 2 O, δ) 1.81 (m, 1H), 2.32 (m, 1H), 3.24-3.37 (m, 8H), 3.51 (m, 3H), 3.68 (m, 2H), 3.79 (d, 1H), 3.95 (d, 1H), 4.35 (d, 1H), 4.62 (s, 1H), 4.82 (s+m, 1H), 4.97 (m, 1H), 6.69 (d, 1H), 6.85 (d, 1H), 7.11 (dd, 1H), 7.37-7.50 (m, 15).
EXAMPLE 35
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(N-isopropyl-N-methanesulfonylamino)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride
M.P. 238° C. (dec.).
Anal. calc'd for C 31 H 39 N 3 O 3 S.2HCl: C, 61.08; H, 6.49; N, 6.74; N, 6.74. Found: C, 61.38; H, 6.81; N, 6.93.
1 H NMR (D 2 O, δ) 1.14 (d, 6H), 1.87 (m, 1H), 2.38 (m, 1H), 3.18 (s, 3H), 3.34-3.61 (m+s, 7H), 3.89 (d, 1H), 4.05 (m, 2H), 4.31-4.46 (m, 3H), 4.8 (s, D 2 O), 5.19 (m, 1H), 7.01 (d, 1H), 7.20 (d, 1H), 7.34-7.52 (m, 11H).
EXAMPLE 36
(1SR,2SR,3SR,4RS)-3-(2-methoxy-5-(1,1-dioxo-2-isothiazolidinyl)benzyl)amino-2-benzhydryl- 2.2.1!-azanorbornane dihydrochloride
M.P. 206°-207° C.
Anal. calc'd for C 30 H 35 N 3 O 3 S.2HCl: C: 60.09; H, 6.39; N, 7.01. Found: C, 59.77; H, 6.15; N, 6.94.
1 H NMR (D 2 O, δ) 1.90 (m, 1H), 2.35 (m, 1H), 2.56 (m, 2H), 3.33-3.62 (m+s, 10H), 3.77-3.83 (m, 4H), 3.96 (d, 1H), 4.15 (d, 1H), 4.41 (d, 1H), 4.8 (s, D 2 O), 5.10 (m, 1H), 7.00 (d, 1H), 7.13 (d, 1H), 7.32-7.47 (m, 11H).
EXAMPLE 37
(1SR,2SR,3SR,4RS)-3- (2,3-dihydro-5-methoxy-1-methanesulfonyl-6-indolyl)methylamino)benzyl!-2-benzhydryl 2.2.1!-azanorbornane dihydrochloride
M.P. 250° C.
Anal. calc'd for C 30 H 35 N 3 O 3 S.2HCl: C, 63.34; H, 6.38; N, 6.33. Found: C, 63.48; H, 6.15; N, 6.32.
1 H NMR (D 2 O, δ) 1.90 (m, 1H), 2.38 (m, 1H), 2.99 (s, 3H), 3.20 (t, 2H), 3.33-3.55 (m+s, 8H), 3.86 (d, 1H), 3.97-4.06 (m, 4H), 4.19 (d, 1H), 4.39 (d, 1H), 4.82 (s, D 2 O), 5.13 (m, 1H), 6.96 (s, 1H), 7.12 (s, 1H), 7.36-7.51 (m, 10H).
EXAMPLE 38
(2S,3S)-N-(2-Methoxy-5-methylthiophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
A. (2S,3S)-2-Diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine
(2S,3S)-N-(2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (4.13 g, 10 mmol) was hydrogenated in methanol (MeOH) (40 ml)/6N HCl (10 ml) by using 20% palladium hydroxide on carbon (0.2 g) at 2.5 kg/cm 2 of hydrogen for 60 hours. The filtrate was concentrated and the residue was partitioned between 2N NaOH and CH 2 Cl 2 . The organic layer was dried over MgSO 4 , and concentrated to give the crude product, which was recrystallized from ethanol (EtOH) to afford the pure title compound (2.80 g, 96%).
B. 2-Methoxy-5-methylthiobenzaldehyde
2-(2-Methoxy-5-methylthiophenyl)-1,3-dioxolane(2.40 g, 10 mmol) was stirred in 1N HCl (2 ml)/acetone (30 ml). After the starting material disappeared (ca. 2 hours), the solution was concentrated. The residue was partitioned between methylene chloride (CH 2 Cl 2 ) and saturated sodium bicarbonate (NaHCO 3 ) solution. The organic layer was washed with H 2 O, dried over MgSO 4 , and evaporated to give the aldehyde. (1.96 g, 100%).
C. (2S,3S)-N-(2-Methoxy-5-methylthiophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
To a solution of a 2-methoxy-5-methylthiobenzaldehyde (765 mg, 4.2 mmol) and (2S,3S)-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (1170 mg, 4 mmol) in CH 2 Cl 2 (40 ml) was added in portions sodium triacetoxyborohydride (933 mg, 4.4 mmol). The mixture was stirred until the amine disappeared. The solution was carefully neutralized with an ice cooled saturated NaHCO 3 solution. The organic layer was washed with H 2 O, dried over MgSO 4 , and concentrated to give the product (1.61 g, 88%). To the solution of the product in acetone was added one equivalent methanesulfonic acid. Then the precipitated mesylate salt was collected (1.51 g, 66%).
M.P. 234° C.
IR (KBr) cm -1 : 3400, 2950, 1630, 1600, 1490, 1455, 1240, 1210, 1195, 1060, 785, 750, 710.
1 H NMR (CDCl 3 ) δ: 8.40 (1H, br), 7.5-7.2 (10H, m), 7.17 (1H, d, J=8.4 Hz), 6.69 (1H, d, J=8.4 Hz), 6.66 (1H, br, s), 4.56 (1H, d, J=12.1 Hz), 4.25 (1H, m), 3.70-3.35 (5H, m), 3.55 (3H, s), 3.30-3.15 (2H, m), 2.46 (3H, s), 2.42 (3H, s), 2.25 (1H, m), 2.05 (1H, m), 2.00-1.60 (3H, m).
EXAMPLE 39
(2S,3S)-N-(2-Methoxy-5-methylsulfinylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Hydrochloride
A solution of (2S,3S)-N-(2-methoxy-5-methylthiophenyl)-methyl-2-diphenylmethyl-1-azabicyclo 2.2.2.!octan-3-amine (180 mg, 0.392 mmol) in MeOH (20 ml) was added to a solution of sodium periodate (NaIO 4 ) (92 mg, 0.432 mmol) in H 2 O (10 ml). The mixture was stirred for 24 hours. The precipitate (NaIO 3 ) was filtered off. The filtrate was concentrated and the residue was partitioned between H 2 O and CH 2 Cl 2 (20 ml). The water layer was extracted twice with CH 2 Cl 2 . The combined CH 2 Cl 2 was dried overd MgSO 4 and concentrated to give the sulfoxide, which was converted to HCl salt by using HCl-ether. (Yield, 180 mg, 97%).
M.P. 183° C.
IR (KBr) cm -1 : 3420, 3190, 1605, 1495, 1455, 1260, 1020, 755, 710.
1 H NMR (CDCl 3 +DMSO) δ: 8.11 (1H, br), 8.00 (1H, br), 7.70 (2H, m), 7.65 (1H, m), 7.44-7.20 (7H, m), 6.92 (1H, m), 6.48 (1H, br), 5.49 (1H, m), 4.45 (1H, br), 4.20 (2H, m), 3.95 (1H, m), 3.16 (1.5H, s), 3.12 (1.5H, s), 3.15 (2H, m), 2.80 (1.5H, s), 2.77 (1.5H, s), 2.85-2.50 (5H, m), 2.15-1.85 (2H, m).
EXAMPLE 40
(2S,3S)-N-(5-Ethylthio-2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Hydrochloride
The title compound was obtained using the same procedure as described in Example 38, except that 5-ethylthio-2-methoxybenzaldehyde was substituted for 2-methoxy-5-methylthiobenzaldehyde. The yield of the product was 76%.
M.P. 254° C.
IR (KBr) cm -1 : 3450, 3190, 2950, 1490, 1455, 1250, 1030, 715.
1 H NMR (DMSO) δ: 7.97 (1H, br), 7.68 (2H, m), 7.51 (2H, m), 7.50-6.85 (9H, m), 5.46 (2H, m), 4.25-3.30 (4H, m), 3.44 (3H, s), 3.16 (2H, m), 2.89 (2H, q, 7.3 Hz), 2.65 (1H, m), 2.30 (1H, m), 2.15-1.80 (4H, m), 1.19 (3H, t, 7.3 Hz).
EXAMPLE 41
(2S,3S)-N-(5-Trifluoroacetylamino-2-methoxyphenyl)-methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
The title compound was obtained using the same procedure as described in Example 38, except that 5-trifluoroacetylamino-2-methoxybenzaldehyde was substituted for 2-methoxy-5-methylthiobenzaldehyde. The yield of the product was 96%.
M.P. 148° C.
IR (KBr) cm -1 : 3430, 3050, 1610, 1500, 1200, 1060, 750, 710, 565.
1 H NMR (CDCl 3 ) δ: 9.50 (1H, br), 7.80 (1H, m), 7.5-7.1 (12H, m), 6.68 (1H, d, J=9.2 Hz), 4.68 (1H, m), 4.49 (1H, m), 3.80-3.50 (2H, m), 3.52 (3H, s), 3.50-3.20 (5H, m), 2.48 (3H, s), 2.42 (1H, m), 2.23 (1H, m), 1.99 (2H, m), 1.71 (1H, m).
EXAMPLE 42
(2S,3S)-N-(2-Methoxy-5-dimethylaminophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
The title compound was obtained using the same procedure as described in Example 38, except that 2-methoxy-5-dimethylaminobenzaldehyde was substituted for 2-methoxy-5-methylthiobenzaldehyde. The yield of the product was 75%.
M.P. 240° C.
IR (KBr) cm -1 : 3420, 2960, 1620, 1510, 1455, 1240, 1210, 1195, 1060, 785, 750, 710.
1 H NMR (CDCl 3 ) δ: 8.37 (1H, br), 7.45-7.20 (10H, m), 6.67 (2H, m), 6.38 (1H, m), 4.60 (1H, m), 4.23 (1H, m), 3.30-3.70 (5H, m), 3.49 (3H, s), 3.10-3.35 (2H, m), 2.86 (6H, s), 2.51 (3H, s), 2.42 (1H, m), 2.26 (1H, m), 2.15-1.50 (3H, m).
EXAMPLE 43
(2S,3S)-N-(5-Amino-2-methoxyphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
(2S,3S)-N-(5-Trifluoroacetylamino-2-methoxyphenyl)-methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (1.52 g, 3 mmol) in CH 2 Cl 2 (20 ml)/saturated NaHCO 3 (20 ml) was stirred vigorously for 8 hours. The CH 2 Cl 2 layer was washed with water, dried over MgSO 4 , and concentrated to give the title compound, which was converted to HCl salt by using HCl-ether. (Yield, 1.35 g, 81%).
M.P. 237° C.
IR (KBr) cm -1 : 3430, 2900, 1625, 1505, 1455, 1270, 1020, 755, 710.
1 H NMR (CDCl 3 ) δ: (free base) 7.45-7.05 (10H, m), 6.55 (1H, m), 6.47 (1H, m), 5.79 (1H, m), 4.50 (1H, d, 12 Hz), 3.70 (1H, m), 3.52 (3H, s), 3.50 (1H, d, 14 Hz), 3.28 (1H, d, 14 Hz), 3.20 (1H, m), 2.92 (1H, m), 2.79 (2H, m), 2.61 (1H, m), 2.04 (1H, m), 1.91 (1H, m), 1.65 (1H, m), 1.55 (1H, m), 1.28 (1H, m).
EXAMPLE 44
(2S,3S)-N-(2-Methoxy-5-methylsulfonylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine Mesylate
The title compound of Example 38 (free amine) (1.20 g, 2.62 mmol) was treated with methanolic HCl to give the hydrochloride salt. Evaporation of the solvent gave crude (2S,3S)-N-(2-methoxy-5-methylthiophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine dihydrochloride.
To a stirred and ice-cooled solution of (2S,3S)-N-(2-methoxy-5-methylthiophenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine dihydrochloride in methanol (25 mL) was added a solution of oxone (2.41 g) in water (25 mL). The reaction mixture was stirred at room temperature for 2.5 hours. The reaction mixture was basified to pH 10-11 with 1N NaOH aq. solution with ice-cooling, and extracted with CHCl 3 (80 mL×4). The combined organic layers were washed with brine (80 mL), dried (MgSO 4 ) and concentrated in vacuo to give crude (2S,3S)-N-(2-methoxy-5-methylsulfonylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (white soap, 1.49 g). The residue was purified by chromatography on silica gel (60 g) with chloroform-methanol (20:1-10:1) to give (2S,3S)-N-(2-methoxy-5-methylsulfonylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (1.08 g, 79%) as a white amorphous solid.
To a solution of (2S,3S)-N-(2-methoxy-5-methylsulfonylphenyl)methyl-2-diphenylmethyl-1-azabicyclo 2.2.2!octan-3-amine (400 mg, 0.82 mmol) in acetone (10 mL) was added methanesulfonic acid (0.41 mmol, 39.2 mg). The precipitated white solid was filtered off to give the title compound (218 mg, 30.3%, 1st crop).
M.P. 240°-241° C.
IR (KBr, free amine): 3430, 2940, 1597, 1493, 1449, 1350, 1306, 1256, 1186, 1128, 960, 820, 800, 754, 704 cm -1 .
1 H NMR (270 MHz, CDCl 3 , ppm) (free amine): 7.77 (1H, dd, J=2.6, 8.4 Hz), 7.50 (1H, d, J=2.6 Hz), 7.37-7.03 (10H, m), 6.81 (1H, d, J=8.4 Hz), 4.47 (1H, d, J=12.1 Hz), 3.71 (1H, dd, J=7.7, 12.1 Hz), 3.62 (3H, s), 3.61 (1H, d, J=13.6 Hz), 3.21 (1H, d, J=13.6 Hz), 3.28-3.10 (1H, m), 3.01 (3H, s), 2.94 (1H, dd, J=4.4, 7.7 Hz), 2.83-2.74 (2H, m), 2.63 (1H, br.t, J=11.7 Hz), 2.10-2.03 (1H, m), 1.95-1.45 (3H, m), 1.35-1.20 (1H, m).
Anal. calc'd for C 29 H 34 N 2 O 2 S.CH 3 SO 3 H.2H 2 O: C, 57.86; H, 6.80%; N, 4.50%. Found: C, 57.93%; H, 6.97%; N, 4.34%.
EXAMPLE 45
Cis-2- Diphenylmethyl)-N-((5-amino-2-methoxyphenyl)methyl)-1-azabicyclo 2.2.2!octan-3-amine
To a 50 mL round-bottomed flask equipped with Dean-Stark trap, condenser and N 2 inlet were added 430 mg (2.38 mmol) 2-methoxy, 5-nitrobenzaldehyde, 578 mg (1.98 mmol) cis-2-(diphenylmethyl)-1-azabicyclo 2.2.2!octan-3-amine, 4 mg camphorsulfonic acid, and 10 mL toluene. The reaction was refluxed with removal of water for 14 hours, then cooled and evaporated. The residue was dissolved in 10 mL tetrahydrofuran, treated with 5 ml (10 mmol) of a 2.0M solution of borane/methyl sulfide in tetrahydrofuran, and refluxed for 3 days. The reaction was then cooled and evaporated, taken up to 10 mL ethanol, treated with 1 g sodium carbonate and 1 g cesium fluoride, and refluxed for 2 days. The reaction was cooled, partitioned between water and methylene chloride, and the organic layer was separated, washed with brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using acetonitrile/water/acetic acid as eluant, and the product fractions were isolated to afford 347 mg (41%) of an amorphous solid, which crystallized from isopropanol to give M.P. 164°-169° C.
1 H NMR (δ, CDCl 3 ): 1.23 (m, 1H), 1.49 (m, 1H), 1.60 (m 1H), 1.90 (m, 1H), 2.03 (m, 1H), 2.60 (m, 2H), 2.75 (m, 2H), 2.89 (m, 1H), 3.20 (m, 1H), 3.39 (ABq, J AB =16, Δν=62, 2H), 3.51 (s, 3H), 3.66 (dd, J=8,12, 1H), 4.49 (d, J=12, 1H), 5.78 (m, 1H), 6.4-6.6 and 7.0-7.4 (m, 13H).
13 C NMR (δ, CDCl 3 ): 20.1, 24.8, 25.6, 42.1, 45.9, 49.3, 53.7, 54.3, 56.0, 61.8, 111.5, 114.0, 116.6, 125.9, 126.3, 127.6, 128.4, 129.0, 129.1, 139.7, 143.6, 145.7, 150.6.
IR (cm. -1 , KBr): 1620 and 1580.
MS (%): 428 (parent+1, 1), 291 (22), 260 (100), 136 (54), 106 (23).
Anal. calc'd for C 28 H 33 N 3 O: C 78.65, H 7.78, N 9.83. Found: C 78.73, H 7.87, N 9.71.
The title compounds of Example 46 to 58 were prepared by a procedure similar to that described in Example 9.
EXAMPLE 46
(5-Isopropylsulfonyl-2-methoxybenzyl)-(2-phenylpiperidin-3-yl)amine dihydrochloride
17% yield, m.p. 278°-280° C. (dec.).
MS: m/e 402 (M + ), 398, 283, 275.
1 H NMR (CDCl 3 , free base) δ1.25 (dd, 6H), 1.35-2.2 (m, 6H), 2.8 (m, 2H), 3.15 (m, 1H), 3.25 (d, 1), 3.35 (d, 1H), 3.5 (s, 3H), 3.65 (d, 1H), 3.9 (d, 1H), 6.75 (d, 1H), 7.25 (m, 5H), 7.55 (s, 1H), 7.65 (dd, 1H).
Anal. calc'd for C 22 H 30 N 2 O 3 S.2HCl: C, 55.57; H, 6.78; N, 5.89. Found: C, 55.24; H, 6.54; N, 5.87.
EXAMPLE 47
N-Cyclopentyl-N- 4-methoxy-3-(2-phenylpiperidin-3-ylaminomethyl)phenyl!methanesulfonamide dihydrochloride hemihydrate
30% yield, m.p. 249°-252° C.
FABMS: m/e 458 (M +1 , 100%), 282 (10), 160 (55%).
1 H NMR (CDCl 3 , free base) δ1.25-1.65 (m, 8H), 1.75-2.05 (m, 5H), 2.15 (d, 1H), 2.8 (m, 2H), 2.9 (s, 3H), 3.25 (d, 1H), 3.35 (d, 1H), 3.5 (s, 3H), 3.7 (d, 1H), 3.9 (d, 1H), 4.45 (m, 1H), 6.65 (d, 1H), 6.9 (d, 1H), 7.05 (dd, 1H), 7.25 (m, 5H).
Anal. calc'd for C 25 H 35 N 3 O 3 S.2HCl.1/2H 2 O: C, 55.65; H, 7.10; N, 7.79. Found: C, 55.69; H, 6.55; N, 7.78.
EXAMPLE 48
N-Cyclohexylmethyl-N- 4-methoxy-3-(2-phenylpiperidin-3-ylaminomethyl)phenyl!methanesulfonamide dihydrochloride hydrate
21% yield, m.p. 255°-256° C. (dec.).
FABMS: m/e 486 (M +1 ), 408.
1 H NMR (CDCl 3 , free base) δ0.9-2.2 (m, 17H), 2.7-2.9 (m, 5H), 3.2-3.5 (m, 5H), 3.5 (s, 3H), 3.6 (d, 1H), 3.7 (d, 1H), 3.9 (d, 1H), 6.7 (d, 1H), 7.0 (d, 1H), 7.3 (dd, 1H), 7.4 (m, 5H).
Anal. calc'd for C 27 H 39 N 3 O 3 S.2HCl.3/4H 2 O: C, 56.68; H, 7.49; N, 7.34. Found: C, 56.63; H, 7.11; N, 7.59.
EXAMPLE 49
(5-Methoxy-2-methyl-1-methylsulfonyl-2,3-dihydro-1H-indol-6-ylmethyl)-(2-phenylpiperidin-3-yl)amine dihydrochloride
16% yield, m.p. 257°-259° C.
FABMS: me 430 (M +1 , 10%), 254 (100%).
1 H NMR (CDCl 3 , free base) δ1.45 (dd, 3H), 1.65 (t, 1H), 1.8-2.2 (m, 4H), 2.6 (m, 1H), 2.75 (d, 3H), 2.85 (m, 1H), 3.3 (m, 1H), 3.4 (d, 3H), 3.45 (m, 1H), 3.65 (m, 1H), 3.9 (d, 1H), 4.4 (m, 1H), 6.55 (d, 1H), 7.15 (d, 1H), 7.25 (m, 5H).
Anal. calc'd for C 23 H 31 N 3 O 3 S.2HCl: C, 54.97; H, 6.22; N, 8.36. Found: C, 54.76; H, 6.45; N, 8.20.
EXAMPLE 50
1- 5-Methoxy-6-(2-phenylpiperidin-3-ylaminomethyl)-2,3-dihydroindol-1-yl!-heptan-1-one dihydrochloride hemihydrate
7% yield, m.p. 170°-172° C.
FABMS: m/e 450 (M +1 , 100%), 274, 160.
1 H NMR (CDCl 3 , free base ) δ0.9 (t, 3H), 1.25-1.45 (m, 6H), 1.5-1.8 (m, 3H), 1.85-2.25 (m, 4H), 2.4 (t, 2H), 2.8 (m, 2H), 3.15 (t, 2H), 3.25 (m, 1H), 3.3 (s, 3H), 3.35 (d, 1H), 3.7 (d, 1H), 3.9 (d, 1H), 4.05 (t, 2H), 6.5 (s, 1H), 7.25 (m, 5H), 8.0 (s, 1H).
Anal. calc'd for C 28 H 3 N 3 O 2 .2HCl.1/2H 2 O: C, 63.27; H, 7.96; N, 7.90. Found: C, 63.33; H, 8.51; N, 8.19.
EXAMPLE 51
2,4-Dimethylthiazole-5-sulfonic acid 4-methoxy-3-(2-phenylpiperidin-3-ylaminomethyl)phenyl!-methylamide dihydrochloride hemihydrate
24% yield, m.p. 260°-264° C.
1 H NMR (CDCl 3 , free base) δ1.3-2.0 (m, 5H), 2.05 (d, 1H), 2.15 (s, 3H), 2.7 (s, 3H), 2.8 (m, 2H), 3.15 (s, 3H), 3.25 (d, 1H), 3.35 (d, 1H), 3.45 (s, 3H), 3.6 (d, 1H), 3.85 (d, 1H), 6.55 (d, 1H), 6.8 (d, 1H), 6.95 (dd, 1H), 7.25 (m, 5H).
Anal. calc'd for C 25 H 32 N 4 O 3 .2HCl.1/2H 2 O: C, 51.54; H, 6.06; N, 9.62. Found: C, 51.31; H, 5.79; N, 9.76.
EXAMPLE 52
N-(4,5-dimethylthiazol-2-yl)-N- 4-methoxy-3(2-phenylpiperidin-3-ylaminomethyl)phenyl!methanesulfonamide dihydrochloride hemihydrate
40% yield, m.p. 247°-249° C.
FABMS: m/e 501 (M +1 ), 421, 381, 247 (100%).
1 H NMR (CDCl 3 , free base) δ1.4 (d, 1H), 1.6 (t, 1H), 1.75 (m, 2H), 1.9 (m, 1H), 2.15 (d, 1H), 2.3 (m, 6H), 2.85 (m, 2H), 3.25 (d, 1H), 3.35 (d+s, 4H), 3.55 (s, 3H), 3.7 (d, 1H), 3.9 (d, 1H), 6.7 (d, 1H), 7.15 (d, 1H), 7.25 (m, 6H).
Anal. calc'd for C 25 H 32 N 4 O 3 S 2 .2HCl.1/2H 2 O: C, 51.54; H, 6.06; N, 9.62. Found: C, 51.87; H, 5.81; N, 9.55.
EXAMPLE 53
{5- (4,5-dimethylthiazol-2-yl)methylamino!-2-methoxybenzyl}-(2-phenylpiperidin-3-yl)amine trihydrochloride hydrate
26% yield, m.p. 220°-225° C.
MS: m/e 436 (M + , 16%), 317 (45%), 262 (100%).
1 H NMR (CDCl 3 , free base) δ1.5 (m, 1H), 1.6 (m, 1H), 1.9 (m, 1H), 2.1 (s, 3H), 2.2 (s, 3H), 2.8 (m, 2H), 3.2 (m, 1H), 3.3 (s, 3H), 3.4 (d, 1H), 3.5 (s, 3H), 3.6 (d, 1H), 3.9 (d, 1H), 6.4 (d, 1H), 6.9 (d, 1H), 7.1 (q, 1H), 7.4 (m, 5H).
Anal. calc'd for C 25 H 32 N 4 OS.HCl.3/2H 2 O: C, 52.40; H, 6.68; N, 9.78. Found: C, 52.12; H, 6.64; N, 9.55.
EXAMPLE 54
{5- (4,5-dimethylthiazol-2-ylamino)-2-methoxybenzyl}-(2-phenylpiperidin-3-yl)amine trihydrochloride
28% yield, m.p. 272°-275° C.
MS: m/e 422 (M + , 40%), 303 (54%), 248 (100%).
1 H NMR (CDCl 3 , free base) δ1.35-2.15 (m, 7H), 2.18 (s, 3H), 2.23 (s, 3H), 2.8 (m, 2H), 3.28 (d, 1H), 3.4 (d, 1H), 3.5 (s, 3H), 3.65 (d, 1H), 3.9 (d, 1H), 6.65 (d, 1H), 6.75 (d, 1H), 7.15 (dd, 1H), 7.3 (m, 5H).
Anal. calc'd for C 24 H 30 N 4 OS.3HCl: C, 54.19; H, 6.25; N, 10.53. Found: C, 53.91; H, 6.39; N, 10.27.
EXAMPLE 55
{ 4-Methoxy-3-(2-phenylpiperidin-3-ylaminomethyl) phenyl!-methyl-sulfamoyl}-acetic acid ethyl ester
48% yield, m.p. 245°-248° C.
MS: m/e 475 (M + , 5%) 356, 175, 150 (100%).
1 H NMR (CDCl 3 , free base) δ1.3 (t, 3H), 1.3502.15 (m, 6H), 2.8 (m, 2H), 3.3 (d, 1H), 3.35 (s, 3H), 3.4 (d, 1H), 3.5 (s, 3H), 3.65 (d, 1H), 3.9 (d, 3H), 4.3 (q, 2H), 6.7 (d, 1H), 7.15 (d, 1H), 7.35 (m, 6H).
EXAMPLE 56
2-Hydroxyethanesulfonic acid 4-methoxy-3-(2-phenylpiperidin-3-ylaminomethyl)phenyl!-methylamide hydrochloride
4% yield, m.p. 255°-260° C. (dec.).
MS: m/e (433, M + ), 314 (85%), 258 (100%).
1 H NMR (CDCl 3 , free base) δ2.55 (bs, 4H), 2.75 (t, 1H), 2.85 (m, 1H), 3.15 (t, 2H), 3.2 (s, 3H), 3.35 (d, 1H), 3.5 (s, 3H), 3.65 (d, 1H), 3.9 (d, 1H), 3.95 (t, 2H), 6.65 (d, 1H), 7.1-7.4 (m, 7H).
Anal. calc'd for C 22 H 31 N 3 O 4 S.HCl: C, 52.17; H, 6.57; N, 8.29. Found: C 51.89, N 6.27, N 7.95.
EXAMPLE 57
N-(3,4-Dichlorobenzyl)-N- 4-methoxy-3-(2-phenylpiperidin-3-ylaminomethyl)phenyl!-methanesulfonamide dihydrochloride hydrate
13% yield, m.p. 240°-243° C. (dec.).
MS: m/e 548 (M +1 , 8%), 428 (30), 159 (100).
1 H NMR (CDCl 3 , free base) δ1.35-2.15 (m, 6H), 2.65 (m, 1H), 2.8 (t, 1H), 2.85 (s, 3H), 3.25 (d, 1H), 3.35 (d, 1H), 3.5 (s, 3H), 3.65 (d, 1H), 3.9 (d, 1H), 4.65 (q, 2H), 6.6 (d, 1H), 6.9 (d, 1H), 7.0 (dd, 1H), 7.15 (dd, 1H), 7.2-7.4 (m, 7H).
Anal. calc'd for C 27 H 31 Cl 2 N 3 O 3 S.1HCl.2/3H 2 O: C, 51.19; H, 5.46; N, 6.63. Found: C, 51.17; H, 5.33; N, 6.48.
EXAMPLE 58
4,5-Dimethylthiazole-2-sulfonic acid methyl- 3-(2-phenylpiperidin-3-yl-aminomethyl)-4-trifluoromethoxyphenyl!-amide trihydrochloride hydrate.
12% yield, m.p. 239°-240° C. (dec.),
MS: m/e 555 (M +1 ), 380.
1 H NMR (CDCl 3 , free base) δ1.5 (m, 1H), 1.7 (m, 1H), 1.9 )m, 4H), 2.1 (m, 1H), 2.2 (s, 3H), 2.7 (s, 3H), 2.8 (m, 2H), 3.2 (S,3H), 3.3 (m, 1H), 3.5 (q, 2H), 3.9 (d, 1H), 7.0 (m, 3H), 7.2 (m, 5H).
Anal. calc'd for C 25 H 29 F 3 N 4 O 3 S 2 .3HCl.H 2 O: C, 44.09; H, 4.88; N, 8.23. Found: C, 44.36; H, 4.95; N, 8.51.
The title compounds of examples 59-62 were prepared by a procedure similar to that of Example 38C, starting with the appropriate aldehyde in place of 2-methoxy-5-methylthiobenzaldehyde.
EXAMPLE 59
(2S,3S)-3- 2-Methoxy-5-(N-acethyl-N-methylamino)benzyl-amino!-2-diphenylmethyl-1-azabicyclo 2.2.2!octane dihydrochloride
M.p.: 232°-234° C. (AcOEt).
IR(KBr): 3430, 3055, 3020, 1648, 1500, 1386, 1244, 709 cm -1 .
1 H NMR (270 MHz, CDCl 3 , free amine): 7.36-7.07 (m, 10H), 6.95 (dd, J=8.6, 2.6 Hz, 1H), 6.71 (d, J=8.6 Hz, 1H), 6.37 (d, J=2.6 Hz, 1H), 4.49 (d, J=12.1 Hz, 1H), 3.78-3.71 (m, 1H), 3.65-3.60 (m, 1H), 3.63 (s, 3H), 3.28-3.23 (m, 2H), 3.20 (s, 3H), 2.93 (dd, J=7.7, 4.4 Hz, 1H), 2.81 (m, 2H), 2.68 (m, 1H), 2.04 (m, 1H), 1.82 (s, 3H), 1.95-1.29 (m, 5H).
EXAMPLE 60
(2S,3S)-3- 2-Methoxy-5-(N-methyl-N-trifluoroacetylamino)benzylamino!-2-diphenylmethyl-1-azabicyclo 2.2.2!octane dihydrochloride
1 H NMR (270 MHz, CDCl 3 , ppm) (free amine): 7.38-7.04 (m, 10H), 7.01 (dd, J=2.6, 8.8 Hz, 1H), 6.69 (d, J=8.8 Hz, 1H), 6.42 (br.s, 1H), 4.48 (d, J=12.1 Hz, 1H), 3.77-3.55 (m, 2H), 3.61 (s, 3H), 3.44-3.15 (m, 2H), 3.28 (s, 3H), 2.89 (dd, J=4.0, 7.7 Hz, 1H), 2.86-2.60 (m, 3H), 2.05-1.82 (m, 2H), 1.75-1.40 (m, 2H), 1.38-1.20 (m, 1H).
IR (KBr, cm -1 ) (free amine): 3360, 1699, 1598, 1499, 1465, 1451, 1248, 1203, 1150, 1112, 1071, 1038, 817, 754, 703.
EXAMPLE 61
(2S,3S)-3- 5-(N-Isopropyl)-N-methylsulfonylamino)-2-methoxybenzylamino!-2-diphenylmethyl-1-azabicyclo 2.2.2!octane dihydrochloride
M.p.: 178°-179° C.
1 H NMR (270 MHz, CDCl 3 , ppm) (free amine): 7.34-7.03 (m, 10H), 7.07 (dd, J=2.6, 8.8 Hz, 1H), 6.82 (d, J=2.6 Hz, 1H), 6.68 (d, J=8.8 Hz, 1H), 4.53 (sep, J=6.6 Hz, 1H), 4.49 (d, J=12.1 Hz, 1H), 3.76-3.63 (m, 1H), 3.62 (d, J=13.6 Hz, 1H), 3.53 (s, 3H), 3.30-3.13 (m, 1H), 3.23 (d, J=13.6 Hz, 1H), 2.97-2.86 (m, 1H), 2.93 (s, 3H), 2.84-2.58 (m, 3H), 2.11-2.02 (m, 1H), 2.00-1.40 (m,4H), 1.38-1.20 (m, 1H), 1.15 (dd, J=2.6, 6.6 Hz, 6H).
IR (KBr, cm -1 ) (free amine): 3340, 1603, 1495, 1462, 1450, 1366, 1332, 1232, 1181, 1154, 1130, 1107, 1032, 982, 961, 815, 801, 755, 703.
EXAMPLE 62
(2S , 3S)-3- 2-Methoxy-5-(N-methyl-N-methylsulfonylamino)benzylamino!-2-diphenylmethyl-1-azabicyclo 2.2.2!octane monomethanesulfonate
M.p.: 197°-203° C. (IPA-Hex).
IR (KBr): 3430, 2945, 1500, 1340, 1218, 1166, 1039, 746 cm -1 .
1 H NMR (270 MHz, CDCl 3 , free amine): 7.35-7.07 (m, 11H), 6.82 (d, J=2.6 Hz, 1H), 6.68 (d, J=8.8 Hz, 1H), 4.49 (d, J=12.1 Hz, 1H), 3.76-3.67 (m, 1H), 3.61-3.53 (m, 1H), 3.54 (s, 3H), 3.26 (s, 3H), 3.26-3.18 (m, 2H), 2.93 (dd, J=7.7, 4.0 Hz, 1H), 2.83 (s, 3H), 2.82-2.77 (m, 2H), 2.65 (m, 1H), 2.06 (m, 1H), 1.91-1.55 (m, 4H), 1.34-1.23 (m, 1H).
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The present invention relates to novel substituted benzylamino nitrogen containing non-aromatic heterocycles and, specifically, to compounds of the formula ##STR1## wherein W, R 1 , R 2 , R 3 and A are as defined in the specification, and to intermediates used in the synthesis of such compounds. The novel compounds of formula I are useful in the treatment of inflammatory and central nervous system disorders, as well as other disorders.
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RELATED APPLICATIONS
[0001] This application claims priority under 35 U.S.C. §119 based on U.S. Provisional Application No. 60/975,666, filed Sep. 27, 2007, the disclosure of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] A. Field of the Invention
[0003] The present invention relates to amusement games such as pinball and pachinko machines and, more specifically, to dynamically altering playfield elements.
[0004] B. Description of Related Art
[0005] As is well known, pinball games typically comprise an inclined playfield mounted in a game cabinet and supporting a rolling ball. Players control the game ball with flippers to score points by projecting the ball towards game features, such as targets, bumpers, and the like. Conventional pinball games provide the player with a predetermined number of game balls that are played on the game playfield.
[0006] Over the years pinball machines have lost space in arcades and location-based entertainment centers to video arcade games. In 1931 Baffle Ball (D. Gottlieb & Co.) sold 50,000 units. That same year Ballyhoo (Bally Mfg.) sold 75,000 units. In contrast, the only surviving pinball manufacturer Stern Pinball is “striving towards 10,000 machines a year.” One of the major reasons for this decline is game-play time. Video arcade games have an operator-settable game-play time. Pinball game-play time is typically solely related to a player's skill.
[0007] Pinball games derive their appeal from the challenge they present to game players. Players are rewarded for skillful play with bonuses, extended game play, and free games. Usually, skillful play requires a significant investment of game time and expense before the new player becomes familiar with the particular scoring scheme and game features and develops the eye-hand coordination to control the ball and hit the desired targets. Game appeal thus depends on a player's willingness to learn the game. Often, a novice player with little skill and experience will quickly drain all of the game balls and experience an unexciting, short-lived game play. He or she may become intimidated and quickly lose interest in that particular pinball game or in pinball games in general. Thus, in order to permit players to develop their skills and maintain interest in a particular pinball game, it is desirable to provide new players with the option to learn and master a particular pinball game at a more reasonable cost. At the same time, the skilled player may become bored with a game that is “too” easy and doesn't provide enough challenge to keep him interested.” (Sullivan, U.S. Pat. No. 5,707,059)
[0008] As a gamer becomes skilled with a particular pinball machine, his game-play time increases. This decreases potential revenue from a machine. All amusement games are often subject to a queue. One skilled individual may tie up a pinball machine for 30 minutes or more, on one play. Unlike waiting to play a video arcade machine, the wait for a pinball machine may be long and variable, thus causing an individual to lose interest in a particular machine or in pinball in general.
[0009] One method of adjusting a pinball machine's difficulty is the position of posts. Many machines were built with multiple positions for posts. For example, a post near an out-hole typically has three positions, conservative, medium and liberal. ( FIG. 3 ) The position of this post determines how likely a pinball would exit through the out-hole or bounce back into the playfield. Thusly the machine's difficulty level could be set, but only by a trained operator while the machine was being serviced.
[0010] One solution to the problem of pinball game-time being to short is addressed by Sullivan, et. al. U.S. Pat. No. 5,707,059 that teaches a “novice” mode where game-time is determined by a timer and not by a pre-determined number of balls. Sheats, Jr. U.S. Pat. No. 6,149,153 teaches helping novices by having the processing circuit activate a flipper, to show the novice where the “money” shots are and to help his or her score. However this solution changes fundamental game play.
[0011] Accordingly, there is a need for dynamically altering pinball playfield elements for the purpose of controlling game-play time while not significantly changing the conventional gaming experience.
SUMMARY OF THE INVENTION
[0012] The present invention teaches dynamically altering pinball playfield elements. Two broad categories are discussed:
Physically moving a playfield component, such as a bumper, and Changing the force of a playfield component, such as an angle bumper kicker or flipper.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate the invention and, together with the description, explain the invention. In the drawings,
[0016] FIG. 1 is a representation of a playfield with a hole drilled in it.
[0017] FIG. 2 is a representation of an angle bumper at multiple angles.
[0018] FIG. 3 is an image showing “Meteor” playfield parts.
[0019] FIG. 4 is an image showing “Meteor” playfield parts with playfield parts that could be adjusted by the methods taught in the current invention marked.
DETAILED DESCRIPTION
[0020] The following detailed description of the invention refers to the accompanying drawings. The same reference numbers in different drawings identify the same or similar elements. Also, the following detailed description does not limit the invention. The term processor is used for convenience and does not imply a specific type of microcontroller. Circuitry may be used to produce processor like functions.
[0021] The following description describes a basic embodiment of our invention.
[0022] There are a number of different playfield elements that may be dynamically altered in order to affect game play in a pinball machine. As previously mentioned, early attempts at modifying game play required operator intervention and skilled technicians in order to make the change (see FIG. 3 ).
[0023] The present invention creates playfield elements that may be dynamically changed as a game is being played. These elements may be controlled by the computer tasked with operating the pinball machine or they may be changed based on sensor data of the element itself.
[0024] For the sake of this discussion, we will be talking at length about the angle bumpers typically found near the flippers at the bottom of the playfield. The term solenoid is used to describe the actuator typically used to impact a ball, but the invention is in no way limited to this device. In a typical pinball machine, a mechanical switch is positioned just behind the rubber bumper to determine when the ball has come in contact with the bumper. The switch closure is used either directly or indirectly to apply power to the solenoid that will propel the ball away from the bumper.
[0025] The present invention does not require any coupling between the switch and the solenoid, meaning that the switch has no restrictions as to its ability to carry power. As such, the switch is not limited to being a mechanical switch, but may be optical, hall effect, or even a virtual switch. Examples of a virtual switch would include the ball position determined by video analysis or an array of sonar transducers on the playfield.
[0026] Given that the switch or imminent contact information is not used directly to power the solenoid, the machine's processor controls the amount of power applied to the solenoid. This allows for a significant change in the way that the bumper works. With a mechanical switch, a glancing strike on the bumper would cause only a low power response from the solenoid, as the ball would not be in contact with the switch for long. With the present invention, a full power stroke may be applied to the solenoid, giving the ball more of a kick than would be expected. Conversely, if the processor decides to make a bumper “dead”, it can give a very low power kick even in the case of a solid hit on the switch.
[0027] Additionally, the present invention is not restricted to being fully reactive as is a typical pinball machine. Using sensors and taking advantage of the onboard processing abilities, the machine may be proactive in its response to the ball. For instance, if the machine determines that the ball will shortly strike one of the angle bumpers, it can send the solenoid in motion in advance of the ball reaching the bumper. This allows for a more powerful kick using the same solenoid. In a mechanical system, by the time the solenoid is in motion, the ball has already begun to slow. By predicting the impact, the optimal impact timing and velocity can be chosen by the processor.
[0028] Another benefit of decoupling the switch from the actuator is that the angle bumper can be set to “catch” the ball. A common technique of pinball players is to catch the ball on a flipper by raising the flipper, and releasing the flipper button as the ball strikes it. When done properly, the ball does not bounce off the flipper, it stops on the flipper. This same technique can be programmed into the angle bumper. As the ball approaches, the solenoid is extended. When the imminent impact with the bumper is detected, the solenoid is released. Depending on the tension of the rubber band around the angle bumper, another solenoid may be used to pull back the bumper's rubber, increasing the stopping power of the bumper. Similarly, a solenoid may be used to release the tension on the bumper's rubber. Once caught, the ball may be kicked back into play or allowed to drop at the discretion of the processor.
[0029] In the preceding example we touched on the benefits of being able to adjust the power to a given solenoid under processor control. This also applies to the solenoid that drives the flippers. When the player presses a flipper button, power is typically directly coupled from the button to the solenoid. If the player taps the button, the flipper will have just a light bounce. If the player holds the button, the flipper will have full power and remain in the extended position. In the current invention, the processor may decide to decouple the flipper buttons and the flipper solenoids. This allows a great amount of flexibility in dynamically changing game play. By changing the amount of time that power is applied to the solenoid when a flipper button is pressed, the processor can increase or decrease the strength of the flippers. The processor can also release the flippers after a specific amount of time, preventing the player from holding onto a ball forever. One skilled in the art would understand that these techniques would give the processor an unprecedented amount of control over aspects of game play that had formerly been passive.
[0030] The present invention is not limited to adjusting the power of the standard elements on the pinball playfield, it also provides for dynamically moving playfield elements. Going back to the angle bumper example, many older pinball machines had multiple holes drilled into the playfield in the area where a post may be positioned (see FIG. 3 ). A technician could modify the game's difficulty by moving the post to one of the other positions.
[0031] FIG. 2 is a representation of an angle bumper. In this example the angle bumper may be at an angle of 45 degrees 201 or an angle of 50 degrees 202 . With proper game design, changing the angle of an angle bumper can affect game play, with one setting harder than another. Alone or in combination with changing the force of the kicking mechanism associated with the angle bumper, gameplay difficulty can be adjusted.
[0032] In pinball games such as “Klondike” and “Heat Wave” a pinball can drain in the space between the angle bumper and the edge of the playfield. On machines such as these an angle bumper at 45 degrees would have a smaller space for a ball to drain than an angle bumper at 50 degrees.
[0033] Three are three broad categories to consider when moving features on a pinball machine:
Stability Positioning Cost
[0037] Stability. A feature that is moved must not be knocked out of position by a pinball striking it. To this end a feature may be attached to a motor with a worm gear, or a feature may be mounted to a plate and the plate with feet for stability, the plate moved by an actuator, among other methods known in the art. Additionally the feature or plate may use pins to help stabilization.
[0038] Positioning. For exact positioning a system of pins described below can be used. Additionally physical blocks can be used to stop plate movement, help stabilize and position. Other systems include using a stepper motor, a worm gear, among other methods known in the art.
[0039] Cost. Cost both in production and cost of maintenance must be considered. For example most pinball playfield features could be moved with a heavy motor driving a worm gear. However in moving a single post such as 409 this would be overkill. A single post could be more economically moved by a system such as one using muscle wires. Additionally bell cranks and similar devices known in the art may be used to multiply the force of an actuator.
[0040] The current invention allows the processor to change the position of bumpers during game play. In one embodiment, a motor with a worm gear is attached to the playfield and is used to move the post on an angle bumper. A slot is milled in the playfield allowing the post to travel a short but significant distance. The position of the post may be determined in any number of ways, ranging from using a stepper motor and counting the steps moved to using standard servo feedback techniques. Additionally, end of travel switches may be used to avoid overdriving the motor.
[0041] In another embodiment, muscle wire is used to move the post from one location to the next. Motors are preferable in some situations due to the flexibility in positioning that they provide, but muscle wire provides a very low cost way to occasionally move a post.
[0042] An actuator would not necessarily be connected directly to a post, but could attach to a plate to which the post is attached. The plate can have additional support hardware underneath the playfield to give the post the necessary rigidity for pinball play while allowing for smooth movement. This support could include Teflon coated “feet” to allow for stability and ease of motion.
[0043] In another embodiment, holes are drilled into the playfield 101 corresponding to desired stopping location for the motion plate. A spring loaded pin 102 is used to secure the plate to the hole. When the plate is to be put into motion, muscle wire is used to raise the pin out of its hole, the plate moves, and the muscle wire releases the pin. This allows for a way to strongly secure the plate when it reaches a predetermined stopping point. In another embodiment, the holes that are used for the pin are filled with an insert harder than wood, typically of metal, that is wider on the top narrowing down to a close fit for the pin 103 . This insert makes it easier for the pin to hit the hole and reduces wear on the playfield.
[0044] One skilled in the art would appreciate that these techniques can be used with many of the elements typically found on pinball machines. Using the same techniques taught above, many features can be adjusted to have an impact on game play. For some examples, please refer to FIG. 4 . 401 - 412 are examples of posts that can be moved to change game play. 420 is a flipper whose angle relative to the drop target bank above it could be changed. 430 is a pop bumper that could be moved to affect game play.
[0045] With the proper application of these techniques, a pinball machine is changed from being a passive, reflexive device to one that has an active playfield. With so many elements under the control of the machines processor, it is possible to have the machine interact with the player in ways that were never before possible. Please see U.S. patent application “SYSTEMS AND METHODS FOR ADJUSTING GAME-PLAY TIME OF PINBALL MACHINES” by the inventors.
[0046] No element, act, or instruction used in the description of the present application should be construed as critical or essential to the invention unless explicitly described as such. Also, as used herein, the article “a” is intended to include one or more items. Where only one item is intended, the term “one” or similar language is used.
[0047] The scope of the invention is defined by the claims and their equivalents.
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The present invention teaches systems and methods to dynamically alter pinball playfield elements. The key observation is that these systems and methods are organic to conventional pinball play, and thus acceptable to a typical pinball player. The present invention has two broad components under control of a game's processor. One, physically moving a playfield component such as a bumper, and two, changing the force of a playfield component, such as an angle bumper kicker or flipper.
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TECHNICAL FIELD
[0001] The method and the system relate to the field of body toning and in particular to the field of management and operation of body toning devices.
BACKGROUND
[0002] External appearance is of concern practically to every person. In recent years, methods and apparatuses have been developed for different skin toning and cosmetic treatments. Among these methods and apparatuses are hair removal, treatment of vascular lesions, wrinkle removal, body shaping, fat removal or reduction and skin rejuvenation. In these treatments a volume of skin or tissue to be treated is heated to a temperature that is sufficiently high as to achieve a desired effect. Such temperature is typically in the range of 38-60 degrees Celsius.
[0003] One method that has been used for heating the skin is application to the skin of pulsed or continuous radio-frequency (RF) energy. In this method, electrodes are applied to the skin and an RF voltage in continuous or pulse mode is applied across the electrodes. The properties of the RF voltage are selected so as to generate an RF current in the tissue to be treated, current which heats the tissue to the required temperature.
[0004] Concurrently, a number of light based skin surface or deeper skin layer treatments have been developed. These treatments usually employ a laser, a LED, a Xenon lamp (Intense Pulsed Light or IPL) or incandescent lamp radiation to expose a surface of skin where vascular lesions, varicose veins, acne, mole marks and similar disorders are present. The optical radiation may be of a single wavelength or include several wavelengths. The wavelengths are selected to be optimal for the color of the contrasted component of the target, and are typically in the range of 400 to 1800 nm.
[0005] Reduction of subcutaneous fat layers, or adipose tissue, is another skin treatment for which there is a growing demand. Among the different physical therapies available, the application of ultrasound is emerging as another adipose tissue removal and body shaping technology. Methods associated with this technology are based on the delivery of a dose of electromagnetic energy (RF) or ultrasound waves through the skin of a recipient into the subcutaneous adipose tissue to a volume of tissue to be treated.
[0006] The above described equipment is both costly and bulky, and it is typically operated in an ambulatory set-up by a qualified operator and frequently requires presence of medical personnel specialized in such treatments or toning. Recently, equipment allowing application of any one of the listed above treatments or a combination of them by a non-professional person in a conventional residential setting has been developed. When such equipment is in use, the user has no means for tracking the toning progress, select most appropriate for him/her tissue affecting energy parameters, apply the energy in the most effective way to the segments of tissue to be treated or toned.
[0007] There is a need for an integrated system that would collect the toning process parameters related to the application of tissue affecting energy to the user skin or tissue, analyze it, and recommend to the user current toning session tissue affecting energy parameters. There is also a need in a device capable of collecting such data and communicating it to the system as well as receiving and operating according to the recommended tissue affecting energy parameters.
BRIEF SUMMARY
[0008] The problem of tracking the toning history of a person (subject) and determining parameters of the current toning session can be solved by recording and storing into the memory of a toning device, or a computer or some other processing device, parameters of each of the preceding tissue toning procedures, as well as segments of the subject body affected by such toning procedures. Next, the recorded data can be analyzed and one or more protocols related to the current tissue toning session can then be derived. Concurrently, with the protocol, recommendations on skin care options, new products adapted for skin care and complementary to the skin/tissue toning, and any other skin care news that may be relevant to the subject skin care can be identified and provided.
GLOSSARY
[0009] The terms “tissue” or “skin” as used in the present disclosure have the same meaning and are used interchangeable through the text of the disclosure.
[0010] The term “tissue affecting energy” as used in the present disclosure means energy capable of causing a change in the tissue, or enabling such change. Such energy for example, may be RF energy, optical radiation in visible or invisible part of electromagnetic spectrum, ultrasound waves energy, and kinetic energy provided by a massaging device.
[0011] The term “tissue toning device” as used in the present disclosure means any device providing energy affecting the tissue. Such device for example, may apply to the tissue RF energy, optical radiation existing in the visible or the invisible part of spectrum, ultrasound waves energy, kinetic energy provided by a massaging device or some other source of energy.
[0012] The term “tissue toning” as used in the present disclosure includes operations that provide, among other things, skin rejuvenation treatment, cellulite management treatment, body contouring procedures, acne treatment procedures, hair removal, and other skin or tissue treatments.
[0013] The term “current tissue toning protocol” means a protocol according to which the immediate tissue toning will be performed.
[0014] The term “terminations” and “terminations configured to couple energy to the tissue” as used in the present disclosure includes electrodes that couple RF energy to the tissue, transducers that couple ultrasound waves to the tissue, windows, lenses, and optical waveguides that facilitate skin by optical radiation exposure, and rollers or balls of the massaging device that couple kinetic energy to the skin, as well as similar devices that are able to communicate energy from a source to the tissue.
[0015] The term “computer” as used in the present disclosure means a device capable of receiving data or information, processing it, and delivering the data processing results to another device. As such, a computer may include, as non-limiting examples, a personal computer, a PDA computer, a mobile telephone, and similar devices. Typically, a computer as defined herein would have a display but, other forms of user feedback, prompting and user interface may also be used such a sound, voice detection, brail screens, or the like.
[0016] As used herein, the terms “person” and “subject” have the same meaning and refer to any human or animal subject, as well as synthetic objects.
[0017] As used herein, the terms “optical radiation sources” and “optical radiation emitters” have the same meaning and refer to any source or emitter of visible or non-visible optical radiation.
[0018] The terms “treatment” or “toning” as used in the present disclosure have the same meaning and are used interchangeable through the text of the disclosure.
[0019] The term “video” as used in the pressed disclosure is related to the visual presentation of information, usually on a display screen.
BRIEF LIST OF DRAWINGS
[0020] For a better understanding of the system and the method, reference is made to the following description, taken in connection with the accompanying drawings, in which like reference characters refer to the same parts throughout the different views. The drawings are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the method and/or apparatus.
[0021] FIG. 1 is a schematic illustration of an exemplary embodiment of the present system for personal tissue toning.
[0022] FIG. 2 is a schematic illustration of an exemplary computer display indicating locations of desired tissue affecting energy coupling.
[0023] FIG. 3A is a schematic illustration of an exemplary embodiment of the present tissue toning device.
[0024] FIG. 3B is a schematic illustration of the bottom view of an exemplary embodiment of the tissue toning device of FIG. 3A .
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0025] In the following detailed description, reference is made to the accompanying drawings that form a part hereof and wherein like reference numerals denote like elements through the several views.
[0026] Reference is made to FIG. 1 which is an exemplary embodiment of a personal tissue toning system. System 100 includes a tissue toning device 104 , a computer 108 with a display 112 , and a data transmission link 116 operative to transmit bi-directionally data between tissue toning device 104 and computer 108 . The data transmission link 116 is shown as being a physical connection but, it will be appreciated that the connection may be wireless or optical as well. Computer 108 , which will be termed the local computer may be of a variety of devices such as a personal computer, a palm computer, or a mobile telephone as non-limiting examples. Practically, any device having a processor and capable of processing data may be used in place of computer 108 . Computer 108 is configured to communicate with a memory device or component 134 of tissue toning device 104 with the help of interface 138 and may be programmed to receive (or read) from memory 134 of device 104 the historical toning data accumulated in memory 134 , analyze the historical toning data and issue a current tissue toning protocol. It should also be appreciated that the tissue toning device 104 may also include an embedded processing unit, for instance memory device 134 may be a microcontroller, and the processing unit may perform some or all of the analysis of the historical toning data and/or issue a current tissue toning protocol. Thus, the processing unit may be internal to the toning device 104 , external in a computer or distributed between the two. The current tissue toning protocol optionally may include a video or virtual user image and suggestions for complementary skin care elements such as the use of various topical creams and lotions, vitamins or other tissue care related food additives or the like. Computer 108 downloads the current protocol to device 104 through the data transmission link 116 . The communication between toning device 104 and computer 108 may be according to Ethernet, Bluetooth, or any other communication protocols and utilizing any of a variety of connection technologies. Local computer 108 would typically communicate with one or more remote computers 120 through dedicated communication links or via a network such as the Internet. Remote computer 120 , with its display 124 , may be located at a remote site 130 to which a proper qualified medical personnel has access. The personnel may review the tissue toning protocols, their effects on the subject and issue additional recommendation.
[0027] System 100 may include a digital or analog video camera 142 configured to take user 200 ( FIG. 2 ) images and/or video and display them on the local computer display 112 , as well as to communicate the same to remote computer 120 . Experienced medical personnel at the remote site 130 may mark on the video images of user 200 ( FIG. 2 ) target tissue segments locations 204 ( FIG. 2 ) to which according to the current protocol, tissue affecting energy should be applied or coupled. The user can optionally have the ability to modify or change the locations 204 to which the tissue affecting energy should be applied. In an alternative embodiment, the user image 200 may be a virtual symbolic image.
[0028] Tissue toning device 104 is configured to apply a tissue affecting energy to a target segment 204 of tissue 212 ( FIG. 2 ). Tissue toning device 104 typically includes at least a memory 134 ( FIG. 3A ) configured to store and accumulate data related to historical or earlier performed tissue toning results and a computer interface 138 facilitating connection and communication with local computer 108 , and an optional display 142 . The toning history may include data indicating to the user the time of the earlier performed or historic tissue toning procedures, their duration, the tissue affecting energy parameters, segments of the body treated, and the expected toning results in textual or graphical representation. The user may display the segments of the body to be treated, and the expected toning results in textual or graphical representation on an optional display 142 of device 104 . The display 142 may assist guiding the user in proper locations of tissue toning energy application.
[0029] FIG. 3 is a schematic illustration of an exemplary embodiment of the present tissue toning device. Tissue toning device 104 for personal skin toning further may include one or more types of terminations, which are elements configured to couple to the tissue, the tissue affecting energy provided by the respective energy sources. The energy sources may be incorporated in the tissue toning device or packed in a stand-alone housing (not shown). The sources of tissue affecting energy may be such as one or more optical radiation sources 304 shown by their power supplies, RF energy source 308 , ultrasound waves source 312 , and kinetic energy sources (not shown). Tissue toning device 104 may include any one of the tissue affecting energy sources 304 , 308 , or 312 and any combination of them. Terminations couple the tissue affecting energy to a segment 204 of user/subject 200 ( FIG. 2 ) tissue 212 to be toned. The terminations may be one or more RF electrodes 316 , ultrasound transducers 320 , and optical radiation sources 324 , and optical radiation emitting and conveying elements, such as lamps, lenses, light guides, optical windows, and kinetic energy sources (not shown) such as massagers equipped with rollers or balls.
[0030] RF electrodes 316 may have elongated and curved bodies and may be solid, flexible, and hollow electrodes made of a heat conductive metal, or metal coated plastic, or composite material. RF electrodes 316 may be permanently attached to tissue toning device 104 or may be detachable from tissue toning device 104 . Ultrasound transducers 320 may be conventional or phased array transducers. Optical radiation emitting elements 324 expose the target tissue segment to the radiation generated by the elements emitting optical radiation, such as incandescent lamps and lamps optimized for emission of red and infrared radiation and a reflector, Intense Pulse Light (IPL) source, a LED, and a laser diode (as non-limiting examples). Optionally, toning device 104 may include a massaging device (not shown) coupling to the target segment of the tissue with the help of rollers or balls kinetic energy. Tissue toning device 104 may include one or more of such sources or any combination of them.
[0031] Each of the terminations of tissue toning device 104 applies to the skin an appropriate type of skin affecting energy. One or more RF electrodes 316 that are in contact with skin 328 apply to the skin RF energy provided by RF energy sources. Ultrasound waves transducers 324 couple to the skin ultrasound energy generated by the ultrasound waves source 312 , and the optical radiation emitting and conveying elements couple the optical radiation to skin 328 by exposing the skin to the energy generated by one or more optical radiation emitters 324 .
[0032] Since all of the tissue affecting energies and methods disclosed alter the skin temperature at least to some degree, monitoring of the temperature is frequently used to control the toning process. Accordingly, tissue toning device 104 for personal skin toning may also include one or more tissue temperature sensors 332 (illustrated in FIG. 3B ) configured to measure the temperature of the target segment of the tissue. Even with performing the temperature monitoring, certain potential skin damage risk still exist because the sensor response time depends on heat conductivity from the skin to the sensor and inside the sensor, and may be too long and even damaging the skin before the sensor reduces or cuts off the skin heating power. In order to avoid such potential skin damage, temperature sensors 332 communicate the measured temperature to a processing circuit capable of deriving in the course of the tissue toning the rate of the temperature change of the target segment.
[0033] It has been experimentally discovered that the temperature change of the treated skin segment, and in particular a skin segment located between the RF electrodes and of the electrodes, being in contact with the skin depends on the applicator displacement speed. Heat transfer from the skin to the electrode and accordingly the temperature measured by the temperature sensor is largely dependent on the quality of the contact between the electrode and the skin. Differences in the quality of the contact could cause large variations in the temperature measurements. The quality of the skin-to-electrode contact may, for example, be monitored by monitoring the skin impedance and correcting the temperature change rate by an appropriate value or offset. Temperature sensor 332 may be of a variety of types, such as a thermistor, a thermocouple, or resistance temperature detectors as non-limiting examples. Further, temperature sensor 332 may be incorporated into a temperature probe 336 or into an electrode 316 .
[0034] The displacement speed of the applicator can be determined in a variety of manners. On such non-limiting example includes the use of an accelerometer. Another non-limiting example includes the use of optical sensors that can determine movement relative to a target tissue segment.
[0035] The coupling of tissue affecting energy to tissue 328 may be improved by application to the tissue of a gel 340 (shown in FIG. 3A ) that improves one or more of the tissue properties. For example, for RF coupling, the gel may have an electrical resistance higher than that of the tissue. Whereas for ultrasound waves, the coupling the gel may have acoustic coupling properties similar to those of the skin. The tissue toning device may optionally be equipped by a gel dispenser 344 that may be manually or automatically operated and configured to dispense over the skin/tissue 328 gel 340 that may have an electrical resistance higher than that of skin 328 and have acoustic coupling properties similar to those of the skin.
[0036] Although the user conducting treatment may be implementing the current protocol provided by the computer, the practical implementation of the protocol may differ from the recommended one and the user has to be given a continuous feedback on the status of interaction of the tissue affecting or heating energy with the tissue. The temperature change rate may be a basis for such feedback. For example, when tissue toning device 104 displacement speed is faster than the desired speed, the tissue does not receive enough heat and the treatment is not producing a desired effect and vice versa. The temperature change rate would be low for a rapidly displaced tissue toning device and vice versa. A visual or an audio signal indicator may be configured to provide the status of interaction of the tissue heating energy with the tissue. Accordingly, tissue toning device may include a visual signal indicator 348 that may be operative to indicate that the tissue toning device displacement speed is faster than the one set by the current protocol and/or that the tissue heating energy level is lower than the desired one. The audio indicator 352 may be operative to signify that the tissue toning device displacement speed is slower than the one set by the current protocol tissue toning device displacement speed and/or that the skin heating energy level is higher than the desired one (high temperature change rate) and may cause skin burns. Either the visual signal of different colors or the audio signal of different tones or a combination of them may be used in various embodiments.
[0037] The method of use of system 100 in tissue toning procedures is now described. For tissue treatment, tissue toning device 104 connects to a computer, which may be local computer 108 ( FIG. 1 ) or remote computer 120 and upon request, communicates or uploads to the computer the earlier performed or historic toning data presently stored in memory 134 . The historical toning data may include sex and age of the treated subject, tissue affecting energy parameters of the earlier performed tissue toning, segments of the subject body that were treated, and what were the toning results in textual or graphical representation. The computer may also hold updated information on relevant topics from the medical field or the device manufacturer as well as studies on different populations and age groups.
[0038] The computer analyzes the toning data received and issues one or more current tissue toning protocols. The current tissue toning protocol includes at least one or more tissue affecting energies, their respective power, duration, and coupling location or target tissue segment 204 ( FIG. 2 ) on the subject 200 body. The segments of the subject body to be currently treated may be displayed in textual or graphical representation on the local computer display 112 or on the tissue toning device display 142 . In case there is a need to consult with a medical specialist, communication with a company expert or an experienced user at the remote computer site 130 may be initiated, or a telephone call via conventional or Internet based lines may be placed to clear some of the issues that may exist.
[0039] The computer (local or remote) downloads the current tissue toning protocol into device 104 memory 134 . Alternatively, local computer 108 ( FIG. 1 ) may control the tissue current tissue toning session. User 200 brings device 104 in contact with tissue 204 and couples to the skin/tissue the tissue affecting energy, which may be RF energy, optical radiation, and/or ultrasound waves or the like. Each of the energies may be coupled alone or, a combination of energies may be coupled simultaneously or in any desired order or combination to the tissue. By displacing or moving device 104 over the tissue, the user applies the current protocol to a target segment 204 and additional to be treated tissue segments of the subject 200 body. In order to facilitate the tissue toning procedure, the target segment 204 of the tissue may be displayed on the device 104 display 142 or on local computer 108 display 112 . Concurrently with displaying the current toning location the expected current toning procedure results may be displayed on the same display.
[0040] The user/subject controls the tissue toning device displacement speed and the quality of at least one type of tissue affecting energy with the skin coupling by observing one of the signal indicators. The visual signal indicator 348 may be operative to indicate that the tissue toning device 104 displacement speed is faster than determined by the current protocol speed, and accordingly that the skin heating energy level is lower than necessary. The audio signal indicator 352 may be operative to signify that the tissue toning device displacement speed is slower than the displacement speed determined by the current protocol and accordingly that the skin heating energy level is higher than the desired one. For optimal toning results the subject adapts the speed so as to avoid any signal indicator activation.
[0041] A number of embodiments have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the method. Accordingly, other embodiments are within the scope of the following claims:
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Tracking toning history of a subject and determining parameters of a current toning session is provided by recording and storing into the memory of a toning device, or a computer or some other processing device, parameters of each of the preceding tissue toning procedures, as well as segments of the subject body affected by such toning procedures. Next, the recorded data is analyzed and one or more protocols related to the current tissue toning session are then derived. Concurrently, with executing the protocol, recommendations on skin care options, new products adapted for skin care and complementary to the skin/tissue toning, and any other skin care news that may be relevant to the subject skin care are identified and provided.
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FIELD OF THE INVENTION
The present invention relates to a process for the production of pulp. More specifically, the present invention relates to an improved process to break down lignin macromolecules and liberate cellulose fibers in lignocellulosic material using delignifying reactants with a gaseous organic agent as a heating and reaction-accelerating media.
BACKGROUND OF THE INVENTION
The majority of the papermaking pulp produced in the world today is produced by the so-called kraft method. Kraft pulping produces strong fibers, a fact that has given the method its name. This method, however, has the drawback of being very capital intensive. This is due to the need for a very complex system for chemicals recovery and very large unit sizes in the reactors. The reactors have in fact become so big that controlling the actual reactions and liquor circulations has become extremely difficult. The huge unit sizes in all parts of the process also leads to very large in-process inventory and a process that reacts very slowly to e.g. grade changes, etc. Any improvement that would lead to a faster process with shorter in-process delays would therefore have to be seen as a big step forward.
Another problem regarding the kraft method is the use of sulfur, which leads to larger amounts of chemicals being in circulation, odor problems, as well as making the recovery of spent chemicals extra complicated. A process without sulfur would make it possible to have much more efficient burning processes for the dissolved organic material in the process.
In order to address the problems of slow and cumbersome processes and to get rid of the sulfur, and often all inorganic chemicals in the process, several researchers have proposed the use of organic solvents to act as a cooking chemical and dissolve the lignin that holds the cellulose fibers together in wood.
According to J. Gullichsen, C-J Fogelholm, Book 6A, Papermaking Science and Technology, Fapet, 1999, Helsinki, Finland, p. B411, the pulping methods using organic solvents can be classified as follows:
Autohydrolysis methods, in which organic acids released from the wood by thermal treatment act as delignification agents Acid catalyzed methods, in which acid agents are added to the material Methods using phenols Alkaline organosolv methods Sulfite and sulfide cooking in organic solvents Cooking using oxidation of lignin in organic solvent
The basic idea in autohydrolysis, as explained for instance in U.S. Pat. No. 3,585,104 (Kleinert), is to cook the wood in a solvent at high temperature. The high temperature leads to hydrolysis of sugars present in the wood, thus releasing acids. These acids are then supposed to break down and dissolve lignin together with the solvent. The drawback of this process is that very harsh conditions are needed in order to properly delignify the wood. This leads to yield losses and low pulp quality. Others have attempted to improve on the basic idea in order to improve the pulp quality. One such attempt is the so-called IDE process described in EP 0 635 080. The idea is to limit the drop in pH in order to salvage pulp quality. The process is proposed to achieve this by cooking using solvent in a countercurrent manner, thus removing the acids as they are formed early in the cook, and by adding alkali to maintain the pH as desired. The method has never been possible to implement on a commercial scale, possibly due to the large amount of solvent needed to maintain the proposed countercurrent flow. Further, even in the laboratory it is not well suited for all wood species.
If pulp quality is not seen as a major criteria (emphasis on by-product value), acid can be added to the system to increase the speed of the pulping process. Processes have for instance been developed that use acetic and formic acid as delignification agents. The drawback for these processes is that there is no market for the inferior quality pulp, and that severe corrosion problems arise in the equipment.
The so-called Organocell process has been closest to large-scale commercialization of the solvent-using pulping methods. This process is a variant of alkaline organosolv pulping, using simultaneous action of soda-anthraquinone and organic solvent on the lignin. The process seemed to give acceptable pulp quality in the laboratory, but when tried on mill scale the results were not satisfactory.
All prior pulping methods employing organic solvents have been attempts to develop substitutes for the presently dominating kraft pulping method. However, kraft pulping has been constantly improved upon for the last 100 years and is today quite efficient and thus hard to compete with. This can be seen from the fact that no solvent pulping method has proven to be commercially viable. There is, however, still room for improvement in the kraft process itself. For example, the odors of the process are seen as a problem, as is the fact that the reactors are becoming increasingly large and hard to control. Steps have been taken to improve alkaline kraft pulping. One such method is rapid steam phase pulping. The idea is to impregnate the wood with all the alkaline chemicals needed for the reactions in an impregnation stage, followed by heating in a water steam phase. This would make the reactors smaller and partly remedy the problems with odor as described in Canadian Patent No. 725,072. However, this method has not demonstrated enough improvement over the kraft process in liquid phase—yield increase has been very small and reactors still very big, leading to too high chip columns in vapor phase, in turn leading to compaction and collapsing of the digester content, thus plugging flows and destroying pulp quality.
In light of the current research it is clear that the previous research has failed largely because the true role of the organic solvent was not identified. In the current research it has been clearly seen that organic solvents do not participate in the reactions themselves as a solvent of lignin or active chemical, but in fact only have the impact of providing such a reaction environment as to boost the efficiency of other delignifying chemicals.
SUMMARY OF THE INVENTION
In accordance with the present invention, these and other objects have now been realized by the invention of a process for production of pulp from comminuted lignocellulosic material comprising impregnating the comminuted lignocellulosic material in a liquid phase containing fresh reactants at a first temperature so as to produce impregnated lignocellulosic material, removing a majority of the liquid surrounding the impregnated lignocellulosic material, heating the impregnated lignocellulosic material to a second predetermined reaction temperature using the heat released by the condensation of a gaseous organic agent, and maintaining the second predetermined reaction temperature for a desired reaction time, the second predetermined reaction temperature being higher than the first temperature. In a preferred embodiment, the fresh reactants comprise a solution containing at least one of a hydroxide, a sulfide, an anthraquinone, a carbonate, a polysulfide ion, a sulfite or an acid.
In accordance with one embodiment of the process of the present invention, the gaseous organic agent is an aliphatic alcohol, a ketone, or an aldehyde. In a preferred embodiment, the organic agent is methanol, ethanol, propanol, butanol, acetone or a mixture of these compounds, preferably in a purity of over 50% with the remainder being water and impurities.
In accordance with one embodiment of the process of the present invention, the first temperature is between about 20 and 130° C.
In accordance with another embodiment of the process of the present invention, the second predetermined reaction temperature is a maximum of between about 120 and 200° C.
In accordance with another embodiment of the process of the present invention, the impregnating step is between about 10 and 120 minutes long.
In accordance with another embodiment of the process of the present invention, the heating step is between about 2 and 400 minutes long.
In accordance with the present invention, an improved method for producing pulp from lignocellulosic material has been provided.
According to the present invention, the lignocellulosic material is first impregnated with reactant chemicals. This can be performed by submersing the material in a solution containing the chemicals, followed by a removal of excess liquid. The liquid can be any solution containing a delignifying agent. Examples of such liquids are aqueous solutions of hydroxide, sulfide, sulfite, bisulfite, carbonate (e.g. the sodium compounds), sulphur dioxide, anthraquinone, amines or acids. The impregnation can also be performed by contacting the material with delignifying chemicals in the gas phase. An example of this is sulphur dioxide gas that is taken up by the chip moisture.
Subsequently, the energy required for the delignification reactions is provided through heating with a gaseous organic agent, condensing and releasing energy to the solid lignocellulosic material. For the purpose of this specification, a gaseous organic agent is any organic material above its boiling temperature at the pressure of the process at the relevant stage. The gaseous organic agent may comprise various amounts of vapors or droplets, i.e. it need not be in a completely gaseous state. Examples are lower alkyl alcohols, ketones and aldehydes. Mixtures of organic agents may be used, and the agent may contain water. In an industrial process it will not be practical to purify the stream of circulated organic agent. Therefore, the composition will change over time and become a mixture of several volatile compounds. For the purpose of the present invention it is considered that the heating media used is the same as originally used, as long as at least 50% (by mass) of the heating stream is made up of the original organic agent or agents. Preferably, the mass percentage of organic agent(s) in the heating stream is at least 60; more preferably, at least 75; and most preferably at least 90.
Preferable agents include methanol, ethanol, propanol, butanol, acetone and any mixture thereof.
Preferably, the temperature during the impregnation step is in the range of from about 20 to 130° C., and the duration of this step is in the range of about 10 to 130 min. The temperature during the heating step with a gaseous organic agent is higher than the temperature during the impregnation step.
Preferably, the temperature during the heating step reaches a temperature in the range of from about 120 to 200° C.; the pressure during the step evidently corresponds to the physical properties of the organic agent or mixture of agents used. Preferably, the duration of this step is in the range of from about 2 to 400 min.
A surprising benefit is seen when pre-impregnated material is heated by this means. The beneficial effects include very rapid reactions, high yield, lowered energy demand, lowered demand of cooking chemicals and lower rejects compared to conventional kraft pulping. In contrast to earlier work on the so called organosolv processes, the present invention does not involve using the organic agent to dissolve or react with lignin, but rather, the organic agent provides a new kind of non-aqueous media for rapid heating and acceleration of reactions taking place inside the impregnated chips.
The benefit seen from the surprising rise in the speed of delignification can be utilized in several ways, including those mentioned below. For instance, a pulp mill restricted in chemicals recovery capacity could produce much more pulp due to better pulp yield and lower cooking chemicals consumption.
On the other hand, a pulp mill restricted by digester volume could enjoy increased throughput due to a faster process. It could use lower temperatures and gain heat efficiency. A mill restricted by the bleaching line could delignify the wood further in cooking and thus increase production.
BRIEF DESCRIPTION OF THE DRAWING
In the following detailed description, the method of the present invention is disclosed in detail, all reference numerals relating to FIG. 1 , which is a schematic elevational view of the essential process steps of the present invention.
DETAILED DESCRIPTION
Lignocellulosic materials, such as any type of wood, straw or bamboo, is comminuted into easily processed parts (chips in the case of wood; in the following, reference is made to chips) as is customary. The chips are steamed to facilitate air removal. Referring to FIG. 1 , the steamed chips ( 1 ) are brought into contact with liquid containing lignin-breaking reactants, as disclosed above, at a high concentration ( 2 ). The chips are impregnated with the liquid under such conditions that enough reactants are transferred to the chips to enable lignin cleavage to the desired level. The dosage of reactants and combination of time and temperature in both the impregnation and the delignification steps are chosen based on the desired degree of delignification.
Impregnation using a gaseous compound can also be used utilizing a chemical that is enriched in the moisture present in the chips.
After impregnation, the excess liquor is removed and concentrated for reuse ( 4 ) and the chips are brought into contact with a gaseous organic agent at the preferred temperature. This constitutes the heat-up stage ( 3 ), where the gaseous organic agent is brought in through line 5 . The condensation of the heated gaseous agent on the chips releases energy, thus heating the chips to the reaction temperature at which the chips are kept for a predetermined time in stage 6 . The temperature is maintained by adding organic agent as needed. After the reaction time the chips are washed and cooled down in stage 7 , according to methods known by those skilled in the art. From the washing stage, a mixture of wash water, spent chemicals and organic agent is removed in stream 9 . This mixture is heated to vaporize the organic agent, which is then recycled to the heating stage. The spent delignification chemicals are recovered using an appropriate technique, such as current recaustisizing methods, and brought back into the impregnation step.
There are several possible ways to utilize the present invention, depending on which aspect of chemical pulping is seen as the most valuable. Below are a few examples of the aim of the process and what a possible embodiment would be to achieve this aim.
In one variation of the process of the present invention, aiming at minimizing the physical size of a batch digester the process is as follows. The digester is filled with chips according to prior art methods. The digester is then filled with white liquor and impregnation is performed for 10 to 120 minutes at 20 to 130° C. After the impregnation time the spent impregnation liquor is withdrawn and recycled. The chips (without free liquor) are then heated to between 140 and 200° C. by allowing gaseous methanol to condense on the chips and by keeping the digester at this temperature for the duration of the reactions by the addition of gaseous methanol.
In a preferable embodiment for a continuous process, the chips are steamed and brought into an impregnation vessel where they are impregnated with white liquor at 20 to 130° C. for 10 to 120 minutes. The impregnation vessel can be built with either co- or countercurrent liquor flow configuration, according to principles known to a person skilled in the art. From the impregnation vessel the chips are transferred to the digester, at the top of which the free liquor is removed from the chips, according to prior art methods. When the liquor has been removed the chips are fed forward so that they are brought into contact with a methanol vapor atmosphere at 140 to 200° C. and kept at this temperature for the duration of the reaction time. The digester used can be similar to present continuous kraft digesters or specifically built for the present invention.
In a preferred embodiment of the present invention aimed at minimizing cooking plant (batch or continuous) steam consumption, impregnation is performed at 30 to 130° C. and a reaction temperature of 120 to 140° C. is used, the reaction temperature however being higher than the impregnation temperature.
In a preferred embodiment aimed at achieving maximum pulping capacity for a given capacity of chemicals recovery, the impregnation is performed using diluted white liquor and the reaction time is extended to that typical of present generation digesters.
In a preferred embodiment aimed at simplifying the chemicals recovery, the improved cooking efficiency can be used to make it possible to use sulfur-free cooking that does not require the use of the so called lime cycle in chemicals recovery. Such processes are green liquor pulping, pulping using carbonate or autocaustisizing using borohydride.
In a preferred embodiment of the present invention, it is used to pulp raw materials other than wood, such as straw, reeds or bamboo. Due to the boost given to the process by heating using a gaseous organic agent, less powerful lignin degrading chemicals, such as carbonate, can be used in the process.
In addition to the embodiments presented above based on the dominating pulping method, kraft cooking, the invention boosts the reactions of any cooking method, such as sulfite and bisulfite cooking.
EXAMPLES
The method of the present invention can be used with a wide variety of raw materials and cooking methods. In the following examples, numerical data for tests with both wood and straw pulping is presented. All tests have been performed using the same laboratory scale digester. “Steam” refers to steam phase water.
The digester used has been purposely built to facilitate the testing of vapor phase processes. The design includes a special heating jacket that prevents the heating power of the vapor from being spent on heating the digester itself. This problem, typical for laboratory scale systems, will not arise in industrial applications as the ratio of wood to equipment weight is much higher.
Wood as Raw Material
Experimental Wood:
fresh softwood mill chips, dry matter
content 50%
Batch size:
400 g wood as oven dry mass
Chemicals:
mill white liquor
Digester size:
2200 ml
TABLE 1
Amounts of liquor used in softwood pulping experiments:
Cooking liquor in batch pulping
2000
ml
(same liquor present throughout the process)
Steam phase & present invention:
Impregnation liquor:
1500
ml
Impregnation liquor removed:
800
ml
Heating agent fed into the system:
600
ml
TABLE 2
Comparison of process conditions in softwood pulping
using prior art technology and the present invention.
Batch
kraft
Kraft
Conventional
with
steam
Present
batch kraft
methanol
phase
invention
Impregnation
90
95
80
80
temperature
(° C.)
Impregnation
60
60
60
60
time (min)
Alkali into
25%
25%
19%
19%
reaction
stage (EA on
wood as
NaOH) 1
Composition of
heating media:
H 2 O steam
100%
Liquid H 2 O
100%
40%
Organic
60%
agent liquid
Gaseous
100%
organic
agent
Reaction
175
175
175
175
temperature
(° C.)
1 In conventional pulping, the term alkali charge is used to determine how much chemical is used. In vapor phase pulping, the important variable is the amount of alkali that has been absorbed by the wood prior to the reaction stage. In the conventional and batch kraft examples the number relates to alkali charge; in the steam phase and in the examples of the present invention, the number has been calculated by subtracting the charge of alkali left in the spent impregnation liquor from the amount originally charged
Results
TABLE 3
Results from softwood pulping using prior
art technology and the present invention.
Batch
kraft
Kraft
Conventional
with
steam
Present
batch kraft
methanol
phase
invention
Kappa
23
23
23
23
number
Reaction
80
73
74
38
time (min)
Alkali
17.4%
18.9%
16.9%
15.5%
consumption
(EA on wood
as NaOH)
Total yield
44.6
45.7
48.7
49.8
(% on wood)
Rejects (%
0.1
0.2
0.1
0.1
on wood)
As can be seen from Table 3, the benefits of the present invention are quite clear. Compared to liquid phase processes (conventional batch kraft and batch kraft with methanol) the amount of chemicals needed in the digester in the reaction stage is much lower. Also, compared to a steam phase without methanol, the present invention offers a huge benefit in terms of total reaction time and alkali consumption. The benefit seen in reaction time can also be translated to a lower need for alkali in the reaction stage, or lower reaction temperature when using the same reaction time as for the other processes, further increasing the flexibility of the process.
In the above example all cooks have been performed at the same reaction temperatures. Therefore, the benefit of accelerated cooking kinetics can be seen directly as a decrease in reaction time. In practical chemical pulping, time and temperature is usually combined into a single variable, the so-called H-factor. In experiments at varying temperatures it has been seen that the benefits of the current process are observed as a decrease of almost 50% in the H-factor required to reach a certain degree of delignification, regardless of temperature.
Non-Wood Raw-Materials
The present invention is also suitable for use with other raw-materials than wood, and also enables the use of cooking chemicals that under normal circumstances lack the delignifying power to produce acceptable pulp. Table 5 shows a comparison between the use of steam phase pulping and the present invention for straw delignification, using only carbonate as the pulping chemical. Both cooks have been performed identically except for the choice of heating media.
Experimental
Raw-material: air dried wheat straw, dry matter content 90%
Batch size: 250 g as oven dry straw
Pre-treatment: the straw was cut into approx. 5 cm long pieces for easy handling
Equipment: present invention and steam-phase pulping performed in the same digester as the softwood experiments. The conventional pulping experiment shown in Table 6 was performed using a simple air-heated autoclave digester.
TABLE 4
Amounts of liquor used in straw pulping experiments:
Cooking liquor in batch pulping
2000
ml
(same liquor present throughout the process)
Steam phase & present invention:
Impregnation liquor:
2000
ml
Impregnation liquor removed:
1000
ml
Heating agent fed into the system:
600
ml
TABLE 5
Comparison of wheat straw pulping performance of
steam phase pulping and the present invention using
Na 2 CO 3 as the delignification reagent.
Carbonate AQ
Present
steam-phase
invention
Impregnation
80
80
temperature (° C.)
Impregnation time
60
60
(min)
Concentration of NaOH
0
0
in
impregnation/cooking
liquor (g/l)
Alkali into reaction
107
99
stage (% Na 2 CO 3 on
straw)
AQ in impregnation (%
0.2
0.2
on straw)
Reaction temperature
160
160
(° C.)
Time at reaction
71
69
temperature (min)
Kappa number
58
18
Total yield (% on
58.3
52.4
straw)
Rejects (% on straw)
15.3
2.9
From Table 5 it can clearly be seen how the accelerating effect of the organic agent makes it possible to produce low-reject pulp using only carbonate as the pulping chemical. The pulp produced with the steam-phase method is unusable as papermaking pulp due to high rejects and high lignin content. The fact that no sodium hydroxide is needed in the present invention constitutes an immense benefit over present industrial processes, as chemicals recovery can be simplified drastically.
TABLE 6
Comparison of the wheat straw pulping performance
of the present invention using Na 2 CO 3 and state
of the art technology using NaOH
Conventional
batch soda
Present
AQ process
invention
Impregnation
No separate
90
temperature (° C.)
impregnation
Impregnation time
No separate
60
(min)
impregnation
Heat-up time (min) 1
45
9
Concentration of NaOH
31
0
in
impregnation/cooking
liquor (g/l) 2
Concentration of
9.3
212
Na 2 CO 3 in
impregnation/cooking
liquor (g/l) 2
AQ in
0.1
0.2
impregnation/cooking
(% on straw)
Reaction temperature
160
160
(° C.)
Time at reaction
10
69
temperature (min)
Kappa number
17
18
Total yield (% on
49.1
52.4
straw)
Rejects (% on straw)
3.4
2.9
1 Heat-up 25-160° C. for conventional, 90-160° C. for present invention
2 In conventional - all liquid used in cooking, in present invention - free liquor removed after impregnation
Table 6 shows a comparison between the present invention and the currently industrially important soda-AQ method. As can be seen, the yield of pulp is superior in the present invention and no sodium hydroxide is needed. The benefits of the present invention are hereby twofold. Investment costs for a new mill are kept low as chemicals recovery is simplified and the operating costs are lower, as less raw material is required for the production of a given amount of pulp.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims.
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The invention relates to an improved process to break down lignin macromolecules and liberating cellulose fibers in lignocellulosic material using delignifying reactants with a gaseous organic agent as a heating and reaction-accelerating media. Lignocellulosic material is first impregnated with reactant chemicals, e.g. commonly used agents such as sodium hydroxide and sodium sulfide. Subsequently, the energy required for the delignification reactions is provided through heating with a gaseous organic agent such as methanol or ethanol, condensing and releasing energy to the solid lignocellulosic material. The temperature during the heating step with a gaseous organic agent is higher than the temperature during the impregnation step.
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FIELD OF THE INVENTION
This invention relates to drive units, more particularly to a motor drive unit which uses a novel integration of a motor and a planetary gear set to contain reaction forces within the drive.
BACKGROUND OF THE INVENTION
Motors generate twisting reaction forces (reverse torque) which are transmitted to their associated mounting brackets. With reference to hand held power tools, these forces may cause operation of the tool to become inefficient, uncomfortable or even unsafe.
An electric motor consists of an armature and an outside case. The armature is part of the motor's drive shaft and will be referred to herein as the action member. The outside case of the motor is separate from the armature and will be referred to as the reaction member. In prior art configurations, the outside case of the motor is mounted solidly within the tool casing. The armature is caused to turn when electricity is supplied to the motor. The reaction forces are then directly transmitted from the outside case of the motor to the tool casing, where they are contained by the mounting brackets of the tool.
With existing portable hand drills, the hand of the operator is actually the mounting bracket. The reaction forces can be felt by the operator as a twisting effort. The twisting effort (or the reaction force) will be equal to the effort at the drill bit (or the action force).
Planetary gear sets are known to be useful as reduction gear sets and for other power transmission purposes, but have not heretofore been used to eliminate undesirable reaction forces in motor-driven tools.
Prior developments in this field may be generally illustrated by reference to the following patents:
______________________________________ Patent No. Patentee Issue Date______________________________________3,134,275 R. Davison May 26, 19642,591,967 H. Ridgely et al. Apr. 08, 19521,151,381 N. Olson Aug. 24, 19152,826,095 B. Dirzius et al. Mar. 11, 19583,204,489 K. Furukawa et al. Sep. 07, 19654,901,602 H. Matoba Feb. 20, 19902,582,698 E. Hirvonen Jan. 15, 19522,899,850 J. Selby et al. Aug. 18, 1959______________________________________
U.S. Pat. No. 3,134,275 shows a hand held power tool which utilizes planetary gears to couple the electric motor to the output member. The outside case of the motor 24 of this device is rigidly connected to the tool casing 12. Therefore, the reaction forces of the motor are transmitted to the tool 10 in the traditional manner.
U.S. Pat. Nos. 2,591,967 and 1,151,381 teach other sun gear and planet gear assemblies. Neither teach a configuration which would isolate the reaction forces of a drive motor from an associated power tool.
U.S. Pat. No. 2,826,095 shows a rotating head for a drill which incorporates a planetary gear arrangement. An arm 25 transfers reaction forces or torque (col. 2, lines 3-7) from the planetary gear set to the tool (in this case a drill press 12) rather than isolating them from the tool.
The rest of the patents are representative of what is in the art.
SUMMARY OF THE INVENTION
The present invention comprises a reaction less drive unit--a mechanical drive which contains the reaction forces within itself. Insofar as the drive does produce reaction forces, but which forces also contribute to the power at the output shaft, the device will be referred to herein as a "reaction containment drive." The reaction containment drive will be particularly useful in hand tools and other applications where the twist of reaction is undesirable or dangerous.
This device consists of a power source, such as an electric or hydraulic motor (or any rotary motor), and a planetary gear set. The motor and planetary gear set are coupled together in such a way that the forces of reaction are kept within the drive. While the planetary gear set is known, the proposed reaction-containing configuration is novel. In effect, the planetary gear set and the electric motor become one unit, instead of two units coupled together.
A planetary gear set consists of three main parts: a center gear called the sun gear; a middle gear set called the planet gears; and an outside gear called the ring gear. There are usually three planet gears. They are solidly mounted in a planet carrier, but they do turn on their mounting posts. The planet gears and carrier are treated as one part of the planetary set. The ring gear, planet carrier and the sun gear are all coaxial.
Power is transmitted through the set when any one part of the set is driven and any other part is held solid or static. The remaining part of the planetary set then becomes the output member of the reaction containment drive.
In the reaction containment drive, the outside case (reaction member) of the motor is solidly attached to the part of the planetary set that is chosen in a particular configuration to be the "solid" part, relatively speaking. Actually no member of the drive, nor part of the gear set, is mounted solid or prevented from turning with respect to the casing of the tool. Instead, the entire motor and planetary gear set assembly is mounted on bearings so that it is free to turn within the tool casing. The reaction member of the drive unit transmits the reaction forces to the output member. If the action member is said to push the output member, then the reaction member pulls it as well. Since all the forces are contained within the drive, there is no twist or reaction felt by the operator of the device.
In one preferred unit (see the discussion of FIG. 3 below), the armature (action member) of an electric motor is connected to the sun gear (input part) of the planetary set. The outside case (reaction member) of the electric motor is attached to the planet carrier group (solid or static part). The ring gear (output part or member) may be used to drive a drill bit or the like.
Regardless of the configuration, the basic theory remains the same. When the reaction member of the electric motor, or other primary power source, is attached to any part of the planetary gear set and the action member is attached to any other part of the same gear set, both the action and the reaction forces are contained within the drive. There is a resultant bias to the output part of the planetary gear set that is available to do useful work.
The unique quality of the reaction containment drive is the fact that the planetary gear set is integrated with a drive motor instead of being connected to it. The drive motor and planetary gear set are one unit. Because of this construction, both the action and the reaction forces combine to deliver power to the output shaft.
FEATURES AND ADVANTAGES
An object of this invention is to disclose, in a power tool of the type which has a tool casing and a rotatable output shaft, a reaction containment drive apparatus which includes a motor having an outside case free to rotate within the tool casing and an internal rotatable drive shaft; and further includes a planetary gear set having three parts, namely a central sun gear part, a middle planet gear part, and an outside ring gear part. The planet gear part is rotatable between the sun gear part and the ring gear part. The planetary gear set connects the drive shaft of the motor to the output shaft of the tool.
A further object is to disclose such a drive wherein one part of the planetary gear set is fixedly connected to the drive shaft and rotatable together therewith as a unitary action member, wherein one part of the planetary gear set is fixedly connected to the outside case of the motor and rotatable together therewith as a unitary reaction member, and wherein the remaining part of the planetary gear set is fixedly connected to the output shaft of the tool and forces the output shaft to rotate together therewith as a unitary output member when power is supplied to the motor.
Preferably, the planetary gear set has three planet gears as a feature thereof.
Still another feature is rotational bearing means between the tool casing and the outside case of the motor and between the outside case of the motor and the drive shaft. Additional bearings are provided where advantageous.
Yet another feature of the reaction containment drive is means for providing power to the motor as its outside case rotates within the tool casing. The power providing means includes a pair of conductive annular slip rings extending around the outside circumference of the outside case of the motor and a pair of conductive brushes, each brush being continuously connected to one of the slip rings as the outside case rotates within the tool casing.
Another feature is an apparatus which is easy and safe to use and is suitable for mass production at relatively low cost.
Other novel features which are characteristic of the invention, as to organization and method of operation, together with further objects and advantages thereof will be better understood from the following description considered in connection with the accompanying drawing in which a preferred embodiment of the invention is illustrated by way of example. It is to be expressly understood, however, that the drawing is for the purpose of illustration and description only and is not intended as a definition of the limits of the invention.
Certain terminology and derivations thereof may be used in the following description for convenience in reference only and will not be limiting. For example, the words "upwardly," "downwardly," "leftwardly," and "rightwardly" will refer to directions in the drawings to which reference is made. The words "inwardly" and "outwardly" will refer to directions toward and away from, respectively, the geometric center of a device and designated parts thereof.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic sectional elevation of a portable hand drill, showing a first reaction containment of this invention;
FIG. 2 is a sectional side elevation of the drill of FIG. 1, taken along line 2--2 of FIG. 1;
FIG. 3 is a schematic sectional elevation of a second reaction containment drive;
FIG. 4 is a schematic sectional elevation of a third reaction containment drive; and
FIG. 5 is a sectional side elevation of an alternate planetary gear set which may be used with the embodiments of this invention.
______________________________________Drawing Reference Numerals______________________________________A arrowB arrowC arrowD arrowE arrowF arrowG arrowH arrowI arrow 1 reaction containment drive 3 tool 4 casing of 3 6 switch on 4 8 cover of 4 10 screw for 8 12 electrical wire 13 electrical wire 14 primary brush 18 support bearing on 4 20 motor 21 shaft of 20 22 outside case of 20 24 slip ring for 14 26 wire connector for 24, 28 28 brush of 20 29 field shoe of 20 30 armature of 20 32 commutator on 30 34 support bearing on 22 for 30 36 planet carrier for 40 on 30 37 post on 36 for 44 38 thrust bearing between 22, 36 40 planetary gear set 42 ring gear of 40 on 22 44 planet gear 46 sun gear on 50 50 output shaft 52 chuck mount area of 50 54 thrust bearing between 36, 46 56 pilot bearing between 36, 50101 reaction containment drive104 tool casing108 cover of 104110 screw for 108112 electrical wire113 electrical wire114 primary brush118 support bearing on 104120 motor121 shaft of 120122 outside case of 120124 slip ring for 114126 wire connector for 124, 128128 brush of 120129 field shoe of 120130 armature of 120132 commutator on 130134 support bearing on 122 for 130136 planet carrier for 140 on 122137 post on 136 for 144140 planetary gear set142 ring gear of 140 on 150144 planet gear146 sun gear on 121147 pilot bearing148 extension of 121150 output shaft201 reaction containment drive204 tool casing208 cover of 204210 screw for 208212 electrical wire213 electrical wire214 primary brush218 support bearing on 204220 motor221 shaft of 220222 outside case of 220224 slip ring for 214226 wire connector for 224, 228228 brush of 220229 field shoe of 220230 armature of 220232 commutator on 230234 support bearing on 222 for 230236 planet carrier for 240 on 250237 post on 236 for 244240 planetary gear set242 ring gear of 240 on 222244 planet gear246 sun gear on 221247 pilot bearing248 extension of 221250 output shaft336 planet carrier for 340340 planetary gear set342 ring gear of 340344 planet gear345 intermediate planet gear346 sun gear______________________________________
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIG. 1, there is illustrated therein a reaction containment drive 1 of this invention. The drive 1 is shown incorporated into a tool 3, namely a portable hand drill, but it could be used in any of a number of tools which utilize a rotating output member to do useful work.
The tool 3 has a casing 4, from which casing it is desired to eliminate reaction forces that tend to twist the tool when it is in the hand of the user. A standard power switch 6 controls the drill. A removable cover 8 may be held onto the casing 4 by means of screws 10. Electrical wires 12, 13 run from the power cord and the switch 6, respectively, to the primary brushes 14 of the electrical motor 20. These wires, together with the slip rings 24 discussed below, constitute means for supplying power to the motor.
The motor, including its outside case 22, may rotate within the tool casing 4, being only held therein by means of the rotational support bearings 18. These bearings cradle the drive shaft 21 of the motor and the output member 50.
As stated, the outside case 22 (reaction member) of the motor 20, unlike prior art motor cases, is free to rotate within the tool 3. It is supported on the motor shaft 21 by means of the rotational bearings 34. A pair of electrically conductive annular slip rings 24 extend around the outside circumference of the outside case 22. As the case 22 rotates, the slip rings 24 serve to continuously connect, by means of wires 26, the conductive primary brushes 14 to the internal motor brushes 28. Part 29 represents the field shoe of the motor. The motor brushes 28 power the commutator 32 of the armature 30. The motor's drive shaft 21, as in the existing art, is a fixed part of the armature 30 (action member) of the motor.
Generally, one part of a three-part planetary gear set will be fixedly connected to the armature (action member) of the motor, another part of the gear set (the "solid" part thereof) will be fixedly connected to the outside case of the motor (the reaction member), and the third part of the gear set (the output member) will be available for useful work.
In this embodiment, the armature 30, more properly the drive shaft 21, is fixedly and integrally connected to the planet carrier 36 of the planetary gear set 40. The planet gears 44 rotate on posts 37 attached to the planet carrier. This makes the planet gears 44 the input part of the gear set, and, together with the armature, the action member of the drive. They are forced to rotate within a ring gear 42, which ring gear is an integral part of the motor case 22 (together, the reaction member). The ring gear is therefore considered the solid part of the set in this embodiment. The central sun gear 46 thus becomes the output part of the planetary set and, together with the output shaft 50 to which it is fixedly attached, becomes the output member of the drive. The output shaft terminates in an area configured in this embodiment as a drill bit chuck mount 52.
The output shaft 50 rotates about pilot bearings 56 in the planet carrier and about support bearings 18 in the cover 8 of the tool casing 4. The planet carrier 36 is freed to rotate against the motor case 22 through thrust bearings 38. The sun gear 46 is supported against axial thrust by bearings 54. It is to be understood that the bearings, the gears, and other common parts of the tool 3 are merely drawn schematically in this and other figures, for clarity of illustration.
The speed of the individual gears depends on the gear ratio of the planetary set as a whole. One preferred gear ratio is four to one.
Turning to the side elevation of FIG. 2, it can be seen how the reaction containment drive 1 contains the reaction forces within itself. The armature 30 of the electric motor 20 drives the planet carrier 36 in, say, a counter-clockwise direction, as indicated by arrow A. This forces the planet gears 44 to turn clockwise within the ring gear 42 (arrow B). In turn, the sun gear 46 and the output shaft 50 are driven counter-clockwise (arrow C) by the planet gears.
The motor case/ring gear turns in a direction opposite to the armature/planet carrier, i.e. clockwise (arrow H). This also forces the planet gears 44 to turn clockwise on their shafts 37 (arrow B). The turning force on the output shaft 50 is therefore a direct result of the rotation of both the action and reaction members. Within the power range of the drive unit the ring gear 42 and the planet carrier 36 turn in opposite directions. Under a very heavy load they turn in the same direction but at different speeds. The drive members will stall under load with a gear ratio of 1 to 1. This relative movement between the planet carrier and the ring gear forces the planet gears 40 to turn on their posts 37 and forces the sun gear 46 and output shaft 50 to turn.
An overdrive and a corresponding loss of torque at the output shaft occurs with this configuration and gear ratio. The power flow is the same regardless of the direction of rotation of the components; thus, the reaction containment drive 1 is fully reversible.
The torque and speed at the output shaft 50 is available without any twisting effort being felt by the user of the drill 3, except for that generated by the friction of the bearings and brushes. This is possible because the output force is a result of both the action and reaction forces. The power curve of any reaction containment drive unit is a function of both the gear ratio of the planetary set and the manner in which it is configured.
FIG. 3 shows a second reaction containment drive 101, in this case illustrated separate from any particular power tool (except for a schematic casing 104). It is to be noted that, for convenience the last two positions of the reference numerals of alternate embodiments of the invention duplicate those of the numerals of the embodiment of FIG. 1, where reference is made to similar or corresponding parts.
A removable cover 108 is held onto the casing 104 by means of screws 110. Electrical wires 112, 113 run to the primary brushes 114 of the electrical motor 120. The motor, including its outside case 122, may rotate within the tool casing 104. The motor is only held therein by means of support bearings 118, which bearings cradle the outside case 122 of the motor and the output member 150.
As stated, the outside case 122 (reaction member) of the motor 120, unlike prior art cases, is free to rotate within the tool casing 104. It supports the motor shaft 121 by means of bearings 134. A pair of annular slip rings 124 extend around the outside circumference of the outside case 122. As the case 122 rotates, the slip rings 124 serve to continuously connect, by means of wires 126, the primary brushes 114 to the internal motor brushes 128. Part 129 represents the field shoe of the motor. The motor brushes 128 power the commutator 132 of the armature 130. The motor's drive shaft 121 is a fixed part of the armature 130 (action member) of the motor.
In this embodiment, the armature 130 (action member), and the drive shaft 121, are fixedly connected to the sun gear 146 of the planetary gear set 140. This makes the sun gear 146 the "input part" of the gear set (as opposed to the planet gears 44 of the embodiment of FIG. 1). The planet gears 144 rotate on posts 137 attached to the planet carrier 136, which planet carrier is an integral part of the motor case 122 (formally "solid part"--as opposed to the ring gear 42 of the embodiment of FIG. 1). The planet gears cause a ring gear 142 to rotate, which ring gear thus becomes the output member of the drive (as opposed to the sun gear 46 of the embodiment of FIG. 1). The ring gear is fixedly attached to the output shaft 150.
The output shaft 150 rotates about support bearings 118 in the tool casing 104. Pilot bearings 147 hold a support shaft 148, which shaft is merely an extension of the drive shaft 121.
FIG. 4 shows a second reaction containment drive 201. A removeable cover 208 is held onto a tool casing 204 by means of screws 210. Electrical wires 212, 213 run to the primary brushes 214 of the electrical motor 220. The motor, including its outside case 222, may rotate within the tool casing 204. The motor is rotatably held therein by means of support bearings 218, which bearings cradle the outside case 222 of the motor and the output member 250.
As in previous embodiments, the outside case 222 (reaction member) of the motor 220 is free to rotate within the tool casing 204. The motor case supports the motor shaft 221 of the armature 230 by means of bearings 234. A pair of annular slip rings 224 extend around the outside circumference of the outside case 222. As the motor case 222 rotates, the slip rings 224 serve to continuously connect the primary brushes 214 to the internal motor brushes 228, by means of wires 226. The field shoe 229 of the motor extends around the armature. The motor brushes 228 power the commutator 232 of the armature 230. The motor's drive shaft 221 is a fixed part of the armature 230 (action member) of the motor.
In this embodiment, the armature 230 (action member) is fixedly connected to the sun gear 246 of the planetary gear set 240. As in the embodiment of FIG. 3, this makes the sun gear 246 the input part of the planetary gear set. The planet gears 244 rotate on posts 237 attached to the planet carrier 236, which planet carrier, unlike in the previous two embodiments, is an integral part of the output shaft 250. It is, therefore, the planet carrier 236 which is the output member of the reaction containment drive 201. As in the device of FIG. 1, it is the ring gear 242 (solid part) which is fixedly attached to the motor case 222. The sun 246 and planet 244 gears cause the planet carrier 236 to rotate, making the output shaft 250 available for useful work.
The output shaft 250 rotates about support bearings 218 in the tool casing 204. Pilot bearings 247 hold a shaft 248 which is a supporting extension of the drive shaft 221.
Other configurations for attaching the motor casing, motor armature, and the tool's output shaft to the planetary gear set are possible, the above three embodiments being presented as representative examples thereof.
FIG. 5 illustrates an alternate planetary gear set 340 which could be substituted for the gear set of any of the previous embodiments. It is to be noted that the gear set 340, like the sets of FIGS. 1-4, is not itself novel--apart from its incorporation in a reaction containment drive as described herein.
As above, any one part of the gear set 340 may be the input part, any other part the output part and the remaining part the solid or static part. Therefore, any description of the turning of the individual gears must be understood to be purely relative. The sun gear 346 turns with an intermediate set of planet gears 345. The intermediate planetary gears turn with an outer set of planet gears 344. The outer set turns with the ring gear 342 and/or the planet carrier 336. One possible set of relative motions is indicated by arrows D-G.
Regardless of the configuration, the basic theory remains the same. When the reaction member of an electric motor, or other primary power source, is attached to any part of a planetary gear set and the action member is attached to any other part of the same gear set, both the action and reaction forces contribute to the force of the output part. The output part of the planetary gear set is available to do useful work without any reaction outside the unit.
While the above provides a full and complete disclosure of the preferred embodiments of this invention, various modifications, alternate constructions, and equivalents may be employed without departing from the true spirit and scope of the invention. Such changes might involve alternate materials, components, structural arrangements, sizes, operational features or the like. Therefore, the above description and illustrations should not be construed as limiting the scope of the invention which is defined by the appended claims.
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A reaction containment drive apparatus for a power tool includes a motor having an outside case free to rotate within the tool casing, and an internal drive shaft. A planetary gear set is an integral portion of the drive. It has three parts, namely, a central sun gear part, a middle planet gear part (the planet gear part having a planet carrier and preferably three planet gears on the planet carrier), and an outside ring gear part coaxial with the sun gear part and the planet carrier. The planet gear part is rotatable between the sun gear part and the ring gear part. One part of the planetary gear set is fixedly connected to the drive shaft and rotatable as a unit therewith; one part of the planetary gear set (for example, the ring gear) is fixedly connected to the outside case of the motor and rotatable as a unit therewith; and the remaining part of the planetary gear set is fixedly connected to the output shaft of the tool and forces the output shaft to rotate as a unit therewith when power is supplied to the motor. The reaction containment drive contains reaction forces within itself and prevents such forces from being transmitted from the output shaft to the tool.
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TECHNICAL FIELD
[0001] The invention relates to a technique for positive identification of digital video signals.
BACKGROUND ART
[0002] Identification of a serial digital video signal from a single source or even a few sources generally presents little difficulties. However, in a typical broadcast facility, many serial digital video signals exist, and identification of each signal often proves problematic, particularly as the signals undergo routing through one or more devices, such as a cross-point switcher, some times referred to as a cross-point matrix. Presently, to positively identify a given serial digital video signal during routing, descrambling and de-serialization of the signal must occur in order to decode the identification information. Carrying out these processes requires a significant amount of hardware. Thus, in a system having many serial digital video signals, providing the necessary descrambling and de-serialization hardware often proves impractical from a cost, space and power consumption perspective. For this reason, broadcast facilities typically rely completely on routing control system status information to determine which input connects to a given output in the cross-point matrix. Such reliance incurs the disadvantage that no automated method exists for checking the actual signal present at a given cross-point matrix output and alerting the user should the status information prove erroneous.
BRIEF SUMMARY OF THE INVENTION
[0003] In accordance with an illustrative embodiment of the present principles, a method for identifying a digital video signal in a video system commences with the step of phase modulating the digital video signal with an identification signal at an input of the video system, thereby identifying that signal. The phase modulated digital video signal undergoes demodulation at an output of the video system to establish the identity of the video signal. In this way, verification of proper routing of the signal through video system can occur.
BRIEF SUMMARY OF THE DRAWINGS
[0004] FIG. 1 depicts a block schematic diagram of video system that identifies at least one digital video signals at an input for confirmation at an output in accordance with an illustrative embodiment of the present principles,
[0005] FIG. 2 depicts a block schematic diagram of one of the input circuits of the video system of FIG. 1 to phase modulate an input signal to identify that signal;
[0006] FIG. 3 depicts a block schematic diagram of one of the output circuits of the video system of FIG. 1 to demodulate an output signal for obtain the identification of that signal.
DETAILED DESCRIPTION
[0007] As described in greater detail hereinafter, in accordance with the present principles, the digital video input signal to a video system, gets identified to enable verification of signals at the system outputs.
[0008] FIG. 1 depicts a video system 10 which illustratively takes the form of cross-point matrix, some times referred to as a cross-point switcher or router, having the capability of routing a digital video signal at one or more of its inputs 12 1 - 12 n to one or more of its outputs 14 1 - 14 m where n and m are both integers greater than zero, but not necessarily equal to each other. The cross-point matrix 10 performs the routing of selected signals at its respective inputs 12 1 - 12 n to selected ones of the outputs 14 1 - 14 m under control of a routing control system (not shown). For a large video cross point matrix where n and m are both large, confirmation of the routing of a digital video signal from an input to any given output previously depended on status information provided by cross-point matrix or its control system. Since no mechanism heretofore existed for independent signal identification, an error in the status information thus could go undetected.
[0009] In accordance with the present principles, the cross-point matrix 10 has a plurality of input circuits 16 1 - 16 n coupled to corresponding ones of the matrix inputs 12 1 - 12 n , respectively. Each input circuit such as input circuit 12 1 receives an incoming serial digital video signal destined from the cross-point matrix 10 and provides the signal with its own identification in a manner described hereinafter. In this way, each input signal routed through the cross-point matrix 10 to one or more outputs 14 1 - 14 m carries its own unique identifier.
[0010] Each of the cross-point matrix 10 outputs 14 1 - 14 m is coupled to a corresponding output circuit 18 1 - 18 m , respectively. Each output circuit, such as output circuit 18 1 serves to strip the identifier from the signal at the corresponding cross point matrix output. The identifier stripped from the output signal is decoded to verify that the output signal corresponds to the input signal routed from the intended input. In other words, if the signal at input 12 1 was to be routed to output 14 1 , the identifier associated with the output signal appearing at that output should match the identifier of the input signal at the corresponding cross-point matrix input. Thus, the combination of the input circuits 16 1 - 16 n and output circuits 18 1 - 18 m provide a mechanism for determining whether an error exists in the cross-point matrix 10 status information.
[0011] FIG. 2 depicts a block diagram of an exemplary input circuit, such as input circuit 16 1 , all of which share the same features. The input circuit 16 1 includes an equalizer and re-clocking circuit 20 for equalizing and re-clocking an incoming serial digital video signal. A phase modulator 22 phase modulates the output signal of the equalizer and re-clocking circuit 20 with a source identification information signal specific to the particular input circuit. In other words, each of the input circuits 16 1 - 16 n makes use of a different source identification information signal to uniquely identify each incoming serial digital video signal.
[0012] The frequency of each source identification signal typically will lie above the pass band of a loop filter (not shown) in the output of the equalizer and re-clocking circuit 20 . In practice, the loop band pass bandwidth usually lies in the 100-200 kHz region. The frequency of the source identification signal is also chosen so that it is not an integer sub-multiple of the serial digital video data rate (i.e. 135 MHz, 90 MHz, 67.5 Hz etc. for a 270 Mb/s signal or 742.5 MHz, 495 MHz, 371.25 MHz etc. for a 1.485 Gb/s signal). Avoiding such frequencies avoids the large amounts of energy present at these frequencies in the serial digital video signal frequency spectrum. The depth of modulation is set so that the combined total of phase modulation and jitter from other sources is less than 20% of the unit interval for the data rate used. Setting the depth of modulation in this manner assures that signal recovery can occur without error by during re-clocking by one of the output circuits 18 1 - 18 m .
[0013] FIG. 3 depicts an exemplary output circuit, such as circuit 18 1 , all of which share the same features. The output circuit 18 1 includes a re-clocking flop-flop register 24 supplied at its D input with the serial digital video signal from the associated output of the cross-point matrix 10 of FIG. 1 . A phase detector 26 within the output circuit 18 1 also receives the serial digital video signal at a first input from the cross-point matrix 10 of FIG. 1 . The phase detector 26 has its second input supplied with the output signal of a voltage controlled oscillator 27 which serves as the clock signal generator for the re-clocking register 24 .
[0014] The phase detector 26 provides an output signal in accordance with the phase difference between the signals at its first and second inputs to both a loop filter 28 and a source identification decoder 30 . The source identification signal decoded by the decoder 30 allows the routing control system for the cross-point matrix 10 (not shown) to verify the correct routing path through the cross-point matrix. The source identification signal has a higher frequency than the pass band of the loop filter 28 so that the loop filter effectively rejects the source identification signal. In this way, the voltage controller oscillator 27 , driven at its input by the output signal of the loop filter 28 , will not track the source identification signal.
[0015] As indicated previously, the output signal of the voltage controlled oscillator 27 serves as the clock signal for the re-clocking register 24 . With the loop filter 28 filtering out the source identification signal from the voltage controlled oscillator 27 , the source identification effectively gets removed from the output of the re-clocking register 24 . In this way, the re-clocking register 24 can drive an output buffer 36 with re-clocked signal corresponding to the incoming serial digital video signal in a normal manner.
[0016] The foregoing describes a technique for identifying serial digital video signals in a video system, thereby enabling verification of the routing of such signals through the video system.
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Incoming digital video signals to a video system each undergo identification with specific identifier prior to receipt at a corresponding one of the video system inputs. At each of the video system outputs, the output signal undergoes decoding to obtain the identity of the signal to confirm proper routing of signals within the video system.
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BACKGROUND OF THE DISCLOSURE
This invention relates to an apparatus and method for monitoring the stitching quality of sewing machines and, in particular, to detecting skipped stitches for Class 301 lockstitch sewing machines.
With the clothing industry becoming increasingly automated, there is a need for systems that monitor and regulate the functions and output of high speed sewing equipment. Certain of these systems are utilized to monitor the stitching of sewing machines to detect skipped stitches in apparel manufactured by Class 301 lockstitch sewing machines. The Class 301 lockstitch is employed in a wide range of areas within the apparel industry because it provides a fast, economical, and strong stitch.
In the general use of lockstitch type 301 sewing machines, improper stitches may from time to time be introduced in a workpiece. Generally, improper stitches may have the form of malformed stitches or skipped stitches. There are many causes of skipped stitches. Skipped stitches can develop from improper synchronization between the active elements within the sewing machine and the needle and bobbin thread loops. Normally, the bobbin hook catches the needle loop and brings the needle thread around the bobbin to form a lockstitch. Skipped stitches are most often formed when the bobbin hook fails to grasp the needle loop.
Malformed stitches are formed when the 301 stitch is not properly set. A stitch is properly set when the needle thread and the bobbin thread interlock in the center of the workpiece. A malformed stitch occurs when the stitch interlocks at either the top of the workpiece or the bottom of the workpiece.
In the prior art, skipped stitch detection systems are based upon monitoring the tension of the needle thread. As an example of this system, in U.S. Pat. No. 4,102,283 (Rockerarth et al.) the loss of thread tension generally is said to correspond to a skipped stitch, and this reduction in normal thread tension triggers a sensing device. The sensitivity of these systems ranges from complete loss of thread tension, for example due to the thread breaking, to sensing a momentary reduction in normal thread tension.
Other systems are based upon monitoring thread consumption, and may correlate thread consumption with total number of stitches, to detect a skipped stitch. As an example of this system, in U.S. Pat. No. 3,843,883 (DeVita et al., Oct. 22, 1974) a monitor is used to measure thread consumption which is then compared to a predetermined standard of thread use, deviation from which activates an output signal.
Another system used for detecting skipped stitches in a lockstitch type 301 sewing machine is disclosed in UK Patent Application No. GB 2008631. That system involves monitoring the length of a seam as compared with the upper thread consumption required to produce the seam. Actual thread consumption is then compared against a predetermined consumption value, any difference of which corresponds to an improperly formed seam. However, the difference in upper thread consumption between correct stitches and skipped stitches is not always substantial enough to be reliable in fast-rate sewing machines. This is best demonstrated when two pieces of thin fabric are being sewn together. Generally, measurements of the difference in thread consumption per stitch includes the thickness of two plies of fabric (assuming the stitch is set at center). For example, letting stitch length (SL)=0.125 inches, and ply thickness (PT)=0.01 inches, then the percentage decrease for a skipped stitch would be: 100 * [(2 * PT)/SL]=100 * [(2*0.010)/0.125]=16%. If thread tensions are not adjusted properly, this percent decrease could go to zero. Thus, there is a need for a direct, effective method of detecting skipped stitches in a fast-speed lockstitch type 301 sewing machine.
A primary shortcoming of the prior art is the unreliability of these systems at high sewing speeds, for example greater than 5,500 stitches per minute. DeVita states that the apparatus disclosed therein makes "mechanically possible the very high running speeds of about 2,000 stitches per minute desirable for such [lockstitch] sewing machines" (emphasis added). These systems fail to detect a momentary reduction of thread tension when the sewing machine is operating at high sewing speeds. The reduction in tension for an improper stitch at high sewing speeds tends to be less and in a range that the prior art fails to detect. As a result, these systems tend to be less reliable and thus fail to perform these functions with great accuracy.
There exists a need for better methods and systems for detecting skipped stitches that are reliable at high sewing speeds. To accommodate the advances in the clothing automation, particularly the increase in sewing speeds, it is an object of the invention to provide a simple, reliable system for detecting skipped stitches that would satisfy a substantial need in the art.
SUMMARY OF THE INVENTION
The present invention is a method and apparatus for detecting a skipped stitch for a Class 301 lockstitch sewing machine. Generally, that type of sewing machine includes an axially reciprocable needle adapted to incorporate one or more needle threads into a succession of Class 301 lockstitches and includes a rotatable bobbin assembly adapted for incorporating a bobbin thread into the lockstitches.
To detect skipped stitches, a monitor assembly determines the passage of the needle thread about the bobbin assembly during the formation of the lockstitches. A second monitor assembly determines the reciprocal movement of the needle by detecting rotation of a shaft which drives the needle. A processor identifies times when the rotational movement of the shaft does not correlate with passage of the needle thread about the bobbin assembly. Since the reciprocal movement of the needle as driven by the shaft enables the needle thread to pass around the bobbin assembly for the formation of a stitch, the identified times correspond to times when improper stitches have occurred.
In one form of the invention, the needle thread detection assembly includes an optical system having an emitter, a beamsplitter, a lens, a detector, and a reflective surface. Light is emitted from the emitter through both the beamsplitter and the lens onto the reflective surface. A detector then detects the passage of light. As the needle thread passes in front of the reflective surface, the amount of light acting upon the detector is decreased and detected by the detector. The absence of such a decrease in light during one stitch cycle indicates a skipped stitch.
In one form of the invention, the reflective surface is a retro-reflective tape which is adhered to the face of the bobbin assembly. In another form of the invention, the reflective surface is recessed below the face of the bobbin assembly.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other objects of this invention, the various features thereof, as well as the invention itself, may be more fully understood from the following description, when read together with the accompanying drawings in which:
FIG. 1A shows in diagrammatic form an exemplary series of proper Class 301 lockstitches;
FIG. 1B shows in diagrammatic form an exemplary skipped Class 301 lockstitch;
FIG. 2A shows a side elevation cut-away view of a sewing machine including a skipped stitch detection system embodying the present invention;
FIG. 2B shows a front elevation cut-away view of the system of FIG. 2A;
FIG. 2C shows the processor of the embodiment corresponding to FIG. 2A and FIG. 2B;
FIG. 3 shows a schematic representation of the thread monitor assembly of a skipped stitch detection system embodying the present invention; and
FIG. 4 shows a flow diagram of the system of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
A diagrammatic representation of Class 301 lockstitches is shown in FIG. 1A. FIGS. 2A and 2B show general representations of a lockstitch sewing machine, adapted to include the present invention. In FIG. 1A, a needle thread 12 generally runs along the top of an upper limp material segment 14a and a bobbin thread 16 generally runs along the bottom of segment 14b. In the illustrated stitch configuration, the needle thread loops 18 are shown with exaggerated width for clarity.
Both the needle thread 12 and the bobbin thread 16 periodically pass partially through one or both segments 14a and 14b, interlock to form the stitches, and then return to the respective top and bottom surfaces of segments 14a and 14b. The interlocking portions of the threads are referred to herein as loops. When the lockstitch is "correctly formed", the loops from the needle thread 12 and bobbin thread 16 interlock approximately mid-way between the top and bottom surfaces of segments 14a and 14b, as shown in FIG. 1A. An exemplary skipped stitch is shown in FIG. 1B.
In practice, the interlock point location may range all the way to either the top surface of segment 14a or the bottom surface of segment 14b, thereby forming "improper" stitches. The difference in needle thread 12 consumption between correct stitches and skipped, or improper, stitches is not always substantial enough to trigger an error or skipped stitch detector systems of the prior art, especially at the speeds of over 5,500 stitches per minute.
Referring now to FIG. 2A generally, in the formation of normal or correct lockstitches, the bobbin hook 124 of sewing machine 100 catches a needle loop and brings the needle thread 12 around the bobbin case 122. A skipped stitch is the result of the bobbin hook 124 failing to grasp the needle thread 12. Based upon this characteristic of skipped stitches, the present invention provides a method and apparatus, including a processor 162 for monitoring, on a continuous basis, the needle thread as it passes around the bobbin assembly of a lockstitch sewing machine as correlated with the rotation of the main drive shaft of the machine, as an indicator of a skipped stitch.
FIG. 2A shows a side elevation cut-away view of a sewing machine 100 including a skipped stitch detection system embodying the present invention. The sewing machine 100 includes a base member 102 having a planar workpiece support surface 104, and having a needle assembly 106 with a reciprocating needle 108 extending along a vertical needle axis 108a. The needle 108 receives needle thread 12 from a needle thread source (111 of FIG. 2B) by way of a tension assembly 110.
Beneath the support surface 104, a bobbin assembly 120 includes a bobbin case 122 which reciprocatingly rotates about axis 120a. The bobbin assembly 120 further includes a bobbin hook 124 for catching the needle thread 12 as it rotates around the bobbin case 122 to form a lockstitch. Also shown in FIG. 2A is a shaft monitor assembly 130 for detecting the rotation of the shaft 20 during the formation of a lockstitch. Monitor assembly 130 is discussed in further detail below. During proper operation of the sewing machine of the illustrated embodiment of FIGS. 2A and 2B, there is one needle thread pulse for every shaft revolution pulse which can be correlated by electronic means, or otherwise, with passage of the needle thread 12 about the bobbin assembly 120. Processor 162 identifies times corresponding to rotation of the output shaft for which no passage of needle thread about the bobbin assembly is detected.
As best shown in FIG. 2B, in a preferred embodiment of the invention, retro-reflective tape 134 is placed on the bobbin case 122, with a needle thread monitor assembly 132 proximately positioned thereto. In the preferred embodiment, the needle thread monitor assembly 132 is a control sensor. An example of such a sensor is schematically shown in FIG. 3, and includes a light emitter (LED) 152, beamsplitter 154, lens 156 and detector 158. Light from the emitter 152 passes through the beamsplitter 154 and the lens 156 to produce a spot of light on the retro-reflective tape, or other reflecting surface forming a target 160, at some distance from the lens 156. Light reflecting off this target 160 returns through the lens 156, then reflects off the beamsplitter 154 and onto the detector 158. The position and size of the optical components are selected to yield a 0.5 mm diameter spot size at a focus distance of 10.0 mm. This type of sensor is typically used with reflective surfaces. Any object that blocks the light returning from the reflective surface decreases the optical signal sensed at the detector 158.
Retro-reflective surfaces are particularly effective in reflecting a high percentage of incident light back toward the light source. The configuration of assembly 132 of FIG. 3 is such that the detector 158 optically appears to be occupying the space as the emitter 152 (or source). In the preferred embodiment, retro-reflective tape 134 is used as the target. The assembly 132 is positioned 10.0 mm from the tape 134 to give the desired yield as stated above. Normally, substantially all the energy from the emitter 152 reflects off of the retro-reflective tape 134, and back into the detector 158. When needle thread 12 passes over the target, i.e. around the bobbin case 122, the optical energy detected at 158 is decreased indicating passage of the thread 12 around the bobbin case 122.
In the preferred embodiment, the emitter is a light source. In other forms of the invention, sensors using other waveforms, e.g. acoustic, may be used. In an exemplary acoustic sensor system, an acoustic wave of specified frequency and amplitude may be directed to a reflective target surface. The interruption or disruption of such acoustic waves would indicate the passage of an object, such as a needle thread, through the wave front.
The processor 162 of the present invention may execute the process depicted by the flow diagram of FIG. 4. In that apparatus, the system receives input from the needle thread monitor assembly 132. If passage of the needle thread about the bobbin case is detected for a stitch (block 150) on a per stitch basis, thread pulse counter (TP) is set to one (block 170); if no thread is detected about the bobbin case, the thread pulse counter remains at zero. .The system then considers the shaft monitor assembly 130 (block 172). If a signal has been received which is indicative of a revolution of shaft 20, then the system tests whether the thread pulse counter is set to one (block 180). If so, then the thread pulse counter is reset to zero (block 190) and the system is recycled. If the thread pulse counter is at zero, an output error signal is generated (block 200) to indicate a skipped stitch. (See also FIG. 2C.)
In the illustrated embodiment, the retro-reflective tape is a discrete element positioned on the face (i.e. outer) surface of a conventional bobbin case. In an alternate form of the invention, the retro-reflective tape 134 may be positioned on a portion of the bobbin case that is recessed below the nominal face surface of the bobbin case, so that the thread will not rub against the tape 134 and wear it off the surface. In yet another form of the invention, the bobbin case itself may be used as the reflective surface, or target, with the monitor assembly 132 positioned accordingly.
In yet another form of the invention, the monitor assembly 132 could be a Hewlett-Packard HBCS-1100 high resolution optical reflective sensor. While described above in conjunction with the lockstitch type 301 sewing machine improper stitch detection system, the apparatus may be used on any sewing machine which uses a bobbin in forming a stitch. It may also be used alone in other applications in which it is adapted to accurately measure rapid motion of thread, or similar elongated, flexible material, about a bobbin-type assembly.
The invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
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The invention is a method and apparatus for detecting a skipped stitch for a Class 301 lockstitch sewing machine. A monitor assembly determines the passage of the needle thread about the bobbin assembly during formation of lockstitches. A second monitor assembly determines the reciprocal movement of the needle by detecting rotation of a shaft which drives the needle. A processor identifies times when the rotational movement of the shaft does not correlate with passage of the needle thread about the bobbin assembly.
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BACKGROUND OF THE INVENTION
This invention relates to a loading system for a material processing machine and more particularly to a system for transferring granular plastic materials into processing machines such as injection molding machines, extruders, blow molding machines and material dryers.
Machines for loading granular plastic materials into injection molding machines and the like have been available for a considerable period of time. Such machines normally include a large hopper assembly placed on top of injection molding machines and the like, making them very difficult to maintain and service.
In addition to the hopper, means are required for loading the hopper, normally an electrically driven vacuum motor. A number of problems have become manifest in the use of such machines. Typically the vacuum motor is very noisy, consumes considerable electricity and is dirty in that it blows fines of the material into the atmosphere. Such motors also require brushes that frequently wear out and have to be replaced. Frequently the machines currently in use also require expensive filter systems that have to be cleaned and replaced often. It is not unknown for such systems to become partially or entirely plugged, making it necessary to clean them out. They also have to be cleaned out after each run of a particular material to keep contamination to a minimum. Where such systems are on top of large hoppers on top of injection molding machines and the like, it becomes necessary for someone to climb up on the machine to effect the cleaning or maintenance. Sometimes machine components are broken, materials are spilled and wasted, or people are injured in falls in the course of effecting such cleaning because of the inaccessibility of such systems. It is, therefore, an object of the present invention to provide a loading system in which the loading process is considerably simplified and in which components for cleaning are readily accessible and easily handled from the floor.
Another area in which prior art machines appear to be unsatisfactory is that the various parts are not easily disassembled for cleaning. It is an object of the present invention to provide a material loading system in which the components are quickly and easily disassembled for cleaning by means of slip fit joints with O-ring seals.
Because of the fact that metal fragments and components sometimes find their way into the material it is known to provide a magnetic field somewhere in the system to trap such fragments and components. Disassembly to remove such metal fragments and components has generally involved a considerable expenditure of time. It is another object of the present invention to provide a material loading system including magnetic means in which the arrangement for removing such metal fragments and components is substantially facilitated.
Where there is an air driven system for transferring the granulated materials to the hopper from sources such as bags or barrels, it is frequently found that the conduit from the source to the hopper becomes plugged with material, frequently from packing and caking of the fines and/or chunks of material in the supply. It is therefore a further object of the present invention to provide an improved air driving system which is much less susceptible to such plugging.
In some applications it is desired to supply to the injection molding machine or the like, a mixture of two different kinds of such granular materials such as virgin plastic and regrind plastic. The usual system for accomplishing this mixture will load the virgin plastic for a few seconds and then load the regrind plastic for a few seconds. This builds up stratified layers of the separate materials in the hopper which causes process conditions to change from part to part and sometimes within the same part. As a result, the quality of the parts produced will vary, sometimes to an unacceptable degree. It is, therefore, a further object of the present invention to produce a material loading system in which a plurality of different granular materials can be supplied and blended together before being supplied to the associated machine.
Other objects and advantages will become apparent from consideration of the following specification taken in combination with the accompanying drawings.
BRIEF DESCRIPTION OF THE INVENTION
Applicants have designed a material transfer system particularly for handling granular plastic materials which are supplied to machines such as injection molding machines and the like, but which can also convey and load other lightweight granular materials, which meets the above objectives. By using a comparatively small lightweight pressure relief chamber combined with a reservoir sight glass assembly attached to each other with a slip fit quick disconnect means having O-rings sealing the joint, and with the sight glass assembly similarly connected to the machine mounting plate of the associated machine, removal and replacement for cleaning of both the pressure relief chamber and the reservoir sight glass assembly is facilitated. The filter unit which forms part of the pressure relief chamber is similarly easy to remove and olean and/or replace as required.
Applicants have provided an improved air driven material acceleration unit which, in addition to being quite efficient at moving material from a source such as a barrel or shipping container, also includes a separate air passage creating a certain amount of turbulence at the input to said unit which has proved effective in inhibiting the blocking or plugging of the unit by fines and/or large chunks in the material.
Applicant's loading system also includes a very simple magnetic structure attached to the reservoir sight glass assembly which creates a magnetic field across the assembly and which is effective to trap ferrous metal objects which might otherwise damage the associated machine. By using simple manually pivotable magnetic members, the magnetic field is easily interrupted to permit the metallic objects to be released from the reservoir sight glass assembly while it is removed from the machine mounting plate for cleaning.
Also attached to applicants'reservoir sight glass assembly is a sensor which effectively looks through the reservoir sight glass and distinguishes whether material is present in the reservoir sight glass assembly. This sensor is adjustable as to its level on the reservoir sight glass assembly and so can determine the starting charge of material and load the needed charge of material for the associated machine automatically. This also avoids the need for supplying a large hopper since the system can respond quickly to supply the amount of material needed to be supplied to the associated machine for each machine cycle.
BRIEF DESCRIPTION OF THE DRAWING
This invention may be more clearly understood from the following detailed description and by reference to the drawing in which:
FIG. 1 is a side view of an injection molding machine including material loading systems incorporating our invention;
FIG. 2 is an enlarged side view of one of the material loading systems of FIG. 1;
FIG. 3 is a perspective view of the accelerator tube and vortex unit shown in FIGS. 1 and 2;
FIG. 4 is a sectional drawing taken along line 4--4 of FIG. 3;
FIG. 5 is a further enlarged view, partly in section, of part of the structure of FIG. 2;
FIG. 6 is a perspective view of a magnetic unit used in association with the machine of FIGS. 2 and 5;
FIG. 7 is an exploded view, partly in section, of the reservoir sight glass assembly of FIGS. 2 and 5;
FIG. 8 is a perspective view of the reservoir sight glass unit of FIGS. 2 and 5 With the magnetic unit of FIG. 6 shown in an alternate position; and
FIG. 9 is a side view of an alternate embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1, an injection molding machine is shown at numeral 10 having an input chamber or throat 12 for receiving a desired amount of granular plastic material for each cycle of its operation. Connected to the input chamber or throat 12 is a loading system 13 including a pressure relief chamber 14 and a reservoir sight glass assembly 16 which receives material from the pressure relief chamber. A conduit 18 carries plastic material from a source, which in this case is a dryer 20, to a tangential inlet duct 21 on the pressure relief chamber 14. A sensor 22 fastened to the side of the reservoir sight glass assembly 16 is connected through an insulated wire 24 to an air pressure regulator 26 which controls the supply of air to an accelerator and vortex unit 28. Air supplied to the regulator 26 from a source, not shown, is controllable supplied, through an air hose 27 to accelerator and vortex unit 28. Material from dryer 20 is caused to flow by air pressure, through the acceleration and vortex unit 28 and through conduit 18 to the pressure relief chamber 14. When the material supplied reaches a desired level in reservoir sight glass assembly 16, this is sensed by sensor 22 which sends a signal to the air pressure regulator to shut off the air supplied through air hose 21 to the acceleration and vortex unit 28.
The dryer 20 which is carried on a separate cart 30, includes a blower and heating unit 32. Mounted on the top of dryer 20 is a second loading system 33 which includes a pressure relief chamber 14' and a reservoir sight glass assembly 16'. Transfer system 33 is essentially identical to transfer system 13 wherein identical parts will be given the same numerals plus a prime. A container 34 containing a supply of plastic granules is connected through a conduit 18' to pressure relief chamber 14'. Carried on cart 30 is an air pressure regulator 26' connected to an air pressure source (also not shown), to a sensor 22' on reservoir sight glass assembly 16' through a wire 24', and to an accelerator and vortex unit 28'. As described above, the sensor 22' on reservoir sight glass assembly 16' responds to the level of granulated plastic material in the reservoir sight glass assembly to cause air pressure regulator 26' to either supply air to the accelerator and vortex unit 28' to cause material to flow through conduit 18' to pressure relief chamber 14' or to shut off the supply of air and, hence, the flow of material to pressure relief chamber 14'. FIG. 1 shows a system in which two of my loading systems are shown connected in series. Details of one such system are discussed below.
FIG. 2 is an enlarged view showing part of loading system 13 in greater detail including pressure relief chamber 14 and reservoir sight glass assembly 16. The tangentially attached inlet duct 21 to which conduit 18 is attached is shown, as well as a filter unit 38 at the upper end of pressure relief chamber 14. A fastening bracket 40 provides means for securing and removing the filter unit 38.
Reservoir sight glass assembly 16 includes an upper end bell member 42 including a flange 44, a lower end bell member 46 including a flange 48, a sight glass 50 secured between the flanges and four support rods 52 which cooperate with a plurality of screws 53 (see FIG. 7) to hold the flanges 44 and 48 and reservoir sight glass 50 together. Secured to two of rods 52 is a magnetic unit including a bracket 54 and a pair of magnetic members 56, 58 (of which only member 56 is visible in this view) pivotally attached to bracket 54. A sensor 22 is fastened to the side of reservoir sight glass 50 by means of a bracket 60 adjustably secured to a pair of support rods 52 to control the level of material in the sight glass 50. Sensor 22 is connected through wire 24 to a switch 62 operating an air valve 64 forming part of air pressure regulator 26 which is connected to a source of compressed air through a hose 66. Air hose 27 is connected between air valve 64 and accelerator and vortex unit 28. At its opposite end from its connection to conduit 18, accelerator and vortex unit 28 is connected to a source of granular plastic material 68, which may be a barrel or other suitable container.
FIG. 3 is a perspective drawing of the accelerator and vortex unit 28, which includes a pipe 71 having an inlet port 70 connected to source 68 of granular plastic material and an outlet port 72 to which conduit 18 is connected. Pipe 71 has a slightly expanded diameter at its center covered with a collar 74 to which is attached an elbow 76. Air hose 27 is attached to elbow 76.
FIG. 4 is a sectional view taken along line 4--4 of FIG. 3. In this view it will be seen that the collar 74 covers an annular groove 78 on the surface of pipe 71 forming an annular chamber 80 communicating with the interior of elbow 76. Chamber 80 communicates with a series of passages 82 directing air toward outlet port 72. From inlet port 70 to the outlets of passages 82 is a venturi.
When air under pressure is supplied from regulator 26 through air hose 27 to the accelerator and vortex unit 28, a vacuum is created upstream of passages 82 which pulls the lightweight granular material from source 68 and causes it to flow through conduit 18 to pressure relief chamber 14. While the unit, as described, does operate, it has been found that over time, the fines and chunks of material have tended to collect and pack together near the inlet port 70. Applicants have provided a passageway 84 substantially smaller than the passage 82 which directs a small jet of air into the throat of the venturi to cause just enough turbulence at that point to inhibit and substantially prevent this packing together of the material.
FIG. 5 is a view of the pressure relief chamber 14 and reservoir sight glass assembly 16 shown partially in section and somewhat enlarged from the showing of FIG. 2. In this view the port 36 of the tangential inlet duct 21 is shown in the sidewall of pressure relief chamber 14. An interior cone 86 and a cylindrical baffle 88 formed in the top of pressure relief chamber 14 cause the flow from port 31 to be directed downwardly as shown by the arrow. In general the air flow will carry all the solids toward the bottom of the pressure relief chamber and into reservoir and sight glass assembly 16. Since the air must escape however, it flows through the passage at the center of baffle 88 and radially outwardly through the filter unit 38. Inevitably some fines will be carried by this air flow and they are blocked by the filter from escaping into the atmosphere. The filter 38 is readily removable for cleaning by loosening the screw on bracket 40 and sliding the filter laterally.
In this view of the reservoir sight glass assembly 16, the magnetic members 56 and 58 (only member 56 is visible in this view) are shown in the lowered position in which they create a significant magnetic field across the reservoir sight glass. A number of magnetic members such as a paper clip, a screw and a washer are shown held in this magnetic field.
The purpose of the magnetic members 56, 58 is to create a field in which ferrous metal contaminants may be caught and prevented from entering the associated machine. FIG. 6 is a perspective view of the magnetic assembly alone with members 5 and 58 shown in the lowered position creating a strong magnetic field between these members. Magnetic members 56 and 58 are pivotally attached to bracket 54. This view also shows screws 86 which are turned inward to secure the magnetic assembly to support rods 52 which pass through bores 87 in bracket 54.
An exploded view of the reservoir sight glass assembly 16 is shown in FIG. 7 with the sensor and the magnetic unit removed In this view it will be observed that the assembly consists of a sight glass tube 50 which is secured between upper and lower end bell members 42 and 46 respectively. Circular seal members 96 and 98 are positioned between the sight glass tube 50 and end bell members 42 and 46, respectively. A plurality of support rods 52 are bolted to the upper and lower end bell members 42,46 by means of a plurality of screws 53. In addition to grooves 100,102 for receiving seals 96 and 98 respectively, end bell members 42 and 46 include internal grooves 104 and 106, which receive O-rings 108 and 110 respectively and which provide an air tight seal against the lower end of the pressure relief chamber 14 and a fitting (not shown) on a mounting plate of the machine input chamber 12. Those skilled in the art will quickly recognize that with the reservoir sight glass assembly connected as described, the pressure relief chamber 14 may be easily disconnected from the top of the reservoir sight glass assembly 16 and the sight glass assembly is similarly easy to remove from the associated machine.
FIG. 8 is a perspective drawing of reservoir sight glass assembly 16 (with the sensor 22 removed) which is attached to pressure relief chamber 14 and to the input chamber or throat 12 of the machine 10 by the quick disconnect slip fit, O-ring sealed joints described above. When the view through the sight glass indicates that there are undesirable ferrous metal objects in the magnetic field between magnetic members 56 and 58, this assembly 16 may readily be removed (after shutting off the air supply) and the magnetic members 56 and 58 manually pivoted to the horizontal position shown which effectively removes the magnetic field, permitting the metallic objects, shown here as a washer, a paper clip, a screw and nut, to simply drop out of the assembly. At this point the pressure relief chamber 14 itself is readily disassembled for cleaning, if desired. The reservoir sight glass assembly 16 may then be quickly reattached to the pressure relief chamber 14 and throat 12, the air supply again turned on, until the level of material in the reservoir sight glass sensed by the sensor 22 is at the point where the sensor 22 will cause the air pressure regulator 26 to discontinue supplying more material to the pressure relief chamber 14.
From the foregoing it will be appreciated that the material loading system described herein affords some significant advantages over earlier systems presently in use. By using quick disconnect slip fit fittings with O-rings to connect the reservoir sight glass assembly 16 to the throat 12 and the pressure relief chamber 14, both the pressure relief chamber and reservoir sight glass assembly are easily removed, cleaned and replaced in the system. The pressure relief chamber 14 and the reservoir sight glass assembly 16 are relatively small and easily handled from the floor level so there is no need to climb up on the associated machine. By locating the magnetic members on the reservoir sight glass assembly, magnetic objects in the reservoir sight glass are easily seen, identified and removed. And the accelerator and vortex unit employed is quite effective to move the material from the source to the pressure relief chamber 14 without incurring the blockage caused by packing and caking of the material at the inlet port 70 which has been experienced in the past.
An additional embodiment of our invention is shown in FIG. 9. There are often circumstances wherein it is desired to supply the associated machine with a mix of different granular materials. One such situation occurs when it is desired to produce molded plastic parts from a mix of regrind plastic and virgin plastic. As described above, the usual current procedure is to supply a hopper with regrind plastic for a few seconds followed by virgin plastic for a few more seconds, repeating the process over and over. One problem with such a system is that the material builds up in the hopper in a series of stratified layers of different kinds of plastic which results in variations in the plastic content from part to part or within the same part.
In the embodiment of FIG. 9, the pressure relief chamber 114 is essentially the same as chamber 14, the filter structure is the same, and the difference is that there are two tangentially directed inlet ducts 118 and 120 fastened to the upper end of chamber 114. Chamber 114 is attached to the reservoir sight glass assembly 16 as described above. Attached to rods 52 of the assembly 16 are a sensor 22 and a magnetic assembly 54, both of which may be identical to the similar parts described above with respect to FIGS. 2 and 5. Sensor 22 is connected through a wire 124 to a control box 125 which receives signals from sensor 22 as described and transmits "on" or "off" signals through wires 119 and 120 simultaneously to each of two switches 161 and 162 respectively. Switch 161 controls operation of an air valve 163 forming part of an air pressure regulator 127 connected to a source of compressed air through a hose 166. An air hose 165 is connected between air valve 161 and an accelerator and vortex unit 129 which is connected to a source of granular plastic material 167, which may; for example, be a barrel containing regrind plastic.
Similarly, switch 162 controls operation of an air valve 126 connected to the air source at hose 166. Air valve 126 controls air flow through a hose 168 to an accelerator and vortex unit 128 which is connected to a source of granular plastic material 170 which may, for example, be a container containing virgin plastic material.
When sensor 22 "sees" material at the desired level in the sight glass, no signal is sent through wire 124 and, hence, no signal to switches 161 and 162, and no material flows through the passages 182 and 183 to the pressure relief chamber 114. When the material in the sight glass drops below the desired level, the sensor 22 sends a signal through wire 124 to control box 125 which relays the signal to both of switches 161 and 162, actuating switches 163 and 164. This causes air under pressure to be delivered simultaneously to both of the accelerator and vortex units 128 and 129 producing an essentially identical quantity of flow of plastic material through passages 182 and 183 to inlet ducts 118 and 120. This results in an even mix of regrind and virgin plastic in chamber 114 and supplied to reservoir and sight glass assembly 16. Should a different proportion of materials be preferred, this may be effected by varying the air pressure by adjusting regulators 126 and 127 as desired.
The above described embodiments of the present invention are merely descriptive of its principles and are not to be considered limiting. The scope of the present invention instead shall be determined from the scope of the following claims including their equivalents.
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A material transfer system for loading lightweight granular plastic material into injection molding machines and the like includes a reservoir sight glass assembly connected to the associated machine and a lightweight pressure relief chamber attached to the reservoir sight glass assembly, both connections being by quick disconnect devices. The reservoir sight glass assembly includes, a sensor which responds to the level of material in the sight glass and a magnet assembly which traps ferrous contaminates and prevents their entering the machine. The flow of material to the pressure relief chamber is controlled by the sensor which turns a regulated source of compressed air on or off depending upon the level of material in the sight glass. The air source is connected to an accelerator and vortex unit which is, in turn, connected to a source of the material. When air is supplied to the accelerator and vortex unit, it is injected into the downstream side of a venturi causing a vacuum which pulls the material into the air stream and then carries it to the pressure relief chamber. To avoid packing and caking of the fines at the throat of the venturi, a small reverse air flow jet is included to provide some turbulence at the venturi input.
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CROSS REFERENCE TO RELATED APPLICATION
[0001] This application is a continuation of U.S. patent application Ser. No. 12/010,033, filed Jan. 18, 2003, now pending, which claims priority to the disclosure of Japanese Patent Application No. 2007-283445, filed Oct. 31, 2007. The entire content of both of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a calibration of a weight measuring apparatus, and more particularly to a weight applying unit for performing a calibration on a weight measuring apparatus comprising a plurality of load sensors and a weight applying method of performing the same.
[0004] 2. Description of the Background Art
[0005] In a weight measuring apparatus, using a load sensor, which is typified by a scale or the like, a calibration is performed on a load sensor-integrated weight measuring apparatus as a finished product, in order to improve an accuracy of measurement results. As a calibration method used for a weight measuring apparatus using a single load sensor, for example, a specific load of a weight is placed on a load platform at a center position thereof, and a calibration is performed based on a detected output of the load sensor. Also, there may be another weight measuring apparatus in which a single load platform is supported by a plurality of load sensors, and detected outputs of the plurality of respective load sensors are added to each other so as to obtain a weight value. Similarly to the weight measuring apparatus using the single load sensor, as a calibration method used for said another weight measuring apparatus comprising the plurality of load sensors, a specific load of a weight is placed on the load platform at a center position thereof, and a calibration is performed based on a total value of the detected outputs of the respective load sensors. Furthermore, as another calibration method, specific loads of weights are respectively placed on a load platform at predetermined positions such as four corners of the load platform, thereby performing a calibration based on detected outputs of the respective load sensors (Japanese Laid-Open Patent Publication No. 3-25325, for example).
[0006] In recent years, in the field of home fitness apparatuses or video games, when using the weight measuring apparatus comprising the plurality of load sensors, for example, it is requested that the weight measuring apparatus not only output the weight of a to-be-measured object placed on a load platform, but also recognize a balance state of the to-be-measured object such as the postural balance of a person on the load platform. In order to recognize the balance state of the to-be-measured object (e.g., a state where a human stands on his or her right foot and a greater amount of load is applied to a right side of the load platform), loads applied to the plurality of load sensors must be individually obtained. Further, in order to improve an accuracy of measurement results detected by the respective load sensors, a calibration must be performed on each of the load sensors, instead of performing the calibration based on the total value of the detected outputs of the respective load sensors.
[0007] In such a weight measuring apparatus integrated with the plurality of load sensors, as a method of performing a calibration on each of the load sensors, there may be a method in which the specific loads of the weights are placed on a load platform in respective four corners thereof, thereby performing the calibration on each of the load sensors based on an output of each of the load sensors (not based on the total value of the outputs of the respective load sensors), as disclosed in Japanese Laid-Open Patent Publication No. 3-25325.
[0008] However, in the aforementioned calibration method in which the weights are respectively placed in the four corners of the load platform, the weights are placed on the load platform, and therefore a load of each of the weights, which naturally should be applied in a perpendicular direction, is to be dispersed in other directions. For example, in the case of a weight measuring apparatus in which a load platform is supported by two load sensors 91 and 92 as shown in FIG. 17 , it is assumed that a weight of 50 kg is placed on the load platform at a right side thereof. In this case, a value of 40 kg is detected in the load sensor 92 located under the weight, while a value of 10 kg is detected in the other load sensor 31 , for example. That is, a load of 50 kg is distributed between the two load sensors. Furthermore, the value of 40 kg or 10 kg is used as an example in FIG. 17 in order to facilitate the description. In practice, however, it is difficult to accurately recognize how and in which direction the load of 50 kg is dispersed. Therefore, in such a calibration method, when a calibration is performed on each of the load sensors, it is extremely difficult to perform a proper calibration.
SUMMARY OF THE INVENTION
[0009] Therefore, an object of the present invention is to provide a weight applying unit for calibration and a weight applying method for calibration, both of which are capable of performing, in a weight measuring apparatus comprising a plurality of load sensors, a proper calibration on each of the load sensors.
[0010] The present invention has the following features to attain the object mentioned above. Note that reference numerals and figure numbers are shown in parentheses below for assisting a reader in finding corresponding components in the figures to facilitate the understanding of the present invention, but they are in no way intended to restrict the scope of the invention.
[0011] A first aspect is a weight applying unit for calibration used for performing a calibration on a weight measuring apparatus in which a load platform is supported by a plurality of load sensor sections and a weight of a measurement target object placed on the load platform is measured based on a load value detected by each of the plurality of load sensor sections, the weight applying unit for calibration comprising: a support section ( 51 ) and a weight applying section ( 53 ). The support section supports the weight measuring apparatus. The weight applying section applies predetermined loads to the plurality of load sensor sections, respectively.
[0012] According to the first aspect, a load can be individually applied to each of the plurality of load sensor sections.
[0013] In a second aspect based on the first aspect, the support section supports a load platform surface of the weight measuring apparatus such that the load platform surface is in a horizontal position. The weight applying section applies the predetermined loads to the plurality of load sensor sections, respectively, in a direction perpendicular to the load platform surface.
[0014] According to the second aspect, the load is applied in the direction perpendicular to the load platform surface. Thus, the load can be prevented from being dispersed, thereby making it possible to easily and assuredly apply the load.
[0015] In a third aspect based on the second aspect, the support section supports the weight measuring apparatus such that the load platform surface of the weight measuring apparatus faces a gravitational direction. The weight applying section applies the predetermined loads in a downward direction.
[0016] According to the third aspect, the load is applied in the gravitational direction. Thus, the load is not to be dispersed, thereby making it possible to more assuredly apply the load.
[0017] In a fourth aspect based on the first aspect, values of the predetermined loads applied by the weight applying section to the plurality of load sensor sections, respectively, are the same as one another.
[0018] According to the fourth aspect, the loads having the same value as one another are applied to the plurality of load sensor sections, respectively. Thus, it becomes possible to perform a calibration on each of the load sensor sections under the same condition.
[0019] In a fifth aspect based on the first aspect, the weight applying unit for calibration further comprises a deflection generating portion ( 61 ) for generating deflection by applying a predetermined pressure to a load platform surface of the weight measuring apparatus.
[0020] According to the fifth aspect, the load can be applied assuming a condition where the weight measuring apparatus is actually used (i.e., where the deflection is generated). Thus, it becomes possible to perform a more proper calibration.
[0021] In a sixth aspect based on the fifth aspect, the support section has a placement table for placing the weight measuring apparatus thereon. The weight measuring apparatus is placed on the placement table such that the load platform surface of the weight measuring apparatus and a load surface of the placement table face horizontally toward each other. Further, the deflection generating portion is a elastic body disposed so as to be interposed between the load surface of the placement table and the load platform surface of the weight measuring apparatus.
[0022] According to the sixth aspect, the condition where the weight measuring apparatus is actually used can be easily created. Furthermore, since the elastic body is used, even if a press is applied to an end of the deflection generating portion, the generated deflection of the weight measuring apparatus can be prevented from being hampered. Still furthermore, it becomes possible to prevent the load platform surface of the weight measuring apparatus from being damaged through calibration steps.
[0023] In a seventh aspect base on the sixth aspect, the deflection generating portion is an elastic body having a shape simulating an area in which the measurement target object contacts the load platform.
[0024] In an eighth aspect based on the sixth aspect, the deflection generating portion is an elastic body having a Shore hardness of Shore A70.
[0025] According to the seventh and eighth aspects, the deflection more similar to that under actual usage conditions can be generated.
[0026] In a ninth aspect based on the sixth aspect, the deflection generating portion is made of ester polyurethane.
[0027] According to the ninth aspect, even if a pressure is applied to an end of the deflection generating portion, the generated deflection of the weight measuring apparatus can be prevented from being hampered. Furthermore, it becomes possible to prevent the load platform surface of the weight measuring apparatus from being damaged through the calibration steps.
[0028] In a tenth aspect based on the second aspect, the weight applying unit for calibration further comprises a deflection generating portion ( 61 ) for generating deflection by applying a predetermined pressure to a load platform surface of the weight measuring apparatus.
[0029] According to the tenth aspect, it becomes possible to obtain an effect similar to that of the fifth aspect.
[0030] In an eleventh aspect based on the tenth aspect, the support section has a placement table for placing the weight measuring apparatus thereon. The weight measuring apparatus is placed on the placement table such that the load platform surface of the weight measuring apparatus and a load surface of the placement table face horizontally toward each other. Furthermore, the deflection generating portion is an elastic body disposed so as to be interposed between the load surface of the placement table and the load platform surface of the weight measuring apparatus.
[0031] According to the eleventh aspect, it becomes possible to obtain an effect similar to that of the sixth aspect.
[0032] In a twelfth aspect based on the eleventh aspect, the deflection generating portion is an elastic body having a shape simulating an area in which the measurement target object contacts the load platform.
[0033] According to the twelfth aspect, it becomes possible to obtain an effect similar to that of the seventh aspect.
[0034] In a thirteenth aspect based on the third aspect, the weight applying unit for calibration further comprises a deflection generating portion ( 61 ) for generating deflection by applying a predetermined pressure to the load platform surface of the weight measuring apparatus.
[0035] According to the thirteenth aspect, it becomes possible to obtain an effect similar to that of the fifth aspect.
[0036] In a fourteenth aspect based on the thirteenth aspect, the support section has a placement table for placing the weight measuring apparatus thereon. The weight measuring apparatus is placed on the placement table such that the load platform surface of the weight measuring apparatus and a load surface of the placement table face horizontally toward each other. Furthermore, the deflection generating portion is an elastic body disposed so as to be interposed between the load surface of the placement table and the load platform surface of the weight measuring apparatus.
[0037] According to the fourteenth aspect, it becomes possible to obtain an effect similar to that of the sixth aspect.
[0038] In a fifteenth aspect based on the fourteenth aspect, the deflection generating portion is an elastic body having a shape simulating an area in which the measurement target object contacts the load platform.
[0039] According to the fifteenth aspect, it becomes possible to obtain an effect similar to that of the seventh aspect.
[0040] In a sixteenth aspect based on the fourth aspect, the weight applying unit for calibration further comprises a deflection generating portion ( 61 ) for generating deflection by applying a predetermined pressure to a load platform surface of the weight measuring apparatus.
[0041] According to the sixteenth aspect, it becomes possible to obtain an effect similar to that of the fifth aspect.
[0042] In a seventeenth aspect based on the sixteenth aspect, the support section has a placement table for placing the weight measuring apparatus thereon. The weight measuring apparatus is placed on the placement table such that the load platform surface of the weight measuring apparatus and a load surface of the placement table face horizontally toward each other. Furthermore, the deflection generating portion is an elastic body disposed so as to be interposed between the load surface of the placement table and the load platform surface of the weight measuring apparatus.
[0043] According to the seventeenth aspect, it becomes possible to obtain an effect similar to that of the sixth aspect.
[0044] In an eighteenth aspect based on the seventeenth aspect, the deflection generating portion is an elastic body having a shape simulating an area in which the measurement target object contacts the load platform.
[0045] According to the eighteenth aspect, it becomes possible to obtain an effect similar to that of the seventh aspect.
[0046] In a nineteenth aspect based on the first aspect, the weight applying unit for calibration further comprises a detection value obtaining section and a setting section. The detection value obtaining section obtains a detection value outputted from each of the plurality of load sensor sections to which the predetermined loads are applied, respectively, by the weight applying section. The setting section sets the detection value obtained by the detection value obtaining section in the weight measuring apparatus so as to be associated with each of the load sensor sections which has outputted the detection value.
[0047] In a twentieth aspect based on the nineteenth aspect, the weight applying section can calibrate the load value applied to each of the plurality of load sensor sections. The setting section sets, in the weight measuring apparatus, data detected based on a plurality of load values by applying loads having values different from each other.
[0048] According to the nineteenth and twentieth aspects, it becomes possible to cause the weight measuring apparatus to store calibration results, thereby improving usability of the weight applying unit for calibration.
[0049] A twenty-first aspect is a weight applying method for calibration used for performing a calibration on a weight measuring apparatus in which a load platform is supported by a plurality of load sensor sections, and a calculation process is performed on a load value detected by each of the plurality of load sensor sections so as to measure a weight of a measurement target object placed on the load platform, the weight applying method for calibration comprising: a supporting step (step 1 ); and a weight applying step (step 4 , 5 ). The supporting step supports the weight measuring apparatus. The weight applying step respectively applies predetermined loads to the plurality of load sensor sections included in the weight measuring apparatus supported by the supporting step.
[0050] According to the twenty-first aspect, it becomes possible to obtain an effect similar to that of the first aspect.
[0051] According to the present invention, a load can be applied individually to each of the plurality of load sensor sections. Thus, it becomes possible to perform a more proper calibration on each of the load sensor sections.
[0052] These and other objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0053] FIG. 1 is a diagram describing a principle of a weight applying/calibration method according to the present invention;
[0054] FIG. 2 is another diagram describing the principle of the weight applying/calibration method according to the present invention;
[0055] FIG. 3A is a diagram illustrating an example of an external view of a weight measuring apparatus 10 according to embodiments of the present embodiment;
[0056] FIG. 3B is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0057] FIG. 3C is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0058] FIG. 3D is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0059] FIG. 3E is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0060] FIG. 3F is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0061] FIG. 3G is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0062] FIG. 3H is a diagram illustrating the example of the external view of the weight measuring apparatus 10 according to embodiments of the present embodiment;
[0063] FIG. 4A is a diagram illustrating an example of a structure of a load sensor section 12 ;
[0064] FIG. 4B is a diagram illustrating the example of the structure of the load sensor section 12 ;
[0065] FIG. 4C is a diagram illustrating the example of the structure of the load sensor section 12 ;
[0066] FIG. 4D is a diagram illustrating the example of the structure of the load sensor section 12 ;
[0067] FIG. 5 is a diagram illustrating the interior of the weight measuring apparatus 10 according to the embodiments of the present invention;
[0068] FIG. 6 is a diagram illustrating an example of an electrical configuration of the weight measuring apparatus 10 according to the embodiments of the present invention;
[0069] FIG. 7A is a diagram schematically illustrating an example of a weight applying unit 50 according to the embodiments of the present invention;
[0070] FIG. 7B is a diagram schematically illustrating the example of the weight applying unit 50 according to the embodiments of the present invention;
[0071] FIG. 7C is a diagram schematically illustrating the example of the weight applying unit 50 according to the embodiments of the present invention;
[0072] FIG. 7D is a diagram schematically illustrating the example of the weight applying unit 50 according to the embodiments of the present invention;
[0073] FIG. 8A is a diagram illustrating a state where the weight measuring apparatus 10 is placed on a placement table 51 ;
[0074] FIG. 8B is a diagram illustrating the state where the weight measuring apparatus 10 is placed on a placement table 51 ;
[0075] FIG. 9 shows an example of data stored in a microcomputer 31 ;
[0076] FIG. 10 is a schematic diagram illustrating a state where the weight measuring apparatus 10 is actually used;
[0077] FIG. 11 is a schematic diagram illustrating a state where a load cell is actually used;
[0078] FIG. 12 is a schematic diagram illustrating a state where the weight measuring apparatus 10 is placed on the placement table 51 with a deflection generating member 61 interposed therebetween;
[0079] FIG. 13 is a schematic diagram illustrating a state where a load is applied with the deflection generating member 61 interposed between the weight measuring apparatus 10 and the placement table 51 ;
[0080] FIG. 14 is a diagram illustrating an example of the deflection generating member 61 ;
[0081] FIG. 15 is a table showing measurement results obtained when using the weight measuring apparatus 10 on which a calibration is performed by a method according to a first embodiment;
[0082] FIG. 16 is a table showing measurement results obtained when using the weight measuring apparatus 10 on which the calibration is performed by a method according to a second embodiment; and
[0083] FIG. 17 is a diagram illustrating an example of values detected by load sensors when a weight is placed on a load platform.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
First Embodiment
[0084] Hereinafter, embodiments of the present invention will be described with reference to the drawings. Note that the embodiments to be described below are not limited to the present invention.
[0085] Firstly, a principle of a weight applying/calibration method according to a first embodiment will be described. As shown in FIG. 1 , in a conventional weight applying/calibration method in which a weight is placed on a load platform with a plurality of load sensors (i.e., leg portions) of a weight measuring apparatus facing downward, one load is distributed among the plurality of load sensors, and thus a proper calibration cannot be performed. On the other hand, according to the present invention, instead of performing a calibration by placing a weight on the load platform so as to indirectly apply weight to the load sensors, the calibration is performed by directly applying the weight to load sensor sections 12 . That is to say, as shown in FIG. 2 , the calibration is performed by applying weight to one load sensor in such a manner that the weight applied to the one load sensor is assuredly not to be distributed with the other load sensor.
[0086] Hereinafter, the weight applying/calibration method according to the first embodiment will be described in detail. FIG. 3A is a diagram illustrating an example of an external view of a weight measuring apparatus 10 (a scale, typically). FIG. 3B is a left side view illustrating the example of the external view of the weight measuring apparatus 10 . FIG. 3C is a right side view illustrating the example of the external view of the weight measuring apparatus 10 . FIG. 3D is a front view illustrating the example of the external view of the weight measuring apparatus 10 . FIG. 3E is a back view illustrating the example of the external view of the weight measuring apparatus 10 . FIG. 3F is a bottom view illustrating the example of the external view of the weight measuring apparatus 10 . FIG. 3G is a perspective view as viewed from a top of the weight measuring apparatus 10 . FIG. 3H is a perspective view as viewed from a bottom of the weight measuring apparatus 10 . The weight measuring apparatus 10 comprises a load platform 11 on which a user stands, the four load sensor sections 12 respectively provided on a bottom surface of the load platform 11 in four corners thereof, and a connector 13 connectable to a predetermined external apparatus.
[0087] Each of the load sensor sections 12 detects a load applied to the load platform 11 . FIG. 4A is an exploded view illustrating an example of a structure of each of the load sensor sections 12 . FIG. 4B is a perspective view illustrating the example of the structure of each of the load sensor sections 12 . FIG. 4C is a top view illustrating the example of the structure of each of the load sensor sections 12 . FIG. 4D is a cross-sectional view along lines A-A shown in FIG. 4C . In FIGS. 4A to 4D , each of the load sensor sections 12 includes an upper plate 22 , a load cell 23 , a lower plate 24 , screws 21 and 25 , a load receiving plate 26 , a housing 27 , and a rubber leg 28 . As shown in FIG. 4A , the load cell 23 is disposed so as to be interposed between the upper plate 22 and the lower plate 24 . The screw 21 is inserted so as to pass through a hole provided with the upper plate 22 and a hole, corresponding to the hole of the upper plate 22 , which is provided with the load cell 23 . Similarly, the screw 25 is inserted so as to pass through a hole provided with the lower plate 24 , and a hole, corresponding to the hole of the lower plate 24 , which is provided with the load cell 23 . Thus, the load cell 23 is fixed by means of the upper plate 22 and the lower plate 24 . Furthermore, the load receiving plate 26 is disposed in a center portion of the interior of the housing 27 , and the load cell 23 fixed by means of the upper plate 22 and the lower plate 24 is disposed above the load receiving plate 26 . The rubber leg 28 is disposed in a center portion of a bottom surface of the housing 27 .
[0088] The load cell 23 is a strain gage type load cell, for example. The load cell 23 is a load conversion unit for converting an inputted load into an electrical signal. In the load cell 23 , a strain element 23 a is deformed in accordance with the inputted load, thereby generating a strain. A strain sensor 23 b attached to the strain element 23 a converts the strain into a value indicating an electrical resistance change so as to be further converted into a value indicating a voltage change. Therefore, the load cell 23 outputs a voltage signal indicating the inputted load from an input terminal when a voltage is applied from a power terminal.
[0089] The housing 27 is formed so as to have a substantially bottomed cylindrical shape by plastic molding, for example.
[0090] FIG. 5 is a perspective view illustrating the interior of the weight measuring apparatus 10 . In FIG. 5 , a frame 15 , disposed along the periphery of the weight measuring apparatus 10 , acts as a skeletal structure of the weight measuring apparatus 10 . Furthermore, a microcomputer board 14 , on which a microcomputer 31 to be described later is mounted, is located in the interior of the weight measuring apparatus 10 . The microcomputer board 14 is electrically connected to the four load sensor sections 12 (more precisely, the load cells 23 ) respectively provided in the four corners of the weight measuring apparatus 10 and the connector 13 .
[0091] FIG. 6 is a diagram illustrating an example of an electrical configuration of the weight measuring apparatus 10 . In FIG. 6 , solid-line arrows indicate signal and communication flows, and dashed-line arrows indicate a power supply.
[0092] The weight measuring apparatus 10 further comprises the microcomputer 31 for controlling an operation thereof. The microcomputer 31 includes a ROM, RAM and the like, all of which are not shown, and controls the operation of the weight measuring apparatus 10 in accordance with a program stored in the ROM. Further, the RAM is, for example, a nonvolatile memory such as a flash memory.
[0093] An AD converter 32 , the connector 13 and a DC-DC converter 33 are connected to the microcomputer 31 . The load cells 23 included in the load sensor sections 12 , respectively, are connected to the AD converter 32 via respective amplifiers 34 .
[0094] The connector 13 is provided so as to allow the weight measuring apparatus 10 to communicate with the predetermined external apparatus such as a personal computer or a game apparatus.
[0095] Furthermore, a battery 35 is mounted in the weight measuring apparatus 10 for a power supply. In the present embodiment, the external apparatus connected to the weight measuring apparatus 10 by means of the connector 13 controls a power supply to the microcomputer 31 . On the other hand, the microcomputer 31 controls a power supply to the load cells 23 , the amplifiers 34 and the AD converter 32 . To the load cells 23 , the amplifiers 34 , the microcomputer 31 and the AD converter 32 , a power is supplied from the battery 35 via the DC-DC converter 33 . The DC-DC converter 33 converts a voltage value of a DC current drawn from the battery 35 into a different voltage value, so as to be outputted to the load cells 23 , the amplifiers 34 , the microcomputer 31 and the AD converter 32 .
[0096] When a power is supplied, each of the load cells 23 outputs a signal indicating the inputted load. The signal is amplified by each of the amplifiers 34 , and the amplified analog signal is converted by the AD converter 32 into a digital signal so as to be inputted to the microcomputer 31 . Identification information of each load cell 23 is assigned to a detection value of the load cell 23 so as to be distinguishable from detection values of the other load cells 23 . As described above, the microcomputer 31 can obtain data indicating the detection values of the four respective load cells 23 at the same time. Then, the data indicating the detection values of the respective load cells 23 is transmitted from the microcomputer 31 to the external apparatus via the connector 13 .
[0097] Next, a weight applying unit used in the first embodiment will be described. The weight applying unit is used for applying weight to the load sensor sections 12 . FIG. 7A is a front view schematically illustrating a weight applying unit 50 . FIG. 7B is a plan view schematically illustrating the weight applying unit 50 . FIG. 7C is a right side view schematically illustrating the weight applying unit 50 . FIG. 7D is a left side view schematically illustrating the weight applying unit 50 .
[0098] In FIGS. 7A to 7D , the weight applying unit 50 comprises a placement table 51 , leg portions 52 for supporting the placement table 51 , four hook portions 53 a to 53 d mounted so as to perpendicularly penetrate the placement table 51 , a plurality of weights 54 a to 54 d detachable from the four hook portions 53 a to 53 d , respectively, and four hoisting and lowering mechanisms 55 a to 55 d disposed at positions corresponding to the hook portions 53 a to 53 d , respectively.
[0099] Furthermore, as shown in FIG. 7B , the placement table 51 has four through holes 56 a to 56 d provided therethrough. Each through hole 56 is provided at a position corresponding to each of the four corners of the weight measuring apparatus 10 placed on the placement table 51 , that is, a position corresponding to a position of each of the load sensor sections 12 .
[0100] The four hook portions 53 a to 53 d have circular shaped load applying plates 531 a to 531 d , and attachment portions 532 a to 532 d for attaching the weights 54 thereto, respectively. As shown in FIG. 7A or the like, each of the hook portions 53 is disposed through the through hole 56 such that the load applying plate 531 is located above the placement table and the attachment portion 532 is located below the placement table 51 . That is, when each of the weights 54 is attached to the attachment portion 532 , the entirety of the hook portion 53 is perpendicularly lowered by the weight of the attached weight 54 .
[0101] Each of the weights 54 is detachable from the attachment portion 532 . Furthermore, each weight 54 is formed of a plurality of weight parts ( 541 to 544 in FIG. 7A ), and the weight applied to the hook portion 53 is adjustable depending on the number of the weight parts attached to the attachment portion.
[0102] Each of the hoisting and lowering mechanisms 55 is used to carry the weight 54 in an up and down direction when performing a process of attaching the weight 54 to the attachment portion 532 .
[0103] Next, the weight applying/calibration method according to the first embodiment will be described. In the first embodiment, a load is directly applied to each of the load sensor sections 12 in such a manner as described above so as to cause the microcomputer 31 of the weight measuring apparatus 10 to store a value outputted from each of the load sensor sections 12 , thereby performing a calibration.
[0104] Firstly, the weight measuring apparatus 10 is placed on the placement table 51 with a load platform surface of the weight measuring apparatus 10 facing downward (i.e., in an inverted position) (step 1 ). At this time, the weight measuring apparatus 10 is placed on the placement table 51 such that the load sensor sections 12 are located at positions where the through holes 56 a to 56 d are provided, respectively. In other words, the weight measuring apparatus 10 is placed on the placement table 51 such that the load sensor sections 12 a to 12 d are located under the load applying plate 531 a to 531 d of the hook portions 53 a to 53 d , respectively. FIG. 8A is a front view illustrating a state where the weight measuring apparatus 10 is placed on the placement table 11 . FIG. 8B is a plan view illustrating the state where the weight measuring apparatus 10 is placed on the placement table 11 .
[0105] Then, the connector 13 is connected to the external apparatus (step 2 ). The external apparatus is used for monitoring a load value outputted from the weight measuring apparatus 10 and causing the microcomputer 31 to write the load value, for example.
[0106] Next, in a state where no load (i.e., 0 kg) is applied to each of the load sensor sections 12 , a detection value thereof is obtained. Thereafter, the external apparatus causes a RAM of the microcomputer 31 to store the detection value so as to be associated with each of the load sensor sections 12 (step 3 ).
[0107] Then, each of the hoisting and lowering mechanisms 55 is used to lift the weight 54 , and the weight 54 having a predetermined weight (e.g., 17 kg) is attached to the attachment portion 532 of each of the four hook portions 53 (step 4 ). In this state, the weight 54 is supported by each of the hoisting and lowering mechanisms 55 . Note that it is preferable that the weights 54 attached to the hook portions 53 , respectively, have the same weight as one another.
[0108] Next, after attaching the weights 54 to the hook portions 53 , respectively, the hoisting and lowering mechanisms 55 are used to simultaneously bring down the weights 54 attached at four locations, respectively (step 5 ). In this state, the weight 54 attached to each of the hook portions 53 is not supported by the hoisting and lowering mechanism 55 . As a result, each of the hook portions 53 is lowered by the weight of the weight 54 , and the load applying plate 531 contacts each of the load sensor sections 12 located so as to be opposed thereto, thereby pressing down each of the load sensor sections 12 . Thus, it becomes possible to directly apply a load corresponding to the weight of the weight 54 attached to each of the hook portions 53 to each of the load sensor sections 12 .
[0109] Then, the external apparatus obtains the detection value outputted from each of the load sensor sections 12 . Thereafter, the external apparatus causes the RAM of the microcomputer 31 to store the detection value as information on the weight of the currently attached weight 54 (i.e., as a detection value obtained when a load of 17 kg is applied) so as to be associated with each of the load sensor sections 12 (step 6 ).
[0110] Such a process of applying a desired load to each of the load sensor sections 12 and causing the microcomputer 31 to store a detection value of each of the load sensor sections 12 to which the desired load is currently applied (steps 4 to mentioned above) is repeated by using a load having a desired weight value. For example, loads of 34 kg, 68 kg and 102 kg are sequentially applied to each of the load sensor sections 12 , and the microcomputer 31 is caused to store a detection value detected when each of the loads is applied to each of the load sensor sections 12 . FIG. 9 shows an example of data stored in the RAM of the microcomputer 31 as a result of such a process. In FIG. 9 , data, indicating a detection value outputted from each load cell 23 each time a load having a predetermined weight is applied, is stored for each of the load sensor sections 12 . Note that in FIG. 9 , the data indicating the detection value outputted from the load cell 23 is represented as an AD converted value. As such, the calibration according to the first embodiment is finished.
[0111] When the weight measuring apparatus 10 calibrated in such a manner as described above is actually used, a value detected by each of the load sensor sections 12 and the data as shown in FIG. 9 are used. For example, in the external apparatus (e.g., a game apparatus) connected to the weight measuring apparatus 10 , the detection value of each of the load sensor sections 12 and the data shown in FIG. 9 are obtained from the weight measuring apparatus 10 . Thereafter, a predetermined calculation process is performed based on the aforementioned value and data, thereby calculating the weight.
[0112] As described above, in the present embodiment, a load can be independently applied to each of the four load sensor sections 12 . Thus, a more proper calibration can be performed on each of the load sensor sections 12 , thereby making it possible to improve a measurement accuracy of the weight measuring apparatus 10 . As a result, in the case where a balance state of a measurement target object is detected based on an output value of each of the load sensors, for example, it becomes possible to more accurately recognize the balance state of the measurement target object.
[0113] In the above embodiment, as a mechanism to apply a load to each of the load sensor sections 12 , the weight measuring apparatus 10 is placed on the placement table 51 in an inverted position, and then the weight 54 is attached to the hook portion 53 , thereby applying a load to each of the load sensor sections 12 . However, the present invention is not limited thereto. Other mechanisms may also be used if they directly apply a load to each of the load sensor sections 12 . For example, the weight measuring apparatus 10 may be placed on the placement table 51 without being inverted such that a load is applied to each of the load sensor sections 12 through the through hole 56 so as to press up the weight measuring apparatus 10 from below.
[0114] In the above embodiment, the external apparatus is used to cause the microcomputer 31 to store the data indicating the detection value outputted from the load cell 23 . However, a function corresponding to the external apparatus may be embedded in the weight applying unit 50 . For example, a connection section electrically connectable to the connector 13 of the weight measuring apparatus 10 , a control section having a calculation control function such as a CPU, and an operation section for transmitting an instruction to the control section may be mounted in the weight applying unit 50 . Then, a process as shown in step 6 mentioned above may be performed by means of the control section. In such an example as described above, it is unnecessary to prepare an external apparatus in a separate manner.
Second Embodiment
[0115] Next, a second embodiment of the present invention will be described with reference to FIGS. 10 to 16 . In the first embodiment described above, a load of the weight 54 is applied to each of the load sensor sections 12 so as to perform a calibration. In the case where the calibration is performed in such a manner as described above, a measurement error can be substantially suppressed as compared to when using a conventional calibration method. However, under actual usage conditions, in the case where the weight measuring apparatus 10 is mounted in the place of use and a person, for example, steps onto the load platform 11 , the load platform 11 is more or less deflected due to the weight of the person, as shown in FIG. 10 . That is, the frame 15 forming the weight measuring apparatus 10 is deformed due to the weight of the person, and each of load sensor sections 12 is accordingly slightly inclined in its entirety. As a result, as shown in FIG. 11 , the load cell 23 is to be accordingly slightly inclined in its entirety. When the measurement is performed in a state described above, the measurement error would be more or less generated even if the calibration according to the first embodiment is performed.
[0116] Specifically, the calibration according to the first embodiment assumes that a load applied to each load sensor section 12 (load cell 23 ) is measured when the load sensor section 12 is in a horizontal state. However, under actual usage conditions, the load applied to each load sensor section 12 is measured when the load cell 23 is inclined in its entirety due to the aforementioned deflection. Therefore, since the calibration is performed assuming that the load sensor section 12 is in a horizontal state, a measurement error between an actual weight and a detection value thereof is generated. Thus, in the second embodiment, a calibration is performed in a state where the aforementioned deflection is taken into consideration, in other words, in a state similar to an actual usage state where the load cell 23 is inclined in its entirety.
[0117] Next, a principle of the weight applying/calibration method according to the second embodiment will be described. Note that the weight applying unit 50 according to the second embodiment is the same as that of the first embodiment except for a deflection generating member 61 to be described below. Therefore, the same components as those of the first embodiment will be denoted by the same reference numerals and will not be further described below. In the second embodiment, when the weight measuring apparatus 10 is placed on the placement table 51 in such a manner as described above, the deflection generating member 61 (to be described later in detail) is disposed so as to be interposed between the placement table 51 and the weight measuring apparatus 10 . FIG. 12 is a schematic diagram illustrating a state where the deflection generating member 61 is disposed so as to be interposed between the weight measuring apparatus 10 and the placement table 51 . In this state, similarly to the first embodiment, the weight 54 is attached to each of the hook portions 53 , thereby applying the weight of the weight 54 to each of the load sensor sections 12 . Therefore, as shown in FIG. 13 , it is possible to create a state where the deflection as mentioned above is generated in the weight measuring apparatus 10 . Thus, a proper calibration can be performed taking into consideration the deflection generated under actual usage conditions.
[0118] Hereinafter, the deflection generating member 61 will be described in detail. FIG. 14 is a diagram illustrating an example of an external view of the aforementioned deflection generating member 61 . FIG. 14 includes seven images: (A) is a plan view; (B) is a left side view; (C) is a right side view; (D) is a front view; (E) is a back view; (F) is a bottom view; and (G) is a perspective view. As shown in FIG. 14 , the deflection generating member 61 has a rectangular plate-like shape. The rectangular plate-like shape is a shape simulating an area in which a weight measurement target object contacts the load platform (i.e., an area to which a load is applied). In the present embodiment, it is assumed that the aforementioned area is a sole of the foot. Considering variations in size of a sole of the foot among individuals and preventing an applied load from being concentrated onto one spot, the deflection generating member 61 has a rectangular shape having a substantial area. In the present embodiment, it is also assumed that one deflection generating member 61 is one foot. Therefore, a total of two deflection generating members, as both feet, are used.
[0119] Next, a material of the deflection generating member 61 will be described. The material used for the deflection generating member 61 has preferably elasticity to some extent. This is because even when a stress is applied to an end of the deflection generating member 61 in a state where a load is applied to the weight measuring apparatus 10 and deflection is generated, the stress would be dispersed if the deflection generating member 61 had the elasticity, thereby not hampering the deflection of the weight measuring apparatus 10 . Furthermore, with the elasticity, the load platform surface of the weight measuring apparatus 10 can be prevented from being damaged through calibration steps. In the present embodiment, the deflection generating member 61 is made of ester polyurethane as an example. Specifically, the ester polyurethane has a specific gravity of 1.20, a Shore hardness of Shore A70 (i.e., approximately a hardness of a rubber ball used in baseball), a tensile strength of 31.3 Mpa, an elongation of 650%, a heat resistance of 70° C., and a cold resistance of −20° C.
[0120] Then, a difference between an effect produced when a calibration is performed with the deflection generating member 61 and an effect produced when a calibration is performed without the deflection generating member 61 will be described with reference to FIGS. 15 and 16 . FIG. 15 is a table showing results detected by a test unit other than the weight applying unit 50 when weights of 34 kg, 68 kg, 102 kg and 136 kg are placed on the load platform of the weight measuring apparatus 10 on which a calibration is performed without the deflection generating member 61 (i.e., by using the method of the first embodiment). Also, FIG. 16 is a table showing results detected by the test unit other than the weight applying unit 50 when the weights of 34 kg, 68 kg, 102 kg and 136 kg are placed on the load platform of the weight measuring apparatus 10 on which a calibration is performed with the deflection generating member 61 (i.e., by using the method of the second embodiment). In each of FIGS. 15 and 16 , the measurement is performed ten times for each of the weights (“sample No” indicates an Nth measurement (N is an integer of 1 to 10)). Also, a maximum value, a minimum value and an average value among values obtained by ten measurements are indicated as “MAX”, “MIN” and “AVG”, respectively. A difference between the average value AVG and the weight of an actually placed weight (a reference value) is indicated as “difference from reference value”.
[0121] For example, when the weight of 34 kg is placed, “difference from reference value” is “−0.191” in FIG. 15 , while the value is “−0.027” in FIG. 16 . That is, an error between the weight of an actual measurement object and a detection value thereof is smaller when using the weight measuring apparatus 10 on which a calibration is performed with the deflection generating member 61 .
[0122] Also, in FIG. 15 , “difference from reference value” obtained when the weight of 34 kg is placed is “−0.191” while the value obtained when the weight of 136 kg is placed is “−0.504”, and a difference between the aforementioned two values is “0.313”. On the other hand, in FIG. 16 , “difference from reference value” obtained when the weight of 34 kg is placed is “−0.027” while the value obtained when the weight of 136 kg is placed is “0.133”, and a difference between the aforementioned two values is “0.106”, which is smaller than “0.313” in FIG. 15 . That is, in both cases shown in FIGS. 15 and 16 , “difference from reference value” tends to be greater as the weight of a measurement object is increased. However, the fluctuation of “difference from reference value” varied in accordance with the weight of the measurement object is smaller in the case shown in FIG. 16 . That is, a more accurate measurement can be performed when using the weight measuring apparatus 10 on which a calibration is performed with the deflection generating member 61 .
[0123] As described above, in the present embodiment, a calibration is performed with the deflection generating member 61 , thereby making it possible to create a state more similar to actual usage conditions. Therefore, a proper calibration can be performed, and thus a measurement accuracy of the weight measuring apparatus 10 also can be improved accordingly.
[0124] In the second embodiment, the aforementioned deflection is generated by interposing an elastic member (the deflection generating member made of polyurethane) between the placement table 51 and the weight measuring apparatus 10 . However, the present invention is not limited to the above example of such a member interposed between the placement table 51 and the weight measuring apparatus 10 if the deflection is generated. For example, a through hole may be provided through the placement table 51 at a position where the deflection generating member 61 is to be disposed, so as to create a mechanism to mechanically apply pressure to the load platform 11 through the through hole from below.
[0125] While the invention has been described in detail, the foregoing description is in all aspects illustrative and not restrictive. It is understood that numerous other modifications and variations can be devised without departing from the scope of the invention.
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A game controller including multiple sensors for detecting a pressure load of a user for use as an input device of a game apparatus. The game controller includes a load platform adapted to receive the pressure load of the user; a plurality of load sensors arranged in the load platform for detecting the pressure load of the user, each load sensor generating an independent detected load signal; and a connector to operationally connect the plurality of load sensors to the game apparatus for transmitting a transmission signal to the game apparatus to facilitate gameplay. The transmission signal includes the independent detected load signal of at least one load sensor such that the transmission signal includes at least one independent detected load signal corresponding to at least one load sensor of the plurality of load sensors.
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FIELD OF THE INVENTION
The present invention relates to a step unit, which includes a step member adjacent to a vehicle sliding door, and a drive device for the vehicle sliding door.
BACKGROUND OF THE INVENTION
Conventionally, a step unit is provided on a vehicle main body at a position that is adjacent to a vehicle sliding door. One type of typical step unit includes a step member and a drive device (motor unit), which is fixed to the step member and operates to open and close a vehicle sliding door. For example, refer to Patent Document 1.
In such a step unit, the step member is typically formed through sheet-metal processing and has a flat plate portion, on which occupants put their feet. The drive device is mounted at a position of the flat plate portion where the drive device is least obstructive to occupants. For example, the drive device is mounted at a position on the flat plate portion that is at the rearmost end.
PRIOR ART DOCUMENT
Patent Document
Patent Document 1: Japanese Laid-Open Patent Publication No. 2007-132141
SUMMARY OF THE INVENTION
However, in the above described step unit, since the drive device is fixed onto the flat plate portion, on which an occupant put a foot, the drive device undesirably protrude upward from the upper surface of the flat plate portion by a significant amount. This, for example, hampers a low-floor design of the passenger compartment. The drive device may be fixed to the lower surface of the step member, or the side that faces the ground surface. However, there is a limitation to the space below the step member, and the configuration has other drawbacks. For example, the waterproof design for the drive device (and its control circuit) would be complicated.
Accordingly, it is an objective of the present invention to provide a step unit that easily reduces upward protrusion of a drive device by a great degree.
According to the present invention, a step unit that includes a step member and a drive device is provided. The step member is provided on a vehicle main body to be adjacent to a vehicle sliding door, and has a flat plate portion for allowing an occupant to put his/her foot thereon. The drive device is fixed to the step member, and is for operating the vehicle sliding door to open and close. The step member is molded of a resin material and has an accommodation portion, which has a bottom that is formed at a position lower than an upper surface of the flat plate portion. The drive device is fixed such that at least a part thereof is accommodated in the accommodation portion.
This configuration reduces upward protrusion of the drive device from the upper surface of the flat plate portion. As a result, a low-floor design of the passenger compartment is possible. Further, unlike conventional step members, the step member is not formed through sheet-metal processing, but is molded of a plastic material. This allows the step member to have wide variety of shapes. Accordingly, it is possible to form the bottom of the accommodation portion at a position significantly lower than the upper surface of the flat plate portion. Therefore, it is possible to reduce upward protrusion of the drive device from the upper surface of the flat plate portion by a great degree.
A peripheral wall may be molded integrally with the step member to encompass the accommodation portion. The peripheral wall extends to a position upward of the upper surface of the flat plate portion.
This configuration restricts liquid from entering the accommodation portion, for example, from the upper surface of the flat plate portion. The drive device is therefore prevented from being wet. Particularly, it is difficult to form the peripheral wall about the accommodation portion through sheet-metal processing. However, since the step member is molded of a plastic material, the peripheral wall can be easily molded integrally with the step member.
A loop belt may be supported by a pulley provided on the lower surface of the step member and be arranged in an opening-closing direction of the vehicle sliding door. In this case, the drive device is used for rotating the belt. Also, a shaft support portion may be molded integrally with the step member, and the pulley may be detachably and rotationally supported by the shaft support portion.
This configuration eliminates the need for additional components such as a bracket for attaching the pulley and facilitates the attachment of the pulley. Particularly, it is difficult to form the shaft support portion, to which a pulley can be detachably attached and rotationally supported, through sheet-metal processing. However, since the step member is molded of a plastic material, the shaft support portion can be easily molded integrally with the step member.
The shaft support portion may be a non-annular shaft support portion, which has an opening on a side opposite to the direction of force that is perpendicular to the axis and applied to the pulley by the belt in a taut state. Further, the pulley may be attached to the non-annular shaft support portion by being inserted through the opening.
According to this configuration, the pulley is attached to the non-annular shaft support portion by being inserted through the opening. This allows the pulley to be easily installed and prevented from falling off by a force in a direction perpendicular to the axis applied by the belt in a taut state.
A loop belt may be provided on the lower surface of the step member and arranged in an opening-closing direction of the vehicle sliding door, and the drive device may be used for rotating the belt. Further, a regulation portion for regulating the position of the belt may be molded integrally with the lower surface of the step member to extend from the lower surface, and a metal sheet member may be fixed to a surface of the regulation portion on which the belt slides.
This configuration easily reduces wear of the regulation portion, which is molded of a plastic material. Also, wear of the belt can be reduced. Further, it is possible to reduce the generation of noise during operation.
The metal sheet member may be press fitted to the step member.
This configuration eliminates the necessity for fasteners such as screws for fixing. Particularly, it is difficult to form the metal sheet receiving portion, to which the metal sheet member is press fitted, through sheet-metal processing. However, since the step member is molded of a plastic material, the metal sheet receiving portion can be easily molded integrally with the step member.
The metal sheet member may have a folded back portion for preventing the belt from falling off downward.
This configuration prevents the belt from falling off downward without increasing the number of components.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view from above illustrating a step unit according to one embodiment;
FIG. 2 is a perspective view from below illustrating the step unit according to the embodiment;
FIG. 3 is a partial plan view illustrating the step unit according to the embodiment;
FIG. 4A is a cross-sectional view of the step member taken along line 4 A- 4 A in FIG. 3 ;
FIG. 4B is a cross-sectional view of the step member taken along line 4 B- 4 B in FIG. 3 ;
FIG. 5 is a partial exploded perspective view from below illustrating the step unit according to the embodiment;
FIG. 6 is a partial bottom view illustrating the step unit according to the embodiment;
FIG. 7 is an explanatory exploded perspective view from below illustrating the support extensions and the rail plate member of the embodiment;
FIG. 8 is a partial bottom view illustrating the step unit according to the embodiment;
FIG. 9A is a cross-sectional view taken along line 9 A- 9 A in FIG. 8 ;
FIG. 9B is an enlarged view illustrating the part surrounded by the line formed by a long dash alternating with a short dash in FIG. 9A ;
FIG. 10 is a partial perspective view from below illustrating the step unit according to a modification;
FIG. 11 is a partial bottom view showing a step unit the modification; and
FIG. 12 is a perspective view showing a metal sheet member according to the modification.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
One embodiment according to the present invention will now be described with reference to FIGS. 1 to 9 .
A vehicle has a step unit 1 shown in FIG. 1 , which is located adjacent to a vehicle sliding door (not shown). In FIGS. 1 and 2 , “outside” refers to the outside of the passenger compartment in the direction of the vehicle width, and “inside” refers to the direction toward the center of the passenger compartment in the direction of the vehicle width.
The step unit 1 is a type that includes a drive device (motor unit) 2 for opening and closing the vehicle sliding door. The step unit 1 is mainly constituted of the drive device 2 and a substantially plate-like step member (step) 3 . The step unit 1 is fixed to the main body (not shown) of the vehicle. The entire upper surface of the step unit 1 is covered with a scuff plate, which is a thin plate-like decorative member (not shown). The upper surface of the drive device 2 (the lower surface of the thin plate-like scuff plate) is covered with a rigid plate or a cover (not shown).
The step member 3 is molded of a plastic material. The step member 3 is located in the passenger compartment at a position adjacent to the vehicle sliding door in the closed state, and includes a flat plate portion 4 , on which an occupant places a foot when getting in or out of the vehicle, and an accommodation portion 5 (see FIGS. 4A and 4B ). The accommodation portion 5 is formed continuous to the flat plate portion 4 and is located on a side of the flat plate portion 4 in the opening direction of the sliding door, or rearward of the flat plate portion 4 . The step member 3 is fixed with a part of the drive device 2 accommodated in the accommodation portion 5 .
Specifically, when the accommodation portion 5 is installed in the vehicle, a bottom 5 a of the accommodation portion 5 is located at a lower position than an upper surface 4 a of the flat plate portion 4 as shown in FIGS. 4A and 4B . The height (depth) of the bottom 5 a of the accommodation portion 5 is determined based on the shape of the drive device 2 . As shown in FIGS. 1 and 3 , the drive device 2 includes a motor 2 a , which is a drive source, an output portion 2 b , which has a gear attached to the motor 2 a and an electromagnetic clutch, a control circuit portion 2 c , which is installed in the output portion 2 b . The accommodation portion 5 includes a motor accommodating section 5 b , an output portion accommodating section 5 c , and a circuit accommodating section 5 d as shown in FIGS. 4A and 4B . The drive device 2 is fixed by screws such that it partly contacts the bottom 5 a of the accommodation portion 5 , that is, a part of the drive device 2 is located lower than the upper surface 4 a of the flat plate portion 4 . One third or more of the entire thickness of the drive device 2 in the vertical direction is located below the upper surface 4 a of the flat plate portion 4 . In the present embodiment, substantially half the entire thickness is located below the upper surface 4 a . In the present embodiment, a peripheral wall 6 is molded integrally with the step member 3 to encompass the accommodation portion 5 . More specifically, the peripheral wall 6 substantially entirely surrounds the accommodation portion 5 as shown in FIGS. 1 , 3 , 4 A and 4 B. The peripheral wall 6 extends to a position above the upper surface 4 a of the flat plate portion 4 .
As shown in FIG. 2 , pulleys 11 , 12 are located on the lower surface of the step member 3 . A loop belt 13 is supported by the pulleys 11 , 12 and extends in the opening-closing direction of the vehicle sliding door. The drive device 2 rotates the belt 13 . That is, as shown in FIG. 4A , an output shaft 2 d of the output portion 2 b of the drive device 2 extends through a through hole 5 e formed in the bottom 5 a of the accommodation portion 5 and protrudes from the lower surface of the step member 3 . The output shaft 2 d transmits power to the belt 13 via a power transmitting portion 14 (see FIG. 2 ), which is provided on the lower surface of the step member 3 , thereby rotating the belt 13 . In the present embodiment, the opening-closing direction of the vehicle sliding door corresponds to the front-rear direction of the vehicle. However, the path of the sliding door is curved inward toward the center of the passenger compartment at a front portion in accordance with the closed position of the vehicle sliding door. The position of the belt 13 is regulated by the pulleys 11 , 12 , which are located at ends in the vehicle front-rear direction, and a regulation portion 15 , which is located between the pulleys 11 and 12 and extends from the lower surface of the step member 3 . The regulation portion 15 is molded integrally with the lower surface of the step member 3 .
Non-annular shaft support portions 16 , which serve as a shaft support portion, are molded integrally with the step member 3 . The pulley 11 , which is located at the front end, is rotationally supported by the non-annular shaft support portions 16 as shown in FIGS. 5 and 6 . The non-annular shaft support portions 16 are formed to support the pulley 11 in a detachable and rotational manner. Specifically, the non-annular shaft support portions 16 are formed in a pair each having an opening 16 a on the side opposite to the direction of the force that is perpendicular to the axis and applied to the pulley 11 by the belt 13 in a taut state. In other words, the openings 16 a are located on the front side. The pulley 11 has a shaft 11 a , which is fitted to the openings 16 a , so that the pulley 11 is rotationally supported by the non-annular shaft support portions 16 . The width of the openings 16 a is slightly smaller than the diameter of the shaft 11 a of the pulley 11 to form a holding structure, in which, regardless of the force applied by the belt 13 , the pulley 11 does not come off when receiving a small force. The pulley 12 , which is located at the rear end, is rotationally supported by the cover of the power transmitting portion 14 as shown in FIG. 2 .
A pair of lower rails 21 , 22 is molded integrally with the lower surface of the step member 3 as shown in FIG. 2 . The lower rails 21 , 22 extend in the opening-closing direction of the vehicle sliding door (substantially, the front-rear direction of the vehicle). The lower rails 21 , 22 are connected to each other at both ends in the opening-closing direction (that is, substantially the front-rear direction of the vehicle). As shown in FIGS. 7 and 8 , a cutout portion 21 a is formed in a part of the lower rail 21 . A rail plate member 31 is arranged at the cutout portion 21 a to make the lower rail 21 continuous in the opening-closing direction of the vehicle sliding door. Rollers 32 (see FIG. 8 ) are provided between the lower rails 21 , 22 (including the rail plate member 31 ). The rollers 32 are coupled to the vehicle sliding door, for example, via brackets (not shown). Thus, the rollers 32 and the vehicle sliding door are guided in the opening-closing direction by the lower rails 21 , 22 . The rollers 32 are coupled to the belt 13 via brackets (not shown), so that, as the belt 13 rotates, the rollers 32 are moved in the opening closing direction while being guided by the lower rails 21 , 22 .
Specifically, as shown in FIGS. 7 to 9A , the step member 3 has an insertion slit 23 extending in the vertical direction at a position that corresponds to the cutout portion 21 a . Also, the step member 3 has support extensions 21 b . The support extensions 21 b extend from the ends of the cutout portion 21 a of the lower rail 21 to support the rail plate member 31 against the load applied to the rail plate member 31 by the rollers 32 (see FIG. 8 ). As shown in FIG. 8 , the pair of support extensions 21 b extend from the ends of the cutout portion 21 a of the lower rail 21 in the direction in which load is applied (upward as viewed in FIG. 8 , and toward the outside with respect to the vehicle width direction), to approach each other without being connected to each other, so that there is a space therebetween. The support extensions 21 b are thicker than the lower rail 21 in the direction in which the load is applied (the up-side direction as viewed in FIG. 8 ).
On the other hand, the rail plate member 31 is formed by processing a metal plate, and installed by being inserted through the insertion slit 23 from above the step member 3 as shown in FIG. 7 . As shown in FIGS. 1 and 7 , the rail plate member 31 has an angled portion 31 a at the upper edge (the upper edge in a state after being installed). The angled portion 31 a extends in a direction perpendicular to the vertical direction, or into the passenger compartment in the present embodiment. The rail plate member 31 is inserted into the insertion slit 23 such that the lower side of the angled portion 31 a contacts the upper surface of the step member 3 . In the present embodiment, the rail plate member 31 is fixed through press-fitting as shown in FIG. 9B . Specifically, the rail plate member 31 has a pair of press-fit portions 31 b , which protrude from the sides of the rail plate member 31 that face the ends of the cutout portion 21 a to be press fitted to the ends of the cutout portion 21 a . When being inserted through the insertion slit 23 from above the step member 3 , the rail plate member 31 is press fitted when the press-fit portions 31 b are pressed against the ends of the cutout portion 21 a of the lower rail 21 . At this time, the sides of the cutout portion 21 a of the lower rail 21 are shaven or elastically deformed by the press-fit portions 31 b . However, as long as the rail plate member 31 can be press fitted, the structure may be changed.
In the above described configuration, the rail plate member 31 can be removed to insert rollers 32 into the space between the lower rails 21 , 22 through the cutout portion 21 a or remove the rollers 32 from the space between the lower rails 21 , 22 . When the drive device 2 is operated, the belt 13 is rotated. Accordingly, the rollers 32 are moved while being guided by the lower rails 21 , 22 , and the vehicle sliding door is operated to open or close. The output shaft 2 d of the drive device 2 or the housing of the drive device 2 has an O-ring, which is not shown, so that water is completely or almost completely prevented from entering the interior of the drive device 2 or the bottom 5 a of the accommodation portion 5 through the through hole 5 e formed in the bottom 5 a of the accommodation portion 5 .
The present embodiment operates and has advantages as described below.
(1) The drive device 2 is fixed such that a part thereof is accommodated in the accommodation portion 5 , which has the bottom 5 a , and the bottom 5 a is formed at a position lower than the upper surface 4 a of the flat plate portion 4 , on which an occupant put a foot. This structure reduces the amount of protrusion of the drive device 2 from the upper surface 4 a of the flat plate portion 4 . As a result, the low-floor design of the passenger compartment is possible. Further, unlike conventional step member, the step member 3 is not formed through sheet-metal processing, but molded of a plastic material. This allows the step member 3 to have wide variety of shapes. Accordingly, it is possible to form the bottom 5 a of the accommodation portion 5 at a position significantly lower than the upper surface 4 a of the flat plate portion 4 . Therefore, it is possible to reduce upward protrusion of the drive device 2 from the upper surface 4 a of the flat plate portion 4 by a great degree.
(2) The peripheral wall 6 is molded integrally with the step member 3 to encompass the accommodation portion 5 of the step member 3 . The peripheral wall 6 extends to a position above the upper surface 4 a of the flat plate portion 4 . This reduces entry of liquid to the interior of the accommodation portion 5 from the upper surface 4 a of the flat plate portion 4 . The drive device 2 is therefore prevented from being wet. Particularly, it is difficult to form the peripheral wall 6 about the accommodation portion 5 through sheet-metal processing. However, since the step member 3 is molded of a plastic material, the peripheral wall 6 can be easily molded integrally with the step member 3 .
(3) The step member 3 includes the integrally molded non-annular shaft support portions 16 , which is a support shaft portion for detachably and rotationally support the pulley 11 . This eliminates the necessity for additional components such as brackets. Also, the pulley 11 can be easily assembled with the non-annular shaft support portions 16 . Particularly, it is difficult to form the shaft support portion, to which the pulley 11 can be detachably attached and rotationally supported, through sheet-metal processing.
However, since the step member 3 is molded of a plastic material, the shaft support portion can be easily molded integrally with the step member 3 .
(4) The shaft support portion includes the non-annular shaft support portions 16 , which have openings 16 a on the side opposite to the direction of the force that is perpendicular to the axis and applied to the pulley 11 by the belt 13 in a taut state. The pulley 11 is inserted to the openings 16 a to be attached to the non-annular shaft support portions 16 . This allows the pulley 11 to be easily installed and prevented from falling off by a force in a direction perpendicular to the axis applied by the belt 13 in a taut state. It is difficult to form the pair of non-annular shaft support portions 16 described in the present embodiment through sheet-metal processing. However, since the step member 3 is molded of a plastic material, the non-annular shaft support portion 16 can be easily molded integrally with the step member 3 .
The above-described embodiment may be modified as follows.
In the above illustrated embodiment, the regulation portion 15 is molded integrally on the lower surface of the step member 3 to regulate the position of the belt 13 , and the position of the belt 13 is regulated only by the regulation portion 15 . However, as shown in FIGS. 10 to 12 , a metal sheet member 42 may be fixed to a surface of a regulation portion 41 on which the belt 13 sides.
Specifically, the regulation portion 41 for regulating the position of the belt 13 is molded integrally with the lower surface of the step member 3 . The regulation portion 41 has a metal sheet receiving portion 41 a at a position on which the belt 13 is likely to slide as shown in FIGS. 10 and 11 . The metal sheet receiving portion 41 a of this modification is configured to have an arcuate bulge 41 b protruding toward the belt 13 as viewed from below (in the state installed in the vehicle, see FIG. 11 ) and locking grooves 41 c , which are provided on the sides of the bulge 41 b . On the other hand, as shown in FIG. 12 , the metal sheet member 42 is formed to be curved and has an elastic piece 42 a at in a lower portion (lower end when installed in the vehicle, the upper end as viewed in FIG. 12 ). The elastic piece 42 a is formed by cutting and raising from the back of the metal sheet member 42 (concave side). The side edges of the metal sheet member 42 are fitted in the locking grooves 41 c , and the elastic piece 42 a is elastically deformed and pressed against the bulge 41 b , so that the metal sheet member 42 is fixed to the regulation portion 41 of the step member 3 . The elastic piece 42 a is arranged at a position lower than the position of the belt 13 , the vertical position of which is determined by the brims of the pulleys 11 , 12 (refer to FIG. 10 ). Therefore, the belt 13 slides on the smooth front surface (bulging curved surface) of the metal sheet member 42 , on which the elastic piece 42 a is not formed.
The metal sheet member 42 of this modification has a folded back portion 42 b at the lower end (lower end in a state installed in the vehicle, upper end as viewed in FIG. 12 ) as shown in FIGS. 10 to 12 . The folded back portion 42 b prevents the belt 13 from falling off downward.
Since the metal sheet member 42 is fixed to the surface of the regulation portion 41 that slides on the belt 13 , wear of the regulation portion 41 molded of plastic material is easily suppressed. Also, wear of the belt 13 can be reduced. Further, it is possible to reduce the generation of noise during operation.
Since the metal sheet member 42 is press-fitted in the step member 3 , no additional fasteners such as screws are needed. Particularly, it is difficult to form the metal sheet receiving portion 41 a , to which the metal sheet member 42 is press fitted, through sheet-metal processing. However, since the step member 3 is molded of a plastic material, the metal sheet receiving portion 41 a can be easily molded integrally with the step member 3 .
Since the metal sheet member 42 has a folded back portion 42 b for preventing the belt 13 from falling off downward, it is possible to prevent the belt 13 from falling off downward without increasing the number of components.
The metal sheet member 42 may be press fitted to the step member 3 using other structure. Also, the metal sheet member 42 may be fixed to the step member 3 using fastening members such as screws. The folded back portion 42 b may be omitted.
The peripheral wall 6 may be omitted.
As a shaft support portion for rotationally supporting a shaft, the non-annular shaft support portions 16 may be replaced by other separate members such as brackets that rotationally support the pulley 11 . The shaft support portion may have any configuration other than that of the non-annular shaft support portions 16 , which have the openings 16 a , as long as the shaft support portion is molded integrally with the step member 3 and can detachably and rotationally support the pulley 11 . That is, a shaft support portion may be employed that does not have a function for preventing the pulley 11 from being caused to fall off by a force that is perpendicular to the direction of the axis and applied by the belt 13 in a taut state.
The step member 3 does not need to have the accommodation portion 5 , in which the bottom 5 a , which is at a position lower than the upper surface 4 a of the flat plate portion 4 . Even in this case, the advantages (3) and (4) can be achieved.
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A step unit comprises: a step member which is provided on the vehicle body side so as to be adjacent to a slide door of the vehicle and has a flat plate section on which an occupant's foot is placed; and a drive device which is affixed to the step member and drives the slide door to open and close the slide door. The step member is molded using a resin material and has a accommodation portion which is provided with a bottom formed below the upper surface of the flat plate section. The drive device is affixed while at least a part thereof is accommodated within the accommodation portion.
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FIELD OF THE INVENTION
The present invention relates generally to devices used to determine a vertical line in the building construction trade and the like, and more specifically to a plumb bob utilizing a relatively short plumb line and laser device therein to project a laser beam to a target therebelow. The invention also resides in various apparatus used to position the plumb bob accurately, and further to provide an accurate target therefor.
BACKGROUND OF THE INVENTION
Devices for plumbing, or determining and forming a vertical line, have been used in the building and other trades since the earliest of times. Traditionally, these devices have basically consisted of nothing more than a weight suspended from a string or line, with the vertical line determined by gravity. More recently, various relatively complex plumbing and leveling devices have been developed, many of which rely upon the extremely narrow beam of a laser. However, these devices are generally quite costly, use bearings which develop at least some amount of friction which reduces their accuracy, require a relatively large amount of electrical power for operation, are prone to error due to numerous critically adjusted or set components which may be knocked or jarred out of alignment, and/or require a relatively skilled operator in order to produce accurate readings and to ensure proper handling of the apparatus in order to preclude damage thereto.
Accordingly, it has been recognized that simpler, less costly plumb bobs incorporating light means therein, may be valuable in such work. However, such lighted plumb bobs developed to this point rely upon an incandescent light source, which produces incoherent light which tends to spread even when focused through one or more lenses. As a result, such plumb bobs must be used conventionally close to the target and using a relatively long plumb line, in the manner of standard plumb bobs of long use. The only advantage of such lighted plumb bobs is their ability to be used in conditions of low light. However, the disadvantages of a relatively long plumb line, and the time required for oscillations to dampen, still remain.
The need arises for a plumb bob incorporating a relatively simple and low cost laser therein, which plumb bob may be suspended on a relatively short line at some distance from the target. The relatively short line provides relatively rapid damping of oscillations, and further provides for ease of protection from wind and other factors which might cause a conventional plumb line to oscillate. The extremely narrow laser beam provides great accuracy in determining the precise point vertically below the laser plumb bob, and is not affected by wind, diffusion of the light beam, or other factors. A further need exists for various devices or apparatus providing for the rapid deployment of a plumb bob and measurement of a vertical thereby, by a single person, thus freeing others to perform other tasks and reducing the labor costs involved in such plumbing operations.
DESCRIPTION OF THE PRIOR ART
U.S. Pat. No. 3,635,565 issued to George P. Colson on Jan. 18, 1972 discloses a Laser Vertical Collimator comprising a laser light source installed within a tube. The tube is in turn suspended by a spherical bearing having a concentric passage therethrough. The laser source may be reversed within the tube to project upwardly, if desired. While the Colson device offers additional versatility due to the reversibility of the light source within the tube, it is relatively costly and also prone to various problems, ranging from possible misalignment of the laser beam with the vertical, friction and/or damage to the spherical bearings, and further due to friction imposed by the relatively inflexible electrical connector between the top of the housing and the suspended laser source.
U.S. Pat. No. 3,771,876 issued to Erland S. Ljungdahl et al. on Nov. 13, 1973 discloses an apparatus for Producing A Plane Or Conical Optical Reference Surface comprising a laser or other light source which transmits a beam vertically downward to pass through a prism or lens. The light transmitting means is suspended by two leaves at right angles to one another, which leaves are able to bend in only a single plane each. The perpendicular axes provide the required pendulum mounting for the light source. However, Ljungdahl et al. rely upon the two leaves not only to suspend the light source, but also to act as a conductor for the required electrical power. Thus, each leaf is formed of a non-conductive center portion, sandwiched on each side by a conductor. The resulting construction would appear to be somewhat stiffer than the flexible line or string used with the present invention, and the entire apparatus is more complex.
U.S. Pat. No. 4,333,242 issued to Robert K. Genho, Sr. on Jun. 8, 1982 discloses a Construction Laser providing automatic leveling and projection of a laser beam in a horizontal direction. However, the device is exceedingly complex and costly in comparison to the present invention, and cannot project a beam vertically downward as required in plumbing operations. The various bearings, supports, automatic adjustments, etc., require constant inspection to confirm the accuracy of the device, whereas the present invention requires little, if any adjustment at any time.
U.S. Pat. No. 4,448,528 issued to Acie J. McManus on May 15, 1984 discloses a Portable Laser Vertical Collimator And Plumb Line Indicator comprising a dual laser projecting from opposite ends, 180 degrees opposed from one another and projecting upwardly and downwardly. The device is suspended by a gimbal which produces relatively greater friction than the string or line suspension of the present plumb bob and thus reduces accuracy. While the McManus device permits vertically upward and downward projections, if the laser device is misaligned, the error is effectively doubled due to the dual projection from a single laser device.
U.S. Pat. No. 4,597,186 issued to Peter Markos on Jul. 1, 1986 discloses a Lighted Plumb Bob comprising a conventional plumb bob body essentially housing a penlight or the like therewithin. The device uses a relatively small diameter passage for the light from the incandescent bulb therein to pass through, which small diameter passage serves to some extent to narrow the projected beam. However, in practice the Markos plumb bob "is suspended in a conventional manner . . . so that (the) tip . . . is approximately 3/4 to one inch above the surface." (Col. 2, lines 44-47.) The present device uses a laser emitting a relatively long, narrow beam.
U.S. Pat. No. 4,625,428 issued to Gerald E. Griffin on Dec. 2, 1986 discloses a Lighted Plumb Bob generally similar to the Markos device discussed immediately above, but including a switch activated by the weight of the plumb bob suspended therefrom. The same limitations exist as with the Markos device, in that the incandescent bulb providing incoherent light cannot be focused to a pinpoint some distance away from the plumb bob, particularly without the use of lenses. If an attempt is made to narrow the light passage in the tip of the plumb bob to too great a degree, the result is similar to a pinhole camera, in that the light begins to spread again due to interference with the hole diameter. Accordingly, Griffin uses his plumb bob in the same manner as that of Markos, using "a line . . . of a conventional nature for plumb bobs . . . ." (col. 2, lines 53-54.) This is done to position the tip of the plumb bob relatively close to the target, in order to obviate the problem of beam spread with the incandescent light source.
U.S. Pat. No. 5,012,585 issued to Charlie J. DiMaggio on May 7, 1991 discloses a Laser Plumb Bob Apparatus in which a single laser is used to project a beam upwardly and downwardly, so the device may be suspended between floor and ceiling to provide a plumb line therebetween, in the manner of the McManus device discussed further above. The device includes a spherical center portion, which is suspended within a concave spherical ring. The possibility of misalignment of the lenses, as well as the bearing friction of the spherical central portion and its supporting ring, would appear to require considerable care in alignment and the possibility of instrument error occurring, which problems are largely precluded by the present plumb bob invention.
U.S. Pat. No. 5,075,977 issued to Joseph F. Rando on Dec. 31, 1991 discloses an Automatic Plumb Bob And Level Tool utilizing a single laser therewithin and projecting a beam to a mirror which is mounted on a compensating spring, thus permitting the device to be used to project either a horizontal or vertical beam and to adjust automatically for non-level surfaces upon which it is placed. No provision is made for suspending the device from a line or other means of suspension. The weight and compensating spring must be carefully calibrated for accuracy, and the pivotally mounted laser may be knocked out of alignment with hard use. The present plumb bob has no moving parts or components which require adjustment, or which may be misaligned.
Finally, European Patent No. 341,812 to Spectra-Physics Inc. and published on Nov. 15, 1989 discloses a Level/Plumb Indicator With Tilt Compensation. The mechanism of the device is somewhat related to the device of the Rando patent discussed immediately above, and in fact one of the co-inventors of the Spectra-Physics European Patent is Rando. Accordingly, the same potential drawbacks exist in the Spectra-Physics device, i.e., mirrors and/or lenses suspended by various means, each of which can lead to misalignment problems which are obviated by the present invention.
None of the above noted patents, taken either singly or in combination, are seen to disclose the specific arrangement of concepts disclosed by the present invention.
SUMMARY OF THE INVENTION
By the present invention, an improved laser plumb bob and apparatus is disclosed.
Accordingly, one of the objects of the present invention is to provide an improved laser plumb bob and apparatus which includes a conventional plumb bob body which has been hollowed to provide for the permanent and immovable installation of a laser therein, which laser is capable of projecting a narrow, coherent light beam vertically downward to provide a laser plumb line when the laser plumb bob is conventionally suspended.
Another of the objects of the present invention is to provide an improved laser plumb bob and apparatus which plumb bob is adapted to use a relatively short suspension line or string and to be suspended at a relatively great distance above the plumb target.
Yet another of the objects of the present invention is to provide an improved laser plumb bob and apparatus which plumb bob precludes need for adjustment and obviates erroneous readings, due to the lack of lenses and moving parts therein.
Still another of the objects of the present invention is to provide an improved laser plumb bob and apparatus which includes extension devices and cooperating targets, which provide for operation and use by a single person, thus providing greater economy and efficiency in construction.
A further object of the present invention is to provide an improved laser plumb bob and apparatus which may include a telescoping pole or column, having a laser plumb bob suspended at the upper end thereof and a cooperating target secured to the opposite lower end thereof.
An additional object of the present invention is to provide an improved laser plumb bob and apparatus which may include a wind shield providing shielding for the plumb bob as it is suspended adjacent its suspension point.
Another object of the present invention is to provide an improved laser plumb bob and apparatus which requires no special training or technique on the part of the user thereof.
A final object of the present invention is to provide an improved laser plumb bob and apparatus for the purposes described which is inexpensive, dependable and fully effective in accomplishing its intended purpose.
With these and other objects in view which will more readily appear as the nature of the invention is better understood, the invention consists in the novel combination and arrangement of parts hereinafter more fully described, illustrated and claimed with reference being made to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is partially sectioned elevation view, showing the laser plumb bob of the present invention.
FIG. 2 is a perspective view of the laser plumb bob of FIG. 1, in use providing a plumb line along a frame wall.
FIG. 3A is an elevation view in section of the present apparatus providing for the remote holding of the present laser plumb bob, so a single person may check a plumb line.
FIG. 3B is a target usable with the apparatus and plumb bob of FIG. 3A.
FIG. 4 is a perspective view of the laser plumb bob and apparatus of FIGS. 3A and 3B, in use providing a plumb line for a wall corner frame structure.
FIG. 5A is an elevation view of the upper end of the laser plumb bob and adjustable column therefor, showing its details.
FIG. 5B is an elevation view of the lower end of the column of FIG. 5A, showing its details and telescoping mechanism.
FIG. 6 is a perspective view of the laser plumb bob and column of FIGS. 5A and 5B, in use providing a plumb line for a wall corner frame structure.
Similar reference characters denote corresponding features consistently throughout the several figures of the attached drawings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, the present invention will be seen to relate to a laser plumb bob and an apparatus therefor providing for the plumbing of vertical lines by a single person. FIG. 1 discloses an elevation view in partial section of a laser plumb bob 10, showing its general configuration. The laser plumb bob 10 comprises a body portion 12 having an interior cavity 14 therein. The interior cavity 14 is adapted for the fixed installation of a laser device 16 therein. (Details of the laser device 16, electrical batteries therefor, etc., are not disclosed, as the laser device 16 is conventional in nature. Such devices are disclosed in the prior art discussed above, or alternatively, other laser devices for other purposes, e.g., laser pointers and the like, may be used in combination with the present laser plumb bob 10.) A lens element (or multiple elements) 17 may be provided as required, to provide for the sharper focus of the laser beam at relatively long distances from the plumb bob apparatus 10. The lens element(s) 17 may be provided with adjustability, if desired, in order to provide the sharpest and most accurate focus for the laser beam at varying distances, according to the specific requirements of the particular plumbing operation. Provision of a virtually "pinpoint" light at the target or object, will be seen to provide an easily recognized point even in relatively bright conditions, particularly with colored lasers.
The laser plumb bob 10 includes an open lower end 18 having the same diameter as the interior cavity 14, providing for the projection of a laser beam or laser plumb line L therefrom, as shown in FIG. 2 and other figures. The opposite upper end 20 of the laser plumb bob 10 includes plumb line attachment means 22, whereby a relatively short plumb line 24 may be secured to the laser plumb bob 10. The opposite upper end 20 and lower end 18 define a length therebetween, which is conventional in nature with the exception of the truncated lower end 18 providing for the insertion of the laser device 16 therein. It will be seen that a sharp point or the like is not required for the present laser plumb bob 10, as the laser plumb line L itself provides a sharp projected beam, due to the coherent nature of the light emitted by the laser device 16.
Precise alignment of the laser line L is provided by precise assembly of the laser device 16 within the plumb bob body 12. As the axis of the plumb line or string 24 is concentric with the longitudinal axis A of the plumb bob body 12, and the laser device 16 is installed within the plumb bob body cavity 14 so that the projected beam L is coaxial with the longitudinal axis A of the plumb bob body 12, a laser line L projected by the laser device 16 will fall along a precise vertical line when the plumb bob 10 is suspended from the plumb line or string 24. As the coherent light of the laser line L may extend a relatively great distance from the laser device 16 without spreading, to provide a pinpoint of light at a target some distance away, the blumb bob 10 may be suspended from a relatively short length of line 24; it is not necessary to have the laser plumb bob 10 suspended immediately adjacent the target, as with conventional plumb bobs.
The use of a relatively short string or line 24 has definite advantages over the prior art, in that the period of oscillation of the plumb bob pendulum is much more rapid with a shorter line, and will therefore pendulum oscillations will dampen out more quickly. Also, the shorter length of the line or string 24 makes it much easier to protect the laser plumb bob 10 and the line 24 from wind when plumbing incomplete structures exposed to wind and the outdoor environment, as will be discussed further below. Any shortening of the line 24 will have some benefit, even a line length less than half the vertical distance, but preferably the length of the line 24 is no greater than the length of the plumb bob body 12 in order to maximize the advantages of the present invention.
FIG. 2 shows the present laser plumb bob 10 in use in plumbing a wall frame structure W. As discussed above, the line 24 from which the plumb bob body 12 is suspended may be relatively short, on the order of the length of the plumb bob body 12 or even less. The concentricity of the plumb bob body suspension line 24, the plumb bob body 12 with the laser device 16 concentrically housed therein, and the laser line L projected from the laser device 16, serve to cause the laser line L to be projected along the same path which would be described by a longer plumb bob string or line if the plumb bob were to be lowered adjacent the bottom of the wall, as is done conventionally. The pinpoint of light projected by the laser device 16 defines a spot precisely vertically below the center of the laser plumb bob 10, when the plumb bob 10 is in a steady position with no oscillations. The pinpoint of laser light provided by the present invention is also visible in relatively darkened areas, which is advantageous in structures which have not yet had electrical power installed.
FIGS. 3A and 3B disclose an apparatus providing for the use of the present laser plumb bob 10 by a single person. In FIG. 3A, a plumb bob suspension plate or member 26 is shown in section and includes a passage 28 therethrough, which provides for the installation of a blumb bob line or string 24 therethrough to suspend the plumb bob 10 as described above. The member 26 has an edge 30 establishing a distance 32 between the edge 30 and the passage 28, with the longitudinal axis A of the plumb bob 10 aligned with the passage 28 and plumb bob suspension line 24 disposed therethrough.
The plumb bob suspension member 26 includes a shroud or windshield 34 depending therefrom, with the shroud or shield 34 being of the same width as the plumb bob suspension member 26. The shroud or shield may include an extension 34a extending downward a sufficient distance to completely surround a plumb bob suspended from the suspension member 26 by a short line 24, in order to better shield such a plumb bob and line from the wind or other effects, or alternatively a shorter shield 34 may be used to shield the string or line 24 itself, as desired.
An extension shaft or column 36 (shown completely in FIG. 4) is secured to the plumb bob suspension member 26 (or to the depending shield 34) by means of a pivot 38, permitting the column 36 to be held at varying angles relative to the suspension member 26, in order for the suspension member 26 to be held generally level. (It will be understood that slight angular deviations of the suspension member 26, and its shield or shroud 34/34a will not effect the accuracy of the plumb bob 10, due to its depending vertically from the central passage 28 and suspension line 24.) An extension fitting 40 provides for the attachment of the column 36.
FIG. 3B discloses a plan view of the target 42 which is used in combination with the above plumb bob suspension member 26 and extension column 36, with their accompanying features. The target 42 has a peripheral edge 44 and a central target point 46 therein, with a distance 32a between the edge 44 and the target point 46 equal to the distance 32 between the edge 30 and the plumb line passage 28 of the plumb bob suspension member 26. The target point 46 may be defined by orthogonally placed grooves 48 each dividing the target equally, or by other means. As distance 32a of the target 42 and distance 32 of the plumb bob suspension member 26 are equal, it will be seen that the longitudinal axis A of the plumb bob (and a laser line L projected therefrom, as shown in FIG. 4) will precisely coincide with the target point 48, when the target 42 is placed vertically directly beneath the plumb bob suspension member 26. If desired, the target 42 may be coated or otherwise provided with a highly reflective and/or buffered surface, wherein the surface further removed from the central point 46 is less reflective, and/or reflects at a different angle, thereby providing maximum return of the laser beam only when centered on the target.
FIG. 4 provides a clearer view of the above described apparatus. In FIG. 4, a wall structure W1 is shown including a top plate T and a bottom plate B, with another wall structure W2 intersecting the first wall W1 and defining an upper corner C1 and a lower corner C2. The plumb bob suspension member 26, with the plumb bob 10 or the like suspended therefrom, is placed in contact with the walls W1 and W2 in the upper corner C1 by means of the extension column 36 (which may have a telescoping handle portion 36a). The target 42 is placed in the lower corner C2. Assuming that both of the walls W1 and W2 are perpendicular, the projected line L from the plumb bob 10 will strike the target 42 directly at the target point 46. The present invention may thus be used to plumb two intersecting walls simultaneously, or a single wall as desired, by only a single person.
FIGS. 5A and 5B disclose an alternative plumb bob extension means. In FIG. 5A, an upper plumb bob suspension plate or member 50 is shown, from which a plumb bob 10 may be suspended by means of a short plumb string or line 24, as in the embodiments discussed above. The line 24 passes through a plumb line passage 52, which passage 52 is formed through the plate or member 50 at a predetermined distance 54 from an edge 56, as in the embodiment of FIGS. 3A, 3B, and 4. The line 24 may be secured by means of a male threaded shaft 58 having a slot or passage therethrough, with a cooperating knob 60 threadedly tightening on the shaft 50 to clamp the line 24 between the plumb bob suspension plate or member 50 and the bottom of the knob 60. Other means, such as the retaining ring shown in FIG. 3A, may be used as desired.
The apparatus of FIG. 5A may also include a cylindrical shroud or wind shield 62, which shield 62 may be removably secured to the underside of the plumb bob suspension plate or member 50 by means of threads 64 formed on the underside of the member 50. The shield 62 may be of sufficient length to completely surround a plumb bob therein and suspended by a relatively short line 24, or alternatively may be of a shorter length, in the manner of the shield 34 of FIG. 3A. The shield 62 serves the same purpose as the shield 34/34a of FIGS. 3A and 4, i.e., serving to prevent unwanted oscillatory motion of the plumb bob or plumb bob suspension line due to wind or other environmental effects, when the present apparatus is used outdoors or in an uncompleted structure which is open to the outdoor environment.
An upper extension column 66 is rigidly secured normal or perpendicular to the underside of the plumb bob suspension plate or member 50, and serves to support the suspension member 50 (and a plumb bob suspended thereby) in order to plumb a wall or the like. The column 66 in turn fits and telescopes over a base column 68 (shown in FIG. 5B), which telescoping column portions 66 and 68 provide adjustment of the height of the plumb bob suspension member 50 according to the height of the wall or structure to be plumbed. The height adjustment may be locked at the length or height desired by means of a threaded column height locking or securing knob 70.
The base column 68 is in turn secured to a target plate 72, e.g. by means of a socket 74 formed thereon and a locking knob 76, or alternatively the base column 68 may be permanently affixed to the target plate 72 if disassembly is not required. The target plate 72 includes a target point 78 therein (more clearly shown in FIG. 6), which target point 78 may be defined by orthogonal grooves 80 formed in the upper surface of the target plate 72, or other means as desired. The target plate 72 has an edge 82, which edge 82 and target point 78 define a distance 54a therebetween which is equal to the distance 54 between the edge 56 and the plumb line passage 52 of the plumb bob suspension member 50 of FIG. 5A (and the longitudinal axis of a plumb bob suspended thereby). Thus, when the respective edges 56 and 82 of the plumb bob suspension member 50 and the target plate 72 are precisely vertically aligned with one another, the plumb line passage 52 of the suspension member 50 (and accordingly the plumb line 24 and plumb bob 10 with its longitudinal axis) and the target point 78 of the target plate 72 are correspondingly vertically aligned.
FIG. 6 discloses a perspective view of the apparatus of FIGS. 5A and 5B in use. In FIG. 6, the plumb bob suspension member 50 is placed in contact with an upper corner C1 of walls W1 and W2, while the target plate is placed in the corresponding lower corner of the walls W1 and W2, similarly to the apparatus of FIG. 4 discussed above. The length of the telescoping upper and base column components 66 and 68 is adjusted in order to place the suspension member 50 adjacent the top plate T of the wall W1 when the target plate 72 is adjacent the bottom plate B. Handles 84 are provided on the column 66 for ease of handling the apparatus and placing it in position as desired. The two handles 84 are symmetrically offset laterally from the plumb line L established when the apparatus is vertical, in order to allow free passage of the plumb line or laser line L therebetween.
It will be seen that any slight angular play between the two extension column members 66 and 68 is of no consequence, as the plumb bob 10 is not rigidly secured to the suspension member 50, but is free to swing therefrom by means of the string or line 24. Thus, even if the upper column is not perfectly vertical, and thus the plumb bob suspension member or plate 50 is not perfectly horizontal, the plumb bob 10 will still be vertically aligned due to its freedom of movement. The accuracy of the present apparatus is not compromised to any appreciable degree, so long as the plumb bob suspension member or plate 50 is disposed generally horizontally. Accordingly, it will be seen that the various embodiments of the present invention require precision of assembly only for the laser device within the plumb bob body, and that the remaining apparatus may be assembled in the field and used without regard for extreme precision of assembly of the components.
While the present invention is primarily directed to a laser plumb bob 10 and apparatus providing for the use thereof by a single person, it will be seen that the apparatus embodiments of FIGS. 3a, 3B, 4, 5A, 5B, and 6 may be used with conventional plumb bobs suspended from a plumb line essentially the length of the wall height, with the lower end of the plumb bob in close proximity to the target. While the use of a conventional plumb bob fails to provide the conveniences of the present laser plumb bob (i.e., ability to be seen more readily in low light conditions, more rapid damping of oscillations, etc.) as explained above, the plumb bob apparatus may nevertheless be used with such conventional plumb bobs, thereby providing for their use by a single person and providing corresponding economies of operation during construction.
It will also be seen that, although FIGS. 4 and 6 of the drawings show the present apparatus being used to plumb a corner in a wall frame construction, thus simultaneously determining whether two adjoining walls are vertical, that the apparatus may just as easily be used to plumb a single wall.
It is to be understood that the present invention is not limited to the sole embodiments described above, but encompasses any and all embodiments within the scope of the following claims.
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A laser plumb bob uses a conventional blumb bob body, hollowed to include a laser device therein. The laser device is affixed within the plumb bob body to preclude relative movement therebetween, to ensure accuracy for the device. With the use of a laser to provide a plumb line of coherent light which beam does not spread, the plumb bob may be suspended from a relatively short line in order to dampen oscillations more quickly. Apparatus providing for use of the plumb bob by a single person is also disclosed, comprising an upper fixture from which the plumb bob is suspended, an extension arm, and a target. The target and upper fixture may be connected by a telescoping column, if desired. The upper fixture may include a wind shield or guard, if desired, so provide greater stability for the plumb bob. The apparatus allows a single person to check plumb lines for walls and the like, thus providing greater efficiency and economy in building construction. The apparatus may also be used with a conventional plumb bob, if desired.
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[0001] This invention relates to image enhancement systems and more particularly to the dynamic control of image enhancement during multiple image display.
BACKGROUND OF THE INVENTION
[0002] It is well known that the sharpness of a displayed picture can be enhanced by peaking certain spatial frequencies of the displayed signal and, or, by modulating the scanning velocity of the display electron beam. Typically, spatial frequency peaking is performed by a circuit arrangement which changes the amplitudes of certain spatial frequencies without altering their relative phase relationships. Such peaking can be achieved with a cosine equalizer or transversal filter. With scanning velocity modulation, a derivative of the luminance portion of the display signal is employed to vary the velocity of the scanning beam. Slowing the scanning beam causes a greater number of electrons to land at a particular point in the displayed image causing a brightening of the display at that particular image location. Conversely, accelerating the scanning velocity at a particular point in the displayed image results in a darkening of the display. Thus, horizontal rate edges are visually enhanced by the variation of display intensity about the edge thus making the rise time of the edge appear steeper or sharper.
[0003] With the convergence of television and computer displays, so called multimedia monitors provide the ability to display images from multiple sources, such as, conventional NTSC, high definition television as defined by the Advanced Television System Committee (ATSC) standards as well as various computer image formats. This array of display signal sources represent a range of differing scanning frequencies and spatial frequency content. Put simply, high definition television has more lines and greater spatial frequency content, and thus is sharper than a conventional NTSC signal. Hence, this range of display signal formats introduces significant display complexity in, for example, the areas of multifrequency time base generation and synchronization, high voltage generation, and sharpness or image enhancement.
[0004] Complexity resulting from the range of signal sources is further complicated when the multimedia monitor simultaneously displays images from multiple, differing sources. The simultaneous display of multiple images is known as picture in picture or PIP or alternatively picture out of picture POP. A special implementation of POP is a side by side display of pictures comparable in size, and by implication, resolution or apparent sharpness. In addition, on screen messages are employed for user setup, control, or indication. However, because these computer generated messages are formed within the display device their representative signals are not subject to the bandwidth constraints or frequency response losses suffered by signals originated external to the display, for example NTSC or ATSC broadcast signals. Hence, to prevent unnecessary display enhancement, which likely results in image distortion of such OSD messages, it is known to inhibit enhancement during the occurrence of an OSD message.
[0005] Clearly a PIP or POP display with images of different scanning frequencies requires that scanning frequency conversion is implemented to enable the simultaneous display by PIP or POP. Furthermore, it can be appreciated that such displays with converted images from different scanning rate sources inevitably are of different signal bandwidth with spatial frequency content that differs from the main picture. Hence this suggests that the PIP or POP display format will receive less than optimum image enhancement when subject to a peaking or sharpening arrangement optimized for the typical spatial frequency content occurring with a single input or specific signal format.
SUMMARY OF THE INVENTION
[0006] In an inventive method, display image sharpness is controlled in a video display apparatus operable to display first and second images simultaneously. The method comprises the steps of; combining the first and second images to form a simultaneous display; and independently controlling the sharpness in accordance with each of said first and second images combined to form the simultaneous display.
[0007] In a further inventive arrangement, display image sharpness is dynamically controlled in accordance with the sources of the displayed images forming the simultaneous display.
[0008] In another inventive arrangement, display image sharpness is dynamically controlled in accordance with the spectral frequency content of the sources forming the simultaneous display.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] [0009]FIG. 1A depicts a simultaneous display of multiple pictures having a picture in picture arrangement.
[0010] [0010]FIG. 1B depicts a simultaneous display of multiple pictures having a picture out of picture, side by side arrangement.
[0011] [0011]FIG. 2 is a block diagram showing an inventive display signal processing arrangement to form a simultaneous display with video peaking and scanning beam velocity modulation.
[0012] [0012]FIG. 3A is a diagram depicting the variation of a peaking with input signal amplitude in a typical enhancement arrangement.
[0013] [0013]FIG. 3B is a diagram depicting the variation of a peaking with input signal amplitude in an inventive enhancement arrangement.
[0014] [0014]FIG. 4 is a block diagram showing an inventive dynamically controlled video peaking arrangement.
[0015] [0015]FIGS. 5A, B and C show impulse and amplitude frequency responses for the inventive dynamically controlled video peaking arrangement of FIG. 4.
[0016] [0016]FIG. 6 is a schematic diagram of an scanning velocity modulation arrangement with dynamic control of SVM signal amplitude.
DETAILED DESCRIPTION
[0017] [0017]FIG. 1A depicts an exemplary wide screen display apparatus, for example having a 16:9 aspect ratio, and showing a simultaneous display of two input picture sources having a picture in picture arrangement. The generation of a picture in picture or PIP arrangement is well known. However, in simple terms a picture in picture is formed by effectively cutting a hole in the main picture, which in exemplary FIG. 1A is St George slaying a dragon. The hole is then filled with a significantly smaller picture, for example the dogs. The switching signal is shown adjacent to the vertical and horizontal edges of FIG. 1A, in actuality the switching signal PIP/POP FSW or fast switch is only present for part of the vertical scan, as indicated by the indicator Vpos, which determines the vertical location.
[0018] The small image forming the PIP may be generated by a variety of well known methods, for example by so called electronic speed up where the image is time compressed horizontally by reading from a memory at a rate higher than its writing speed. The image width may also be reduced by deleting and or interpolating groups of pixels. In addition various combinations of deletion, interpolation and speedup can be employed. The vertical inserted picture dimension may be reduced by deleting or interpolating groups of lines to achieve the desired inserted picture height. Clearly which ever method is selected to reduce the size of the inserted picture, the spatial frequency content of the inserted picture or PIP will be significantly altered. For example, if electronic speed up is used to reduce the PIP image width by an exemplary 80%, i.e. the PIP is to occupy ⅕ of the screen width, the resulting spatial frequency content of the minified image will have been up converted by five times. Hence an ATSC picture source with a modest horizontal resolution of 25 MHz will result in a PIP image with spectral frequency components of 125 MHz. Although such frequency components can be generated, processed and coupled for display, it is doubtful that in such an up-converted image the phase relationships would be maintained to yield a smaller image with the same scene detail as the original picture. Furthermore such high speed processing may be precluded by cost considerations. Additionally the display screen structure, phosphor dot pitch, display viewing distance and human visual acuity will also contribute to diminished detail in the PIP image.
[0019] To minimize the up converted frequency content of a minified image it is usual to decimate, sub-sample or interpolate the PIP image signal to produce the minified image. This processing not only reduces the horizontal size but also reduces the spatial frequency content. To prevent the introduction of geometric distortion as the PIP image width is reduced the original aspect ratio must be maintained by reducing the PIP image height in accordance with the change in horizontal size. Hence, PIP image processing inherently reduces the spatial frequency content of the minified image in both horizontal and vertical directions resulting in a soft or un-sharp appearance. Although the minified image lacks detail it is capable of providing a useful indication of picture activity, for example the scoring of a goal or end of a commercial break. However, it can be appreciated that if an option allows the minified image to be increased in size, then the compromises employed for size and resolution reduction need to be reconsidered in order to display a PIP image with a useful but fuzzy picture content.
[0020] [0020]FIG. 1B depicts an exemplary wide screen display apparatus showing a special implementation of picture out of picture or POP, where pictures of comparable size are presented side by side. Such side by side presentation allows direct image comparison with any resolution differences being quite apparent. Thus there is a requirement that the apparent sharpness of the two images be sufficiently similar, which by implication suggests that the two halves be similarly processed to yield comparable alterations in the picture detail.
[0021] As discussed previously, to maintain picture geometry and aspect ratio, the height must be changed in proportion to the width. However, in a side by side display the individual picture width may be altered by cropping and discarding the edges of each image. For example, in FIG. 1B the left and right edges of each image have been removed such that the combined POP width fills the screen. Thus strips of one quarter the picture width are removed from each edge of each picture. The individual picture height remains unchanged however, thus although no geometrical image distortion has resulted, the image aspect ratio has been altered from an exemplary 16:9 to 8:9.
[0022] In both FIGS. 1A and 1B a horizontal broken line is shown dissecting the screen picture, and as described previously a switching signal PIP/POP fast switch is shown illustrating the timed, or positional occurrence of the alternate picture material. In view of the potential for differential displayed image resolution alteration an inventive arrangement employs a combination of the exemplary fast switching signal and other signals indicative of display signal origin to dynamically control the displayed image enhancement in each picture part by control of either or both video signal peaking and scanning beam velocity modulation.
[0023] [0023]FIG. 2 is a block diagram showing a display signal processing arrangement for the simultaneous display of at least two image sources with an advantageous dynamic control of video peaking and scanning beam velocity modulation specific to the image content of the display. The number of different input signal sources, for example ATSC, NTSC, computer (SVGA), DVD and VHS when combined with the possible simultaneous image displays of PIP, POP and side by side presentations can be optimally enhanced by use of multiple, for example 5, differing levels of enhancement at for example two selectable peaking frequencies. Furthermore specific image content may be beneficially enhanced by use of simultaneous peaking at both frequencies but with different contributions at each frequency, individually controlled to provide specific enhancement effects.
[0024] In addition simultaneous image displays may be further enhanced by controlled interaction between video signal peaking and scanning velocity modulation. In FIG. 2 signal sources for display are input to the display apparatus via an input selection arrangement 100 , which for example, may include tuners for NTSC and ATSC radio frequency signal reception, and or base band signal input from sources such as VCR, DVD, camera, computer, video games etc. Included within input selector 100 is digital video processing which performs picture size manipulation as required by user selection for example, PIP, PIP position and or size, POP position or side by side display. Associated with input signal source selector 100 is controller 150 which facilitates input or display signal selection and provides control and timing waveforms throughout the display apparatus. In particular controller 150 generates fast switching signals for PIP/POP insertion, and on screen display, OSD, messages and insertion signal OSD FSW.
[0025] The signal selector 100 is shown with output signals Y main and Y PIP which are coupled to block 200 where they are combined to form a simultaneous display signal. As described previously, the minified PIP, or POP image, is inserted into the main signal responsive to the timing, or position, of the PIP fast switch signal relative to the main luminance signal synchronization. Often video frequency peaking is implemented in the main signal path prior PIP signal insertion. However, in exemplary FIG. 2 the combined main and PIP or POP Y image signal is coupled to an advantageous dynamically controlled video peaking circuit depicted as block 300 which can change peaking amounts during active picture time. The choice of input signal for advantageous dynamically controlled video peaking in no way effects the dynamic operation of the video peaking arrangement.
[0026] The peaked luminance signal 301 with the PIP or POP image combined is coupled for on screen display, OSD, message insertion in block 400 . As described for PIP insertion, an OSD fast switch signal is used to position the insertion point of the on screen message. The OSD fast switch signal can blank or reduce the signal amplitude of the main signal being overwritten by the OSD message. However, if the main signal is reduced in video amplitude to produce a transparent effect behind the on screen message it is then advantageous to dynamically reduce or remove enhancement of the main signal for the duration of the OSD presence during trace time. Such dynamic control is facilitated by controller 150 which generates the OSD fast switch signal, controls the transparent OSD insertion and provides an additional dynamic control element to control signals Ctrl 1 and Ctrl 2 coupled to transversal filter 300 .
[0027] Following screen message insertion the peaked luminance signal 401 is coupled to a video processor block 500 where display drive signals are formed. In the prior description only the luminance signal component has been discussed, however comparable image manipulation and minification processing is performed on the coloring signal components prior to coupling to video processor block 500 to form exemplary red green and blue image display signals. The image display signals are coupled to an exemplary cathode ray tube for display and further enhancement by modulation of the scanning beam velocity by an SVM coil located on the CRT neck responsive to high frequency components or the derivative of the luminance signal.
[0028] A scanning beam velocity modulation signal is formed from the luminance component of the display signal and is suitably processed to generate a current which is coupled to the SVM coil to perturb the scanning speed of the horizontal component of the deflection field. The SVM signal may be generated from a luminance component Y″ formed prior to, or following luminance signal enhancement however, it is known to inhibit SVM enhancement during OSD and simultaneous image display. In FIG. 2 however, the SVM signal is generated from a luminance component signal Y′ within video processing block 500 subsequent to PIP and OSD insertion. The variety of image sources that can comprise the simultaneous image each with different degrees of resolution or apparent sharpness, suggests that optimum SVM enhancement of the displayed image can be achieved by dynamic control of the SVM signal amplitude. Thus by deriving the SVM signal from the final, or display signal luminance, it is possible to dynamically control enhancement of the individual image parts comprising the actual display signal. For example, SVM enhancement may be varied by dynamic control of the SVM signal amplitude. With an exemplary PIP display comprising a computer derived main picture and an inserted broadcast PIP image, the SVM amplitude may be advantageously reduced by 6 dB during the main picture with the SVM signal amplitude increased, or a 6 dB reduction dynamically removed for the duration of the PIP image insert.
[0029] [0029]FIG. 3A is a diagram depicting the variation of video peaking or sharpening with input signal amplitude in a typical enhancement arrangement. Often peaking is inhibited below certain input signal amplitudes to prevent enhancement of low level noise and consequently low signal levels too. As has been described previously, because differing spatial frequency content occurs in a simultaneous image display, differing image enhancement characteristics are required to provide an optimized correction for each part of the simultaneous image. FIG. 3B depicts an exemplary variation of a peaking amplitude, or sharpness effect, with input signal amplitude in an inventive arrangement. In FIG. 3B various different signal sources are considered with a corresponding sharpness or enhancement characteristic. For example, an HDTV or ATSC signal source may contain spectral signal components in the range of 30 MHz hence image sharpening can be performed as in curve 1 to enhance a band or range of frequencies in excess of the usual image frequencies contained in an NTSC signal. Thus the ATSC curve is depicted with the lowest degree of image enhancement or sharpening. Conversely an NTSC signal source may be subjectively improved by significantly greater amounts of peaking, as depicted in curve 2 , applied over a lower band of frequencies and possibly occurring at a lower video signal level. A PIP image is small and significantly reduced in sharpness, hence may benefit subjectively by enhancement of the signal components remaining in the minified picture part. Curve 3 depicts an empirically determined level of PIP image enhancement which provides a subjective improvement in sharpness if applied with a greater amplitude over a range of frequencies different from those selected for either NTSC or ATSC picture enhancement. Curve 4 depicts levels of enhancement which can be employed to sharpen an up converted NTSC signal source when presented as a PIP display.
[0030] To facilitate the range of enhancement characteristics discussed with reference to FIG. 3B an inventive dynamically controlled video peaking arrangement, shown in FIG. 4, is employed. The block diagram shown in FIG. 4 is illustrative of a peaking arrangement or transversal filter which can be implemented in analog form for use with base band video signals, analog delay lines and analog multipliers. Similarly a digital configuration may be used with digital representation of the video signals, digital shift registers and adders or multipliers. The function and control are substantially the same for either analog or digital circuit implementation. The transversal fitter may, in simple terms, be considered to function as a peaking arrangement where the main signal SM is combined with inverted and attenuated time shifted versions of the input. Thus if the main signal SM is considered to be an impulse, it is augmented by leading and trailing echoes of the impulse, spaced in time by the duration of the delay paths. Thus the summation of inverted, attenuated and time shifted versions of the input signal may be thought of as contributing pre and post lobes to increase the perceived sharpness by reducing the apparent rise time of the impulse signal. FIGS. 5A, 5B and 5 C illustrate the effect of the summation of the inverted pairs of echoes in both time and frequency domains. The transversal filter depicted in FIG. 4 provides dynamically controlled peaking in two bands of frequencies with an amount of overlap or additional enhancement occurring in the overlapping band between the individual peaking frequencies. However, there is no requirement that the bands over lap or that the number of bands be limited to two. For example, in the peaker shown in FIG. 4, delay elements D 1 -D 4 each have the same delay value, for example 74 nano seconds, which represents the period of an ITU 601 sampled signal. Thus maximum enhancement with signal HFpk occurs at approximately 13.5 MHz due to delay elements D 3 and D 4 . The lower frequency enhancement signal LFpk peaks at 6.75 MHz due to the additive effect of Dl plus D 3 and D 2 plus D 4 . Similarly a delay value of 37 nano seconds will produce a high frequency correction peak at 27 MHz with a lower frequency peak at 13.5 MHz. The use of transversal filters with selectable multiple frequency bands is well known. For example, in a video and deflection processing integrated circuit for example Toshiba type TA1276N provides six different peaking frequencies which are selectably controlled via a serial data bus as typified by the I 2 C bus. Although the peaking frequency may be selected via the bus, simultaneous operation at two or more frequencies is not facilitated. Furthermore, the limited transmission speed of the I 2 C data bus, for example 400 Kb/s permits only static filter selection and user sharpness control manipulation. Such I 2 C data bus control precludes the dynamic control of peaking amount or frequency selection required to facilitate selective enhancement of the individual picture parts comprising a simultaneous PIP or POP image.
[0031] Clearly a digital filter implementation with delay elements provided by clocked devices more readily permits the construction of multifrequency filters than with analog signals and delay lines. Thus a digital signal processing embodiment provides greater flexibility for shaping the peaking characteristic to correct or enhance signals subject to other than gaussian shaped losses.
[0032] With reference to FIG. 4, an analog or digital video signal is input at terminal A and is coupled to delay element D 1 and via an inverter and attenuator, not shown, to provide an input signal with an amplitude of minus one quarter that of the input signal at summing device SUM Lf. The delayed main signal, HfE, is coupled to a second summing device SUM Hf and to a second delay element D 3 . Signal HfE, is coupled via an inverter and attenuator, not shown, to provide an input signal with an amplitude of minus one quarter that of the input signal at summing device SUM Hf. The output signal SM from delay element D 3 is coupled to delay element D 4 and to summer SUM O/P where enhancement signals HFpk and LFpk are added to form a peaked luminance output signal Yenh.
[0033] The output from delay D 3 is attenuated, for example by one half, and coupled to summers Hf and Lf where respective correction signals Hf Cor and Lf cor are formed. From delay element D 4 an output signal HfL is coupled as a third input to summing device SUM Hf, via an inverter and attenuator, not shown. Output signal HfL is also coupled to delay D 2 which produces an output signal LfL for coupling through an inverter and attenuator, to form the third input to summing device SUM Lf. The output signals HfCor and LfCor from respective summers SUM Hf, and SUM Lf are each coupled to respective control devices CTHfpk and CTLfpk which are advantageously individually, dynamically controlled in amplitude by respective control signals Ctrl 1 and Ctrl 2 .
[0034] The dynamic control signals are generated by controller 150 in response to the selected video image source, which is indicative of likely spatial frequency content, and the type of display presentation, i.e. normal, PIP or side by side. For example, an ATSC image signal may be enhanced by the addition of only amplitude controlled higher frequency signal components as represented by signal Hfpk. Whereas an NTSC signal may be optimally enhanced with the addition of lower frequency signal components Lfpk. Similarly PIP image content may require enhancement in both low and high frequency bands with an maximum enhancement occurring between the low and high frequency peaks, as illustrated in FIG. 5C by the dashed curve annotated 2 Pk Freq. An up converted image derived from an exemplary NTSC source, although subject to a nominal 2:1 spatial frequency translation, is still significantly less sharp particularly when displayed side by side with an ATSC or computer generated image. Consequently the up converted image is enhanced in both low and high frequency bands to improve perceived sharpness and lessen visible differences.
[0035] Controller 150 generates the advantageous dynamic control signals Ctrl 1 and Ctrl 2 which are coupled to provide independent control of the high frequency and low frequency multipliers Hfpk, Lfpk respectively. For example, in a PIP display the fast switch signal determines the inserted location of the minified image, hence it can be used to advantageously control the degree of enhancement, and the frequency band or bands in which the spectral components of the PIP image will be enhanced. Selection between peaking frequency bands is achieved by means of the control signals Ctrl 1 and Ctrl 2 , which, for example, when either is set for zero enhancement results in zero peaking at that peaking frequency. Clearly in a digital implementation of the transversal filter the fast switch signal (Fast Sw) can be represented by a digital word or words which change value in synchronism with the fast switch signal. Since controller 150 provides independent control of enhancement at each peaking frequency, certain simultaneous images may be optimally enhanced by dynamically and independently controlling the peaking frequency and enhancement amount. At image boundaries between the main and PIP or POP pictures, significant enhancement changes can occur which can potentially result in undesirable transitional peaking effects. Advantageously such undesirable peaking transitions are avoided by controlling the rate, or number of clock periods over which the control words assume the new value. In an analog system the fast switch signal would be filtered to produce a gradual, ramping change in enhancement effect at the PIP boundary.
[0036] [0036]FIG. 6 is a detailed circuit diagram showing an exemplary scanning velocity modulation (SVM) amplifier with advantageous dynamic control of SVM signal amplitude responsive to a digital control word for example Ctrl 1 /Ctrl 2 . As described previously the apparent sharpness of multiple image portions, displayed simultaneously on a single screen, can be optimized by dynamically controlling the degree of signal peaking or enhancement applied to each part of the displayed picture. Typically, scanning velocity modulation for image enhancement is achieved by the SVM system within a limited range of input signal amplitudes in order to produce a sustained, maximized level of enhancement. The sustained SVM signal amplitude is usually controlled by peak to peak SVM signal limiting and often includes a negative feedback loop which samples the coil driver amplifier current to prevent excessive power dissipation. There are also arrangements which employ feed forward open loop signal amplitude control to constrain unintentional emissions within a mandated amplitude/frequency range. However, in the exemplary arrangement shown in FIG. 2, the SVM signal is derived from the enhanced simultaneous display signal hence an advantageous feed forward signal is employed to dynamically control SVM signal amplitude. Because the SVM amplitude is dynamically controlled prior to peak to peak limiting, for example in differential amplifier 601 or diode clipper 602 , the subsequent drive circuitry is thereby prevented from sustained or continuous peak to peak clipping of the SVM signal which consequentially diminishes or degrades image enhancement. Furthermore such sustained peak to peak clipping of the SVM drive signal will, as a result of the clipped signal increase power dissipation in the driver stage cause SVM amplitude degeneration to be invoked to controllably reduce output power dissipation in the SVM coil driver amplifier.
[0037] As described previously the sharpness of multiple images displayed simultaneously on a single screen can be optimized by dynamically controlling the degree of peaking applied to each separate image portion of the displayed picture. Thus in an advantageous arrangement digital control bits are coupled to dynamically control the amplitude of the SVM signal applied to the SVM coil to optimize edge enhancement of the individual multiple image portions.
[0038] As discussed with regard to the transversal filter, controller 150 generates a digital control word in response to the signal source selected for display together with the nature of the displayed image, for example, PIP, side by side or POP. The digital control word may for example comprise 3 bits and as depicted in FIG. 6 be used to dynamically control the SVM signal amplitude and hence the degree of SVM derived image enhancement. In FIG. 6 a luminance signal, Y is coupled via capacitor C 1 to the base electrode of transistor Q 2 , which is configured as an emitter follower. A discussed previously with regard to FIG. 2, this luminance input signal may be derived as signal Y′ from video processor 500 or as signal Y″ formed in processing block 200 . Resistors R 10 , R 11 and R 12 form a potential divider connected between power supply, +VA, and ground for determining the base voltages of transistors Q 2 and Q 4 . The collector of transistor Q 2 is connected to power supply, +VA, typically 24 volts, and the emitter is coupled via resistor R 13 to the emitter electrode of a grounded base amplifier formed by transistor Q 4 . The base electrode of transistor Q 4 is connected to the junction of resistors R 11 and R 12 and is decoupled ground by capacitor C 2 .
[0039] The amplified luminance signal at the collector of transistor Q 4 is differentiated by a parallel connected network formed by capacitor C 5 , inductor L 2 and damping resistor R 19 connected between the transistor collector and ground. The differentiated luminance or SVM signal formed at the collector of transistor Q 4 is coupled via capacitor C 3 and resistor R 20 to the base of transistor Q 6 which together with transistor Q 8 form differential amplifier 601 . A resistor R 21 is coupled to the junction of capacitor C 3 and resistor R 20 to bias the base of transistor Q 6 to the same potential as that of transistor Q 8 . The gain of the differential amplifier is set by resistors R 26 and R 28 , R 36 and the collector current from current source transistor Q 7 . Resistors R 25 , R 33 and R 34 form a potential divider that provides biasing voltages for transistors Q 6 , Q 7 , and Q 8 , where transistor Q 6 is biased via resistors R 20 and R 21 and transistor Q 8 is biased via resistor R 30 . The junction of resistors R 21 , R 30 , R 33 and R 34 is decoupled to ground by capacitor C 14 . Similarly capacitor C 11 decouples the junction of resistors R 25 and R 33 to ground. The collector electrode of Q 6 is directly connected to supply voltage +VA. The differential amplifier 601 formed by transistors Q 6 and Q 8 provides an amplified, amplitude controlled and peak to peak limited signal across resistor R 36 at the collector of transistor Q 8 . Peak to peak limiting can also be provided by an AC coupled reverse poled diode pair arrangement shown in 602 which allows peak to peak SVM signal limiting to be independent of amplifier gain and power supply considerations associated with amplifier 601 . The SVM signal from the collector of transistor Q 8 is coupled to a power amplifier (SVM DRIVER) which generates a current in the SVM coil to affect modulation of the scanning velocity of the horizontal component of the CRT scanning electron beam.
[0040] Block 650 shows the formation of an SVM control word from control signals Ctrl 1 and Ctrl 2 which can be combined and coupled to an exemplary digital to analog converter for example, as depicted within dashed boxes A and B. The digital to analog converter shown in box A includes transistor switches Q 1 , Q 3 , Q 5 .
[0041] Each transistor switch is driven to saturated conduction by a positive logic level, for example, +5 volts which corresponds to a logical 1 state. When anyone of the transistor switches is saturated an AC potential divider is formed at the base of transistor Q 6 by the series combination of ones of transistor switches, Q 1 , Q 3 , Q 5 respectively, collector load resistors R 1 A, R 2 A and R 3 A, DC blocking capacitor C 4 and resistor R 20 . When the SVM control word has a logical zero value, for example as represented by a zero voltage value, the transistor switches are turned off and no AC potential division occurs at the input of differential amplifier 601 . In this way a digital control word is converted to an analog signal attenuation value which determines the SVM signal amplitude and hence the degree of picture sharpening.
[0042] In a second embodiment, depicted within dashed box B, an SVM control word can be formed from control signals Ctrl 1 and Ctrl 2 for example by block 650 , and coupled to a digital to analog converter, for example, as depicted by transistor switches Q 1 , Q 3 , Q 5 . Each transistor can generate a current amplitude in proportion to respective collector resistors R 1 B, R 2 B and R 3 B. These digitally determined currents are summed to form current I. When the data bits have a zero volt, or logical zero value, a maximum current I is conducted from 5 volt positive supply (+). With data bits having a value of nominally 5 volts or logical 1 , the transistor switches are turned off and no digitally controlled currents are generated from positive supply (+).
[0043] The digitally derived currents forming current I are coupled to the junction of resistor R 27 and the emitter of current source transistor Q 7 . The other end of resistor R 27 is connected to ground. The collector of transistor Q 7 is coupled to the junction of resistors R 26 and R 28 which determine the gain in the differential amplifier. As current I from the digital to analog converter B increases, the voltage at the emitter of transistor Q 7 increases. The increase in emitter voltage causes the base emitter potential of transistor Q 7 to be reduced which in turn reduces the collector current. Thus as the current supplied to the differential amplifier is varied in response to the digital value represented by the data word coupled to digital to analog converter B, so too is the SVM output signal amplitude and thus the resulting degree of image enhancement. The variation of source current in the differential amplifier provides dynamic control the gain or amplitude of the SVM signal. Thus, the SVM signal amplitude and resulting enhancement is dynamically controlled in response to digital values derived for each picture part of the displayed image.
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A method for controlling image sharpness in a video display apparatus operable to display first (Ymain) and second (Ypip) image signals simultaneously. This comprises the steps of, combining a first image signal and a second (image signal to form a simultaneous display signal). Generating an SVM signal for display image enhancement in accordance with the simultaneous display signal. Dynamically controlling an amplitude of the SVM signal in accordance with an occurrence of ones of the first and second image signals forming the simultaneous display signal. Driving an SVM coil with the dynamically controlled amplitude SVM signal to enhance image edges displayed by the video display apparatus in accordance with ones of the first and second image signals.
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This is a divisional of application Ser. No. 09/168,026, filed Oct. 8. 1998, now U.S. Pat. No. 6,029,684 which is a divisional of application Ser. No. 08/843,660, filed Apr. 11, 1997, now U.S. Pat. No. 5,826,509.
FIELD OF THE INVENTION
This invention relates to inspection chambers for use in sanitary sewers, to an inspection chamber with an integral back-flow prevention valve, and to a tool for installing a back-flow-prevention valve in an installed inspection chamber.
BACKGROUND OF THE INVENTION
Inspection chambers are required to be provided in sanitary sewer systems in many jurisdictions. An inspection chamber is typically installed where the sanitary sewer outlet from a building joins the sewer main of a municipal sewer system. Inspection chambers serve two main purposes. First, during construction of a new sewage system an inspection chamber can be used as a location for a plug to seal the passage between the new sewage system and the sewer main until the new sewage system has been tested and approved. After testing and approval, the plug can be removed by hooking a handle on the plug and pulling the plug out of the inspection chamber. Second, an inspection chamber can be used as a point of access to remove blockages from a sewer system.
An inspection chamber is typically installed at least several feet underground. The inspection chamber typically has interior dimensions slightly larger than the diameter of the sewage outlet pipe in which it is installed. Typical diameters of sewage outlet pipes from residential or light industrial buildings are in the range of 4 inches to 6 inches. A generally vertical access pipe, which is typically somewhat larger in diameter than the sewage outlet pipe, extends from the inspection chamber to the surface where it is sealed with a cap. The access pipe is typically several feet long. Typical diameters of access pipes are in the range of about 6 inches to 10 inches. After an inspection chamber has been installed it is very difficult to gain access to the inside of the inspection chamber.
It is generally desirable to provide a back-flow valve in the sewage outlet pipe. A back-flow valve serves to prevent sewage from backing up from the municipal sewer into a building. The back-flow valve also serves to prevent vermin, such as rats, from entering a building from the municipal sewer lines through the building's sewage outlet pipe. A problem with back-flow valves is that they are installed in the sewage outlet line which is several feet underground. If the back-flow valve malfunctions or if debris gets stuck in the back-flow valve then it is generally necessary to dig down to the back-flow valve to replace or repair it. This is both disruptive and expensive.
The inventors have recognized a need for an inspection chamber which can be plugged, as described above, during testing and approval of a sewage system and has an integral back-flow valve. It has not been previously practical to provide such an inspection chamber because any back-flow valve would interfere with insertion or removal of a plug. After the plug has been removed the inspection chamber is several feet down the access pipe and is not easily accessible.
SUMMARY OF THE INVENTION
This invention provides an inspection chamber with an integrated back-flow prevention valve. One aspect of the invention provides an inspection chamber for a sanitary sewer line. The inspection chamber comprises: a housing having inlet outlet and access ports for connecting inlet, outlet and access pipes and a flapper valve in the housing. The access port is located in an upper portion of the housing and is oriented generally perpendicularly to each of the inlet and outlet ports. The flapper valve comprises: a valve member comprising a transverse pin, a flap member attached to the pin and a handle member projecting from a central location on the flap member; a clip for receiving the pin of the valve member and detachably retaining the pin in pivotal relation to the housing, the clip located below the access port and above the inlet port and oriented to receive the pin from a direction of the access port; and a sealing surface inside the housing around the inlet port. When the pin of the valve member is received in the clip, the flap member bears against the sealing surface and is capable of blocking a flow of sewage from the outlet port through the inspection chamber and out the inlet port and the valve member can pivot about the pin to permit sewage to flow from the inlet port, through the inspection chamber and out the outlet port.
A second aspect of the invention provides a sanitary sewer system comprising: a sewage outlet pipe extending from a building to a municipal sewer and an inspection chamber connected in the sewage outlet pipe at an underground location between the building and the municipal sewer. The inspection chamber comprises: a housing having an inlet port connected to a portion of the sewage outlet pipe extending to the building, an outlet port connected to a portion of the sewage outlet pipe extending to the sewer, an access port connected to an access pipe extending generally vertically to an unburied location, the access port in an upper portion of the housing oriented generally perpendicularly to each of the inlet and outlet ports; and a flapper valve in the housing. The flapper valve comprises: a valve member comprising a transverse pin, a flap member attached to the pin and a handle member projecting from a central location on the flap member; a clip for receiving the pin of the valve member and detachably retaining the pin in pivotal relation to the housing, the clip located below the access port and above the inlet port and oriented to receive the pin from a direction of the access port; and a sealing surface inside the housing around the inlet port. When the pin of the valve member is received in the clip, the flap member bears against the sealing surface and is capable of blocking a flow of sewage from the outlet port through the inspection chamber and out the inlet port and the valve member can pivot about the pin to permit sewage to flow from the inlet port, through the inspection chamber and out the outlet port. A sealing lid is provided at a top end of the access pipe.
The invention also provides a method for installing a flap valve valve member in an inspection chamber in a sanitary sewer system. The method comprises the steps of: providing a valve member comprising a transverse pin, a flap member attached to the pin and a handle member projecting from a central location on the flap member; attaching the valve member to a holder on an installation tool comprising an elongated shaft, the holder comprising means for holding the handle member and a tab adjacent the pin; lowering the valve member through an access port on the inspection chamber with the installation tool; aligning the pin with a clip in the inspection chamber; hammering the installation tool downwardly to cause the tab to press the pin into engagement in the clip; and removing the installation tool.
In a preferred embodiment, the step of attaching the valve member to a holder on an installation tool comprises inserting the handle member between a pair of fingers biased toward each other. Preferably the step of hammering the installation tool downwardly comprises sliding a weight upwardly along the shaft of the installation tool and dropping the weight onto a stop on the shaft. The method may further include the step of removing the valve member from the inspection chamber by the steps of engaging a ring in the handle member with a hook and pulling the hook upwardly after the step of removing the installation tool.
Yet another aspect of the invention provides a tool for use in practising the methods of the invention. The tool can be used to install a flap valve valve member in an inspection chamber in a sanitary sewer system. The tool comprises an elongated shaft extending from to a handle to a holder, a stop on the shaft between the handle and the holder and a weight slidably mounted to the shaft. The holder comprises: first and second generally parallel opposed fingers spaced apart by a distance sufficient to receive a handle member projecting from a flap valve member; bias means for resiliently displacing the first finger toward the second finger for releasably pinching a handle member projecting from a flap valve member between the first and second fingers; and a tab projecting from the holder generally perpendicularly to the shaft at a base of the fingers, between the handle and the stop.
Yet another aspect of the invention provides a sealing lid for an access pipe of an inspection chamber in a sewer system. The sealing lid comprises a circular plastic body, a piece of a ferromagnetic material moulded into the plastic body, a sealing member extending peripherally around the plastic body, and a pair of opposed locking members each comprising a lug member pivotally mounted to the plastic body and a stop member projecting adjacent the lug member. The stop members allow rotation of the lug members between engaged and disengaged positions.
BRIEF DESCRIPTION OF THE DRAWINGS
In drawings which illustrate preferred but non-limiting embodiments of the invention:
FIG. 1 is a schematic elevational view of an inspection chamber installed in a sewage system according to the invention;
FIG. 2A is a longitudinal section through the inspection chamber of the sewage system of FIG. 1;
FIG. 2B is a detailed view of a portion thereof;
FIG. 2C is a transverse section through the inspection chamber of the sewage system of FIG. 1 looking toward the inlet port thereof;
FIGS. 3A through 3H are views illustrating a sequence of steps for installing a valve member according to the invention in the inspection chamber of the sewer system of FIG. 1 with the tool of FIGS. 4A through 4D;
FIG. 4A is an elevational view of a tool for use in the methods of the invention;
FIGS. 4B, 4C and 4D are respectively side elevational and top plan views of a head for installing valve members in inspection chambers according to the invention for use with the tool of FIG. 4A and a side elevational view of a lateral hook for use in the invention with the tool of FIG. 4A; and,
FIGS. 5A, 5B and 5C are respectively a top plan view, a cross sectional view and a bottom plan view of a sealing lid for the access pipe of the sewer system of FIG. 1.
DETAILED DESCRIPTION
FIG. 1 shows a sewage system 10 according to the invention. Sewage system 10 carries wastewater from a building 12 to a sewer main 15 through a sewage outlet pipe 16. Sewage outlet pipe 16 lies in ground 17 and is inclined slightly toward sewer main 15. An inspection chamber 20 is located in sewage outlet pipe 16 A first portion 16A of sewage outlet pipe 16 extends from building 12 to an inlet port 22 of inspection chamber 20. A second portion 16B of sewage outlet pipe 16 extends from an outlet port 24 of inspection chamber 20 to sewer main 15. An access pipe 18 extends generally vertically from an access port 26 of inspection chamber 20 to the surface of ground 17. The upper end of access pipe 18 is closed by a sealing cap 19.
A back-flow prevention valve 30 is located in inspection chamber 20 adjacent inlet port 22. In use, sewage flows from building 12 through portion 16A of sewage outlet pipe 16, through inspection chamber 20 and to sewer main 15 through portion 16B of sewage outlet pipe 16. Valve 30 prevents vermin from entering building 12 from sewer main 15 and also prevents sewage from backing up from sewer main 15 and flowing into building 12 through portion 16A of sewage outlet pipe 16. Valve 30 comprises a valve member 32 pivotally attached inside inspection chamber 20.
A distinguishing feature of the invention is that valve member 32 and inspection chamber 20 are constructed so that valve member 32 can be inserted into inspection chamber 20 after inspection chamber 20 is in place under ground 17. This permits the use of inspection chamber 20 to receive a plug 21 (FIG. 3) plugging inlet port 22 from inside inspection chamber 20 while building 12 is under construction (as is required by some municipalities). As described below, the methods of the invention also permit valve member 32 to be removed and replaced through access pipe 18. As such, the invention provides significant advantages over the current state of the art which combines a conventional unvalved inspection chamber with a separate buried back-flow prevention valve.
The construction of inspection chamber 20 is shown in detail in FIG. 2. Inspection chamber 20 comprises a housing 40 formed from any suitable material such as injection moulded ABS plastic. Housing 40 supports suitable seals around ports 22, 24, and 26 for sealing connections to portions 16A and 16B of sewage outlet pipe 16 and access pipe 18. Any suitable seals known to those skilled in the art may be used. Those skilled in the art will realize that the shapes and dimensions of ports 22, 24, and 26 may need to be adapted for the particular type of seals used.
A valve seating surface 42 is provided inside housing 40 around inlet port 22. Valve seating surface 42 is preferably planar. Valve member 32 comprises a transversely mounted pin 34 attached to a flap member 36 by a short bridge member 37. Pin 34 is retained by a clip 44. Clip 44 permits pin 34 to pivot relative to housing 40 as indicated by arrow 46. Normally gravity holds valve member 32 with flap member 36 in contact with valve seating surface 42 so that valve 30 is closed. Wastewater or other sewage arriving at valve 30 pushes flap member in the direction of arrow 46, thereby opening valve 30. A suitable resilient sealing material 38 is provided either on seating surface 42 or on flap member 36. Preferably the sealing material 38 is on flap member 36.
Clip 44 preferably comprises a pair of upwardly projecting resilient fingers 48 which grip either end of pin 34 with bridge member 37 extending between fingers 48. Pin 34 is held in a recess 47 between fingers 48 and adjacent portions of the wall of housing 40. Fingers 48 are preferably moulded integrally with housing 40. Fingers 48 are oriented upwardly so that clip 44 detachably receives pin 34 when it is inserted from the direction of access port 26. A notch 49 is preferably provided between fingers 48 below recess 47. Notch 49 can be used to remove a broken valve member 32 as described below.
A handle member 50 projects from a central portion of flap member 36. Handle member 50 is used in the installation of valve member 32 in housing 40 as described below. In the currently preferred embodiment of the invention, handle member 50 comprises a ring 52 of approximately 1 inch in diameter projecting in a plane which bisects valve member 32. Ring 52 has a central aperture 54.
The method for installing valve member 32 in inspection chamber 20 begins with inspection chamber 20 buried in soil 17. Plug 21 plugs inlet port 22 from inside inspection chamber 20 as shown in FIGS. 3A and 3B. Plug 21 is then removed by hooking the ring handle of plug 21 with a hook 63 lowered through access pipe 18, pulling upwardly until plug 21 is released, and removing plug 21 through access pipe 18 as shown in FIG. 3C. Preferably hook 63 comprises a spring-loaded catch so that plug 21 cannot fall off from hook 63 after hook 63 has been fully engaged with the handle of plug 21.
Plug 21 may be removed with a tool 60 as shown in FIG. 4A. Tool 60 comprises a hook 63 connected to a handle 68 by a shaft 64 which is long enough to reach down access pipe 18 into inspection chamber 20. Shaft 64 may comprise several sections 66 so that the length of shaft 64 can be adjusted for the depth of inspection chamber 20.
As shown in FIG. 4A, tool 60 preferably has a weight 72 slidably mounted at the upper end of shaft 64 between handle 68 and a stop 70. Weight 72 preferably weighs about 1 kilogram. An upward pull on plug 21 may be achieved by sliding weight 72 upwardly against handle 68 to jolt hook 63 upwardly. In this case, handle 68 acts as a stop. A separate upper stop may be provided below handle 68 and above stop 70.
After plug 21 has been removed, hook 63 on tool 60 is replaced with a head 62. Preferably hook 63 and head 62 are each connected to the end of shaft 64 with a connector 65 so that they may be readily interchanged. Connector 65 may be a simple threaded fitting, as shown, which screws onto the end of shaft 64 or may be another suitable type of coupling.
A valve member 32 is then attached the head 62 of tool 60. As shown in FIGS. 4B and 4C, head 62 comprises a holder 74 for holding a valve member 32 by its handle member 50. In the currently preferred embodiment of the invention holder 74 comprises a pair of fingers 75, 76. A bolt 77 extends from first finger 75 through a hole in second finger 76. A compression spring 78 on bolt 77 resiliently compresses fingers 75 and 76 together.
Valve member 32 is attached to head 62 by sliding handle member 50 between fingers 75 and 76 so that it is securely but releasably pinched between fingers 75, 76 as shown in FIGS. 3D and 3E. When valve member 32 is attached to head 62 a tab 80 projecting from head 62 lies just above and adjacent pin 34. Holder 74 does not need to grasp handle member extremely tightly. It is only necessary to hold handle member 50 tightly enough to reliably lower valve member 32 through access pipe 18 and align it in inspection chamber 20 as described below.
Next, head 62 of tool 60 is lowered through access pipe 18 into inspection chamber 20 and aligned so that the ends of pin 34 extend between fingers 48 above recess 47 with bridge member 37 between fingers 48 as shown in FIGS. 3F and 3G. This is possible because, as noted above, fingers 48 are oriented so that pin 34 can be inserted into recess 47 from the direction of access port 26.
Pin 34 is then inserted into recess 47 by lifting weight 72 and dropping it onto stop 70. This causes portion 80 of head 62 to snap pin 34 downwardly into engagement in clip 44. If it is necessary, the step of lifting and dropping weight 72 to snap pin 34 into place can be repeated. At this point valve member 32 is installed in inspection chamber 20. All that remains is to disengage head 62 of tool 70 from handle member 50. This can easily be done by simply lifting handle 68 to draw fingers 75 and 76 off from handle member 50.
The methods of the invention can also be used to remove a valve member 32 from an inspection chamber 20. This might be required, for example, if it becomes necessary to clean sewer outlet pipe 16. If valve member 32 is intact then valve member 32 can be removed simply by hooking aperture 54 of handle member 50 with a suitable hook and pulling sharply upwardly. Tool 60 is preferably constructed so that head 62 can be removed and replaced with a hook 63 for this purpose. Hook 63 can also be used to remove plugs 21 as described above. When tool 60 is used this way then weight 72 can be hammered upwardly against handle 68 to provide sharp upward force on hook 63 to dislodge a valve member 32 or a plug 21.
If valve member 32 has broken off then it is still usually possible to replace valve member 32 without digging down to inspection chamber 20. Typically valve member 32 will break at bridge member 37 because bridge member 37 is generally the weakest part of valve member 32. If this happens then a small laterally extending hook 100 can be attached at the end of tool 60 in place of hook 63 or head 62 and inserted into notch 49. The laterally extending hook 100 can then be lifted upwardly to remove pin 34 from clip 44. The portion of a broken off valve member 32 attached to pin 34 is generally small enough that it can safely be left to wash into sewer main 15. The rest of valve member 32 including flap member 36 can be fished out from inspection chamber 20 by hooking handle member 50. The laterally extending hook 100 may be provided in a kit with a hook 63, a head 72 and other components of tool 60.
Sealing lid 19 is preferably made of a suitable plastic material. Sealing lid 19 preferably comprises a piece 90 of a ferromagnetic metal, such as iron or steel so that a metal detector can be used to rapidly locate sealing lid 19 and access pipe 18. Most preferably, sealing lid 19 is moulded from a suitable plastic material and piece 90 is moulded into sealing lid 19. For example, if sealing lid 19 is injection moulded then piece 90 can be placed into the mould before plastic is injected. After the plastic has been injected then piece 90 is partially or entirely encased in plastic.
Sealing lid 19 preferably comprises one or more locking members 92 for locking sealing lid 19 in place at the top of access pipe 18. Locking members 92 may comprise, for example, lugs 94 which can be turned to project outwardly and engage an inwardly projecting step 95 at the upper end of access pipe 18 using cap screws 96. Preferably, a post 98 is provided adjacent each of lugs 94. Posts 98 provide positive stops at the extended (as shown in solid lines in FIG. 5C) and retracted (as shown in dotted outline in FIG. 5C) positions of lugs 94.
While the currently preferred embodiment of the invention is described above, it will be clear to those skilled in the art that there are many ways to vary the designs of the various components described above without departing from the broad scope of the invention. For example, clip 44 could be any suitable kind of clip capable of receiving and detachably and pivotally retaining a valve member comprising a flap member 36 and oriented to receive the valve member from the direction of access port 26. While it is preferred, handle member 50 need not comprise a ring, as described. It is only necessary that handle member 50 provide a means for holding a valve member 32 to an tool 60 so that valve member 32 can be positioned in inspection chamber 20 and engaged with clip 44. It is preferable, however, that handle member 50 comprises a ring because a ring can be grabbed with a hook to remove a valve member 32. Tool 60 need not be equipped with a sliding weight 72. Although it is not preferred, a separate hammer could be used to hammer on an end portion of tool 60 instead.
As will be apparent to those skilled in the art in the light of the foregoing disclosure, many further alterations and modifications are possible in the practice of this invention without departing from the spirit or scope thereof. Accordingly, the scope of the invention is to be construed in accordance with the substance defined by the following claims.
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An inspection chamber for use in sanitary sewer systems has an integral back-flow prevention valve. The valve can be installed through an access pipe with the inspection chamber in place underground. The valve does not interfere with the installation or removal of a plug in the inspection chamber during construction and inspection of the sewer system. The inspection chamber comprises a clip oriented to receive a valve member from the direction of an access port. The valve member comprises a pin connected to a flap member by a narrow bridge member. The flap member has a projecting handle member. An installation tool holds the valve member by the handle member and provides a tab which can be hammered downwardly to snap the pin into the clip thereby securing the valve member in the inspection chamber. An inspection chamber according to the invention avoids the necessity of providing a separate buried back-flow prevention valve.
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RELATED APPLICATION DATA
This invention is related to 1) commonly assigned U.S. patent application Ser. No. 09/017,011 entitled: "Intra-Unit Column Address Increment System for Memory"; 2) commonly assigned U.S. patent application Ser. No. 09/017,015 entitled: "Single Ended Read Write Drive For Memory"; and 3) commonly assigned U.S. patent application Ser. No. 09/017,012 entitled: "Shared Row Decoder"; the three of which are filed on even date herewith.
FIELD OF THE INVENTION
This invention relates to the design of a random access memory (RAM) and more specifically to circuitry which accesses and transfers data with a set of address inputs to and from a storage array within a RAM.
BACKGROUND OF THE INVENTION
Maximization of storage capacity and minimization of power usage and access time are goals in the design of integrated circuits (ICs, "chips"), especially as to ICs containing memory and logic arrays for use in data processing systems.
I. Row Decoder Design
To increase the storage capacity of a random access memory (RAM), it is important to find ways to reduce the amount of area occupied by circuitry other than the storage cell arrays of the RAM. One way in which this can be accomplished is by utilizing a shared row decoder design which permits wordlines in both left and right units of a bank division of the RAM to be accessed through the same set of row decoders, thus decreasing by half the number of row decoders required to perform that function. However, this goal is not well served if the reduction in decoder circuitry is made at the expense of increased access time or higher power consumption for the RAM, especially in cases where the design for a RAM chip requires a plurality of banks.
FIG. 1 shows an example of a 32 Mb double unit 10 which includes left and right units 12, 20, left and right wordline (WL) driver units 14, 18, and a shared row decoder unit 16 which receives inputs including row predecoded addresses XP1 . . . XPn, and block select inputs BLKSELs. This 32 Mb double unit organization has been incorporated into an existing design for a 256 Mb DRAM, the details of which are described in the Article by Y. Watanabe et al. entitled "A 286 mm2 256 Mb DRAM with x32 Both-Ends DQ," IEEE Journal of Solid-State Circuits, Vol. 31, No. 4, April, 1996 ("the Watanabe Article"). Within the shared row decoder unit 16 there are provided are plurality of row decoders 30, the structure of which is shown in FIG. 2.
As shown in FIG. 2, each row decoder 30 of shared row decoder unit 16 (FIG. 1) receives as inputs a plurality of row predecoded addresses, for example three predecoded addresses (XP1, XP2, XP3), and a block select signal BLKSEL. Upon receiving the correct combination of row predecoded addresses XPs to enable the row decoder 30 at a time when the BLKSEL signal is active, the row decoder 30 activates a row decoder output signal RDOUT which is provided to both a left WL driver 14 and a right WL driver 18 of the double unit 10. In this way, only one row decoder 30 is needed to enable the selection of blocks from both left and right units, 12, 20.
In operation, the BLKSEL signal is held active during a time in which both units 12, 20 are in an active state. During a reset phase, when the BLKSEL signal enters an inactive state again, RDOUT signals of row decoders 30 are precharged to HIGH, at which time units 12, 20 are simultaneously deactivated.
It will be understood that the row predecoded addresses XPs must hold the information constant for the duration in which BLKSEL is active. Otherwise, RDOUT might be falsely enabled by the XPs transition between states because the XPs provide the enabling and trigger conditions for RDOUT.
Because the row decoder 30 requires the XPs to hold the information constant during BLKSEL active cycles, it is not possible to use row decoder unit 30 in a double unit 10 in which it is desired to utilize each unit 12, 20 as a separate bank under separate row addressing control. That is, row decoder 30 cannot be used in a double unit 10 which is configured to operate as two or more banks.
FIG. 3 shows a schematic for the design of another existing row decoder unit 40 which permits a pair of left and right units 12, 20 to be configured as a pair of banks, rather than just a single bank, as is the conventional configuration. Row decoder unit 40 includes sets of row decoder circuits 42 -- for each of the left unit 12 and the right unit 20 which are completely independent from each other, i.e. the decoder circuits 42 in each set include independent devices which receive and act upon the row predecoded addresses and block select signals to activate wordlines within the respective left and right units, 12, 20. Consequently, left and right units 12, 20 can each be independently controlled, to access storage locations at different row addresses at the same time.
However, row decoder unit 40, which duplicates the input and output circuits for all predecoded address and block select inputs, requires twice the number of row predecoded address signal lines and row decoder circuits 42 as row decoder unit 16. In consequence, the area occupied by row decoder unit 40 on an IC is substantially greater than the area occupied by row decoder unit 16. It would be advantageous to provide a row decoder unit which permits a double unit to be configured with multiple banks, without requiring row decoder circuits therein to be duplicated.
Accordingly, it is an object of the invention to provide a row decoder circuit of a row decoder unit which permits a plurality of banks to be configured within a pair of memory units, i.e. a pair of physically contiguous memory arrays served by the row decoder unit, while reducing the amount of area occupied by the row decoder unit.
It is another object of the invention to provide a row decoder unit which reduces the consumption of current while permitting a double unit to be configured as multiple banks.
II. Block Address Assignment within Banks
In an existing RAM (as shown, for example, in FIG. 1), blocks are arranged in the same way within left and right units 12, 20, namely, numbered in sequential order from bottom to top (or from top to bottom). As such, blocks which are accessed by the same address inputs are located across from each other at the same distance away from the ends 22 of the units 12, 20. That is, block 0 in the left unit 12 is located across from block 0 in the right unit 20 and lies at the end 22 of the left unit 12, as does block 0 in the right unit 20. In the same way, block 1 in the left unit is located across from block 1 in the right unit 20 and lies one block away from the end 22 of the left unit 12, as does block 1 in the right unit 20.
However, the inventors have found that addressing blocks within the left and right units 12, 20 in such symmetrical fashion is undesirable. Within a unit 12, one or more wordlines in a block are activated at a time by signals supplied to the row decoder from one end 22 of the unit 12. As described above with reference to FIG. 3, units 12, 20 can be accessed independently in an ACTIVE mode when double unit 10 is configured as multiple banks, each bank having independent row decoder circuits 42. However, when double unit 10 is configured as a single bank, units 12, 20 are not independently controlled, such that the row decoder unit 16 accesses the same physical block numbers across both units 12, 20. Even when the double unit 10 is configured as multiple banks, when the double unit 10 is operated in known Column-Address-Strobe (CAS) Before Row-Address-Strobe (RAS) Refresh mode (CBR mode), locations will be accessed within each unit 12, 20 with signals selecting the same block numbers in both units 12, 20.
Thus, in CBR mode, whether in a single bank unit or in a double unit having a multiple bank configuration, wordlines in the same numbered blocks in both left and right units 12, 20 are alternately or simultaneously accessed, first from one unit, for example, the left unit 12, then from the other unit, i.e. the right unit 20 in this example.
When high numbered blocks are accessed, e.g block 15 in the left and right units 12, 20, the greater length of signal travel (and consequent voltage drop) from the end 22 of the units 12, 20 to such blocks requires more current to be supplied than that required to access low-numbered blocks located closer to the end 22 of the left and right units 12, 20, i.e. block 0 in each unit. Thus, in the existing arrangement of blocks, the current consumption within a double unit 10 varies with the address of the block selected for access. Likewise, the average voltage drop on row selection signal lines to both units 12, 20 (e.g. row predecoded addresses and block select signals) varies with the address of the block selected for access. In addition, heating effects due to the consumption of current vary with both time and with the location of a block within a bank.
Accordingly, an object of the invention is to provide an arrangement of blocks within a double unit which reduces or eliminates the dependence of the current consumption, heating effects and average voltage drop upon the address of the block which is accessed.
III. Column Address Increment Design
The need to increase density while decreasing the power consumption of RAMs for applications such as laptop computers imposes limitations upon the speed at which cells within a RAM can be accessed. However, these on-chip considerations must not be allowed to unduly limit the speed of off-RAM access, since otherwise, the off-RAM access speed could become a bottleneck in the performance of the computing system which utilizes the RAM.
One known way of increasing the off-RAM access speed in synchronous dynamic RAMs (DRAMs) is to perform a modified column burst mode operation in which sequentially adjacent addresses are accessed simultaneously from an "odd" column division (left unit) and an "even" column division (right unit) of a bank, rather than merely providing addresses to the left unit and to the right unit in sequence, as described above with reference to FIG. 1. To perform such operation, the lowest order bits of the column address are transferred to one of the odd/even units after being incremented by one, and transferred directly without being incremented to the other one of the odd/even units. Such operation is referred to a "column address increment". An example of a circuit design which performs such operations is described in an article by Yukinori Kodama et al. entitled "A 150 MHz 4-Bank 64 Mbit SDRAM with Address Incrementing Pipeline Scheme," 1994 Symposium on VLSI Circuits Digest of Technical Papers, pp. 81-82 ("the Kodama Article").
The Kodama Article describes a design for a DRAM which performs column address increment to transfer data to and from a storage locations within a bank at twice the access speed of the storage cells within. In that design, each bank is configured as a double memory unit (e.g. as in FIG. 1; 10) having left and right units 12, 20 separated from each other by row decoder circuitry for the bank. Left and right units 12, 20 form odd and even units of the bank which are accessed with consecutive column addresses that are provided simultaneously to both odd and even units. The row decoder circuitry between left and right units 12, 20 decodes a set of row selection signals and activates, at the same time, wordlines in both left and right units 12, 20 in accordance with to the decoding result. A similar concept is discussed in U.S. Pat. No. 5,386,385 to Stephens, Jr.
The Kodama Article, and the Stephens, Jr. Patent describe systems which implement column address increment pipelining, but only in a double unit 10 which is configured as a single bank, i.e. with a left unit 12 implementing an "odd" unit, and a right unit 20 implementing an "even" unit. The Kodama Article and the Stephens, Jr. Patent do not describe a way in which column address increment could be implemented in a double unit 10 which is configured as multiple banks. A way of providing column address increment pipelining in a double unit 10 having any number of banks therein would be desirable.
Accordingly, it is an object of the invention to provide a structure and method of providing column address increment pipelining in a double unit 10 in which more than one odd unit and one even unit are configured within the same unit (e.g. unit 12, or unit 20) and in which wordlines are supported by the same set of row decoders and wordline driver circuitry.
Another object of the invention is to provide a structure and method of providing column address increment operation simultaneously in each bank of a plurality of banks configured within a double unit 10.
IV. Read Write Drive Design
Towards the goal of increasing the speed of memory access while holding the line on or reducing the power consumption, it is important to transmit large current bearing signals within the RAM as efficiently as possible. Therefore, designs which reduce: 1) the amount of current needed to drive large current signals; 2) the number of signals being driven; or 3) the frequency at which large current signals switch between low and high levels, are desirable to reduce the power consumption while increasing the access speed of the RAM.
In an existing RAM described in the Watanabe Article referred to above, and as shown in detail in FIG. 4a, data is transferred to and from a DRAM storage array 400 by a circuit arrangement and signal flow known as "master DQ" (MDQ) architecture. The detailed schematic of storage array 400 in FIG. 4a corresponds to the internal organization of unit 12 or 20 of FIG. 1. Within the storage array 400, as provided by the MDQ architecture, data is passed from bitline pairs within the storage array 400 by a hierarchical arrangement of local DQ lines (LDQs) and master DQ lines (MDQs). A data input output circuit (DIO) 490 is coupled to the storage array 400 by a second sense amplifier unit (SSA) 450. SSA 450 receives data signals on master bitline pairs (MDQs) of the storage array 400, regenerates the data and transmits it again onto bidirectional read write drive lines (RWD, RWD') 480 to the DIO 490.
When accessing the storage array 400 during column burst mode operation in which several adjacent column storage locations are accessed sequentially, the amount of current required to perform such operation is known as the column burst current. The largest single contributor to the column burst current is the current needed to drive the RWD and RWD' lines 480 in transmitting data between the second sense amplifier (SSA) 450 and the data input/output circuit (DIO) 490.
With reference to FIG. 4b, signal levels on either line RWD, or line RWD' 480 are driven, in every clock cycle of the DIO 490, between an (inactive) precharge voltage level and an (active) data level. Regardless of the data pattern, large current is required to drive the rapid swing between the precharge voltage level and the active data level in the presence of large capacitive loads 460, 461.
It would be desirable to have a circuit and method of signal transmission which reduces the amount of current needed to drive signals between the second sense amplifier 450 and the data input/output circuit 490. Reducing the number of signal lines RWD, RWD' for each data bit from two to one, and eliminating the precharge cycle on the RWD signal line would greatly reduce the amount of current required to drive a high capacitive load 460 coupled to the signal line.
Accordingly, it is an object of the invention to provide a second sense amplifier circuit and signal arrangement by which data is transmitted from a second sense amplifier to a data input/output circuit with less current than with existing second sense amplifier designs.
It is another object of the invention to provide a second sense amplifier circuit which outputs data onto a single read write drive signal, in place of two read write drive signals.
It is a further object of the invention to provide a circuit and method of signal transmission which reduces the rate at which voltage levels of the read write drive signal are switched.
Still another object of the invention is to provide a circuit and method of signal transmission by which data bits are transmitted sequentially on a read write drive signal without requiring the signal line to be precharged between each data bit.
SUMMARY OF THE INVENTION
These and other objects are provided by the intra-unit block addressing system of the present invention. Accordingly, the present invention stabilizes the current dissipation, voltage drop, and heating effects related to accessing blocks within first and second storage units of a double memory unit. The system includes a row selection unit located between the first and second storage units, which accesses storage locations of the first and second storage units according to first and second selection signals conducted from the outer extremities of the double memory unit to selected row locations. The blocks at corresponding distances from the outer extremities are numbered differently such that the sum of lengths of signal travel of the first and second selection signals to the numbered blocks remains relatively constant regardless of the block number which is selected for access.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block and schematic diagram showing the structure of a conventional double memory unit of a random access memory (RAM).
FIG. 2 is a block and schematic diagram showing a prior art row decoder 30 unit for a double memory unit.
FIG. 3 is a block and schematic diagram showing a prior art row decoder unit 40 for independent accessing of left and right units of a double memory unit.
FIG. 4a is a block and schematic diagram showing the structure and operation of access circuitry within a prior art dynamic RAM.
FIG. 4b is a timing diagram illustrating the signal swing of signals RWD, RWD' of a read write drive.
FIG. 5 is a block and schematic diagram showing the structure and operation of the shared row decoder 110 of the present invention.
FIG. 6 is a timing diagram for the shared row decoder 110 of FIG. 5.
FIG. 7 is a block diagram showing the structure and operation of a first embodiment of the block address assignment aspect of present invention.
FIG. 8 is a block diagram showing the structure and operation of a second embodiment of the block address assignment aspect of present invention.
FIG. 9 is a block and schematic diagram showing the structure and operation of the column address increment pipelining aspect of present invention.
FIG. 10 is a block and schematic diagram showing the structure and operation of a read write drive signal generator which includes two second sense amplifiers.
FIG. 11 is a block and schematic diagram showing the structure and operation of the single ended read write drive of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
I. Shared Row Decoder
FIG. 5 is a schematic circuit diagram of a shared row decoder 110 of the present invention. Row address input circuit 111 receives row predecoded address input signals, for example XP1, XP2, XP3, and provides an enabled/disabled input at terminal 113 which is determined by the states of the row predecoded address inputs. Separate left block select (BLKSELl) and right block select (BLKSELr) signals are provided to left and right decoder latch circuits 121 and 123, respectively. The block select signals BLKSELl and BLKSELr are held active during an active cycle of a bank in which the left and the right blocks are located. In addition, a pulsed left Row-DECoder-ON (RDECONl) signal, and a pulsed Right Row-DECoder-ON (RDECONr) signal are provided to left and right decoder latch circuits 121, 123, respectively. These pulsed RDECONl and RDECONr signals allow for the activation of units 12, 20 within double unit 10 at different selected times, without requiring separate row decoder circuits 42, as described above with reference to FIG. 3.
By operation of the shared row decoder 110 of the invention, an enabling input 113 is latched into one of the left or the right latch circuits 121, 123 when the values of the predecoded address inputs XP1, 2, and 3 are in the right combination for the particular decoder, and the RDECONl signal or the RDECONr signal becomes active, respectively. (See timing diagram, FIG. 6). Importantly, RDECONl and RDECONr are pulsed at different times so that the values of the predecoded address inputs at XP1, 2 and 3 will be allowed to change from the time the left unit 12 is accessed until the right unit 20 is accessed.
Note that with the pulsed timed control over the latch circuits 121 and 123, the predecoded address inputs are not required to swing once during every RAS cycle. Rather, predecoded address inputs XP1, XP2, XP3, etc. are permitted to maintain the same states from one cycle to the next, and change state only when the information content of the address signals changes. This results in a reduction of the current required to operate shared row decoder 110, in relation to the row decoder 30 described above with reference to FIG. 2. In addition, the pulsed timed control over the latch circuits 121, 123 permits the implementation of a shared row decoder 110 in which the address input circuit 111 and signal lines which carry row predecoded address signals XP1, XP2, XP3, etc. thereto are shared between left and right units 12, 20 (FIG. 1) , resulting in a net savings of area occupied by the row decoder circuitry for a double unit 10 of an IC.
II. Asymmetric Assignment of Block Addresses
A second aspect of the invention is the asymmetric assignment of block addresses within left and right units of a unit or bank. This aspect of the invention can be utilized either together with or separately from the shared row decoder aspect or other aspects of the invention.
With reference to FIGS. 1, in banks of existing RAMs, blocks having the same number, i.e. the same block address, are located at the same position within the left and right units of a unit or bank. For example, block 0 in the left unit is located on the bottom left, and block 0 in the right unit is located on the bottom right.
In this aspect of the invention, addresses are assigned to blocks in left and right units of each bank such that the same numbered blocks of the left and right units are not located adjacent to each other. In a first embodiment of this aspect of the invention, as shown in FIG. 7, the blocks can be arranged such that the bottommost block in the left unit is addressed as block 0 while the bottommost block in the right unit is addressed as block 15. Then, the next block up from the bottom in the left unit is addressed as block 1, while the next block up from the bottom in the right unit is addressed as block 14.
By assigning addresses to blocks in this manner, the uneven current dissipation, heating, and changing signal voltage drop effects described above are greatly reduced or eliminated. This is so because when accessing block 0 in both units, the path of the current bearing signals to block 0 in the left unit is relatively short, while the path of the current bearing signals to block 0 in the right unit is relatively long, with the result that the current dissipated by the path of the signals to blocks 0 in both units averages out. In this manner, the current consumed while accessing sequentially numbered locations alternately from the left and the right units, as is commonly performed in column burst mode operation, will remain at a nearly constant average level, regardless of the block address from which the data is accessed. Moreover, the uneven heating and voltage drop effects are reduced because signal currents extend to physically different locations in the left and the right units and the signal voltage drop is subject to an averaging effect from the end 22 of the double unit into the selected blocks.
A second embodiment of this aspect of the invention is described with reference to FIG. 8. As shown therein, a double memory unit 210 of 32 Mb capacity is arranged with a left 16 Mb unit 220 including 1 Mb physical blocks 0 to 15 (numbers correlating with physical locations), and a right 16 Mb unit 222 including 1 Mb physical blocks 0 to 15. Lower row domains 226 include blocks 0 to 7, while upper row domains 228 include blocks 8 to 15.
Between the left and right units, 220, 222 is a row decoder and driver unit 224, which is arranged to activate wordlines in particular blocks of each unit 220, 222, in accordance with three row address bits AR11, AR10, AR9, with AR11 being the most significant bit.
In the case of the left 16 Mb unit 220, row decoders are arranged such that the blocks selected by row address bits AR11, AR10, AR9 correspond directly to the physical block numbers. For example, in the left unit 220, for row address values on AR11, AR10, AR9 of (1,1,1), block 7 is activated.
In the case of the right 16 Mb unit 222, row decoders are arranged differently such that blocks selected by the row address bits AR11, AR10, AR9 lie at different locations than the physical block numbers which correspond to the combination of row address bits. For example, in FIG. 8, row address input on AR11, AR10, AR9 of (1,1,1) selects block 3 in the right unit 223 rather than block 7 as in the left unit 220.
Blocks in the upper row domains 228 are selected such that the physical block number selected for access equals the physical block number of the selected block in the lower domain 226 plus 8. For example, in the left unit 220, the selected blocks are block 7 and block 15, while in the right unit 22, the selected blocks are block 3 and block 11.
In addition, the combination of this important aspect of the invention with the shared row decoder (FIG. 5) of the invention helps to ensure that adjacent blocks within a unit or bank are not activated simultaneously. In consequence, signals propagate at more uniform speed to and from locations within the left and right units of a unit or bank.
Intra-Unit Column Address Increment Pipelining
FIG. 9 is a block and schematic diagram showing the design for a 32 Mb double unit 308 of a 256 Mb DRAM. The goal of this design is to permit a single unit to operate as a bank, while implementing column address increment pipelining to boost memory access speed. The double unit 308 includes a pair left and right units 310, 311 of 16 Mb capacity. Left and right units 310, 311 are configured to operate as separate banks which share a row decoder unit 312 having shared row decoders therein such as those described above with reference to FIG. 5.
Each unit 310, 311 is divided into odd and even column domains; left unit 310 includes odd and even column domains 314 and 316; and right unit 311 includes even and odd column domains 318 and 320. Each column domain 314, 316 of a bank 310 is further divided into four 2 Mb double segments, each of which includes an upper 1 Mb segment and a lower 1 Mb segment. For example, within a double segment of the even domain 316, 1 of 64 column select lines (CSLs) is used to access four master DQ line pairs (MDQE 4-7) from the upper segment and four master DQ line pairs (MDQE 0-3) from the lower segment.
Units 310, 311 are divided row-wise into sixteen 1 Mb array blocks, (only two blocks 340a, 340b, shown for the purpose of simplicity), each block containing a storage array block having 512 rows, i.e. 512 wordlines (WLs). Sense amplifier (SA) units 342 are placed in pairs with each storage array block, one SA unit 342 above each storage array block 340a and one SA unit 342 below. Each SA unit 342 contains 1024 sense amplifiers which are active on alternate bitline pairs in interleaved fashion with respect to the other SA unit 342 of the pair to support the 2048 total bitline pairs of the storage array block 340a. In addition to the sixteen 1 Mb unit blocks 340a, 340b, etc., a redundancy array block of 160 Kb capacity which has 80 redundancy wordlines (RWLs) is provided within each unit 310, and 311. Redundancy logic 346 controls access to regions of redundancy array block 344.
Associated with each unit 310, 311 are column address circuitry as follows. Associated with the even column domain 316 is a plus-one adder 322a which receives the lowest order column address bits YADD0-2, and increments the bits by one. An even column domain counter (CTRE) 324a receives the incremented YADD0-2 and cyclically updates the value. Associated with the odd column domain 314 is an odd column domain counter (CTRO) 326a which receives the column address bits YADD0-2 directly from address bus 330 and cyclically updates that value. Column predecoder (CPD) 348 predecodes other column address bits. Coupled to the outputs of CPD 348, CTRE 324a and CTRO 326a are column decoder/second sense amplifier (CDEC/SSA) units 329a, 328a, respectively, which perform the final decoding operations to activate selected column select lines CSLO and CSLE in the odd and even column domains 314, 316, respectively.
Column address increment pipelining performed by the invention within a unit will now be described. Within the left unit 310, for example, odd unit counter CTRO 326a receives the three lowest order address signals YADD0-2 from address bus 330 and transfers them to the CDEC/SSA 329a for the odd column domain 314. No incrementing of address signals provided to odd column domain 314 is required.
For the even column domain 316, a plus-one adder 322a receives the lowest order column address bits YADD0-2, increments the bits by one and outputs the result to an even unit counter (CTRE) 324a, which then passes the incremented address to CDEC/SSA 328a for the even column domain 316. Column predecoder (CPD) 348 decodes address bits YADD3-7, and provides predecoded signals for these higher order bits to both the odd and the even column domains 314, 316.
Simultaneous storage access to sixteen bits is provided as follows. A single wordline in each of two 1 Mb blocks 340a, 340b is activated in accordance with predecoded row addresses provided to shared row decoder 312. The lowest order column addresses YADD0-2 are incremented by plus-one adder 322a and output provided to CTRE 324a. The lowest order column addresses YADD0-2 are provided directly to CTRO without being incremented. In consequence, column select lines CSLO and CSLE are activated in odd and even column domains 314, 316, respectively, in accordance with the predecoded addresses provided by CPD 348 and the outputs of counters CTRO and CTRE.
In a read operation, with the activation of CSLO and CSLE four data bits are transferred from storage cells coupled to the activated wordline in block 340a onto four bitline pairs in the upper 1 Mb segment of the odd column domain 314, which data bits are then transferred onto master bitline pairs MDQO 4-7. Likewise, four data bits are transferred from storage cells coupled to the activated wordline in block 340a onto four bitline pairs in the upper 1 Mb segment of the even column domain 316, which data bits are then transferred onto master bitline pairs MDQE 4-7. In addition, four data bits are transferred from storage cells coupled to the activated wordline in block 340b onto four bitline pairs of the lower 1 Mb segment in the odd column domain MDQO 0-3, which data bits are then transferred onto master bitline pairs MDQO 0-3. Likewise, four data bits are transferred from storage cells coupled to the activated wordline in block 340b onto four bitline pairs of the lower 1 Mb segment in the even column domain MDQE 0-3, which data bits are then transferred onto master bitline pairs MDQE 0-3. The data bits on lines MDQE 0-7 are sensed and transmitted on even domain read write drive bus RWDE 0-7 to DIO 490 (FIG. 4) and the data bits on lines MDQO 0-7 are sensed and transmitted on odd domain read write drive bus RWDO 0-7 to DIO 490 (FIG. 4).
Thus, the circuitry and method of the present invention has been shown to provide column address increment pipelining within a single unit 310.
III. Single Ended Read Write Drive Conversion
FIG. 10 contains a block and schematic diagram showing the design for a second sense amplifier unit (SSA) 550. The second sense amplifier unit (SSA) 650 described below is a further improvement over SSA 550. However, the SSA unit 550 is not admitted by the Applicants to be prior art. The SSA 550 includes two current mirror sense amplifiers (CMPs) 500 and 501 and a precharge/equalization circuit 510 (shown exemplarily as including three PFETS, coupled to a constant voltage source V ARRAY , and to a time-varying precharge signal DQRST'). In addition, SSA 550 includes RWD switches 520 and 521 (shown exemplarily as NFETs), RWD precharge devices 530 and 531 (shown exemplarily as PFETs), and support devices 540-546.
When all column select lines CSLs are LOW (at a low voltage level), the signal DQRST is HIGH (at a high voltage level) and the signal DQRST', the inverted signal thereof from inverter 546, is LOW, which causes PFETs 544 and 545 to be ON (in the on state). In consequence, signal lines GL and GL' which are tied to source terminals of PFETs 544 and 545 are maintained HIGH. Nodes GD and GD' are then both LOW, since NFETs 540, 541 are ON, PFETs 542 and 543 are OFF, and NFETs 520 and 521 are OFF. Then the read write drive signal pair RWD and RWD' are precharged to a voltage level V DD by PFETs 530 and 531.
When a CSL is raised HIGH, a corresponding pair of bitlines BL and BL' are switched into electrical contact with an MDQ line pair, as described above. During this interval, DQRST is held high which precharges the MDQ line pair. When DQRST falls, the CMP pair 500, 501 becomes enabled and develops sensing results corresponding to the signal values on the MDQ line pair. At that time signals GL and GL' follow the sensing results developed by CMPs 500 and 501, which signals are then followed by signals GD and GD'.
Here, the operation of SSA 550 can be best explained with an example. When the value of the data being sensed from a bitline is `0`, as represented by a lower voltage level present on signal line MDQ than line MDQ', by operation of CMPs 501 and 500, GL falls LOW while GL' remains HIGH. The LOW going signal GL causes PFET 542 to turn on, forcing signal output RWD to LOW. Signal RWD', by contrast, remains HIGH, since NFET 521 remains in OFF condition. When signal DQRST rises HIGH again, signals GL and GL', GD and GD', RWD and RWD' are precharged to HIGH, LOW, and HIGH levels again, respectively.
This system, however, has the following disadvantages:
1. RWD and RWD' both drive large capacitive loads 560, 561, respectively. The capacitance is generally of the order of 5 pF. For DRAMs which have a x32 organization, as that term is used in the Watanabe Article referenced herein, a typical operational voltage swing of 2.5 V, and bit access speed of 200 MHz, the steady state current required to drive these loads is 80 mA.
2. The necessity of a precharge interval for restoring levels on signals RWD or RWD' between data intervals makes it more difficult to implement faster machine cycles in synchronous DRAMs, and increases the design complexity of DIO circuitry.
A further improved SSA circuit 650 is shown schematically in FIG. 11. Like the SSA circuit 550 shown in FIG. 10, SSA circuit 650 includes two CMPs 600, 601, a precharge/equalization circuit including three PFETs 610, and support devices 640 through 646, which are essentially the same as or identical to those shown in SSA circuit 550. However, SSA 650 replaces the NFETs 520, 521 used to drive the RWD, RWD' signals in SSA 550 (FIG. 10) with a unitary CMOS driver including NFET 620 and PFET 630 to provided single-ended RWD operation. PFETs 530, 531, used to precharge signals RWD, RWD' in SSA 550, have been eliminated from SSA 650.
The operation of SSA 650 will now be described, with reference to FIG. 11. When the CSL is not enabled, DQRST remains at a HIGH level which precharges the MDQ pair and maintains CMPs 600, 601 in disabled condition. When the CSL is activated, DQRST falls, ending the precharge operation and CMPs 600, 601 become enabled simultaneously. As a result, signals GL and GL' follow the sensing results of CMPs 600 and 601, which results are then followed again by signals GD, GD' and GD'.
Here, the operation of SSA 650 can best be explained with an example. When the value of the data being sensed on a bitline is `0`, as represented by a lower voltage level present on signal line MDQ than line MDQ', by operation of CMPs 600 and 601, GL falls LOW while GL' remains HIGH. The low-going GL signal turns on PFET 642, which in turn, causes signal GD' to go HIGH, while signals GD and GD' are maintained LOW and HIGH, respectively. In consequence, NFET 620 turns on, driving output RWD to LOW level and latching the data thereon with devices 652. Signal DQRST rises HIGH again soon; however, the data is latched onto RWD and cannot change until DQRST falls again. The switching of DQRST to the HIGH level again causes signals GL, GL', and GD, GD' and GD' to be precharged again to HIGH, and LOW levels, respectively.
It will be understood that the advantages of SSA circuit 650 of the present invention over SSA circuit 550 (FIG. 10) include the following:
1. The single-ended RWD signal drives a large capacitive load 660 of typically 5 pF, but the voltage level thereon swings only when the data in a given cycle changes from its state in the last previous cycle. In SSA circuit 550, at least one of signals RWD or RWD' had to be precharged in every cycle. Then, the voltage level had to swing on at least one of signals RWD or RWD' to indicate the data bit for that cycle, i.e. a `0` would appear in the current cycle on signal RWD', while a `1` would appear on signal RWD. Since the SSA circuit 650 eliminates the precharge interval entirely, at least one half of all voltage swings on the RWD line are eliminated.
Further, assuming that randomized data are stored and read out from the memory, the probability that the data changes in a given cycle is one half. With SSA circuit 550 (FIG. 10), a voltage swing on at least one of RWD and RWD' signals was required to indicate the presence of either a `0` or `1` in the data stream. SSA circuit 650 (FIG. 11) of the present invention, which transmits both `0` and `1` data on the same single-ended RWD line, does not require the voltage to swing from one cycle to the next if the next bit in the data stream is the same as the last. Therefore, the number of voltage swings for the RWD signal are reduced again by half in relation to the operation of the SSA circuit 550. Considered together, the operation of SSA circuit 650, under the same conditions as those described for SSA circuit 550, results in a reduction of current by 75% from 80 mA to 20 mA. Even assuming worse conditions in which the transferred data bits change levels once in every cycle, the amount of required current increases only by a factor of 2 to 40 mA.
2. The elimination of a precharge interval on the signal RWD permits faster machine cycles to be implemented in synchronous DRAMs, without increasing the design complexity of the DIO circuitry. With the SSA circuit 650, as shown in FIG. 11, data can be transferred from the RWD to the DIO at DIO input clock frequencies of at least 400 Mhz.
3. In addition, it will be understood that the invention reduces the number of RWD signal lines within the DRAM by one half. While the invention has been described in accordance with certain preferred embodiments thereof, those skilled in the art will recognize the many modifications and enhancements that can be made without departing from the true scope and spirit of the appended claims.
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A system is disclosed herein for stabilizing the current dissipation, voltage drop, and heating effects related to accessing blocks within first and second storage units of a double memory unit. The system includes a row selection unit located between the first and second storage units, which accesses storage locations of the first and second storage units according to first and second selection signals conducted from the outer extremities of the double memory unit to selected row locations. The blocks at corresponding distances from the outer extremities are numbered differently such that the sum of lengths of signal travel of the first and second selection signals to the numbered blocks remains relatively constant regardless of the block number which is selected for access.
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[0001] This application claims the benefit of Taiwan application Serial No. 095106664, filed Feb. 27, 2006, the subject matter of which is incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates in general to a supporting structure, and more particularly to a height-adjustable supporting structure applied in a display device.
[0004] 2. Description of the Related Art
[0005] Liquid crystal display (LCD) device, having the features of light weight, slimness, small size, low power consumption, low radiation and low pollution, has gradually replaced conventional cathode ray tube (CRT) display device and become a standard item of equipment to a new generation computer.
[0006] Normally, a liquid crystal display device at least includes a casing and a panel. A plurality of supporting structures are disposed on the casing to support the panel. However, different panels manufactured by different manufacturers have different measures of thickness. In order to correspond to the panels with different measures of thickness, different sets of charge cores are developed to match the supporting structures with different measures of height, not only increasing the production cost but also reducing the production efficiency.
SUMMARY OF THE INVENTION
[0007] The invention is directed to a height-adjustable supporting structure. The height-adjustable supporting structure, when disposed in a display device, is able to support various display panels with different measures of thickness. Consequently, there is no need to develop different sets of charge cores to correspond to the display panels with different measures of thickness, not only reducing the production cost but also increasing the production efficiency of the display device.
[0008] According to a first aspect of the present invention, a supporting structure applied in a display device is provided. The display device includes a casing and a display panel. The supporting structure includes a fastening component and a sustaining component. The fastening component including a hook set is used for supporting the display panel. The sustaining component having a plurality of slot sets is disposed on the casing.
[0009] According to a second aspect of the present invention, a display device including a display panel, a casing and a supporting structure is provided. The supporting structure includes a fastening component and a sustaining component. The fastening component having a hook set is for supporting the display panel. The sustaining component having a plurality of slot sets is disposed on the casing.
[0010] The invention will become apparent from the following detailed description of the preferred but non-limiting embodiments. The following description is made with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a perspective of a display device according to a first embodiment of the invention;
[0012] FIG. 2A is a perspective of a supporting structure with a first height according to the first embodiment of the invention;
[0013] FIG. 2B is a perspective of a supporting structure with a second height according to the first embodiment of the invention;
[0014] FIG. 3 is a perspective of a supporting structure being disposed on a casing according to the first embodiment of the invention; and
[0015] FIG. 4 is a perspective of a supporting structure being disposed on a casing according to a second embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
First Embodiment
[0016] Referring to FIG. 1 , a perspective of a display device according to a first embodiment of the invention is shown. Referring to both FIG. 2A and FIG. 2B . FIG. 2A is a perspective of a supporting structure with a first height according to the first embodiment of the invention. FIG. 2B is a perspective of a supporting structure with a second height according to the first embodiment of the invention. In FIG. 1 , the display device 100 includes a display panel 120 , a casing 130 and a supporting structure 200 . The supporting structure 200 used for supporting the display panel 120 is disposed on a bottom surface 132 of the casing 130 .
[0017] Referring to FIG. 2A , the supporting structure 200 includes a sustaining component 150 and a fastening component 101 . The sustaining component 150 at least includes two slot sets each including an upper slot and a lower slot. In the present embodiment of the invention, the sustaining component 150 includes a first slot set 1501 and a second slot set 1502 . The first slot set 1501 includes a first upper slot 1501 a and a first lower slot 1501 b , wherein the first upper slot 1501 a is slightly higher than the first lower slot 150 b . The second slot set 1502 includes a second upper slot 1502 a and a second lower slot 1502 b , wherein the second upper slot 1502 a is slightly higher than the second lower slot 1502 b . In addition, the sustaining component 150 further includs a fixing part 156 connected to one end of the sustaining component 150 , and the fixing part 156 has a top surface 157 and a bottom surface 159 , wherein the top surface 157 of the fixing part 156 is connected to the sustaining component 150 . Besides, the fixing part 156 includes at least two through slots 158 a and 158 b , which penetrate through the top surface 157 and the bottom surface 159 of the fixing part 156 .
[0018] The fastening component 101 includes a hook set 102 , a pressing part 104 , a column 106 and an elastic element 107 . A hook set 102 includes a first hook 102 a and a second hook 102 b . The second hook 102 b is slightly longer than the first hook 102 a , wherein the first hook 102 a and the second hook 102 b respectively have a first engaging surface 108 a and a second engaging surface 108 b . The pressing part 104 is connected to the hook set 102 . The hook set 102 is extended along a direction D. The column 106 is connected to the pressing part 104 and extended along the same direction D. Examples of the elastic element 107 is a spring which is fitted over the column 106 at the action of which the column 106 can move up and down. Preferably, one end of the spring is connected to the column 106 and the other end is supported by the top surface 157 of the fixing part 156 .
[0019] Referring to both FIG. 1 and FIGS. 2A˜2B . The fastening component 101 is used for supporting the display panel 120 . The sustaining component 150 is disposed on the bottom surface 132 of the casing 130 . When the display panel 120 and the casing 130 are divided by a first height H 1 , the hook set 102 pass through the first slot set 1501 , such that the supporting structure 200 has the first height H 1 . In other words, the first hook 102 a of the hook set 102 passes through the first upper slot 1501 a , and the second hook 102 b of the hook set 102 passes through the first lower slot 1501 b as indicated in FIG. 2A . Despite the present embodiment of the invention is exemplified by passing the hook set 102 through the first upper slot 1501 , however, in practical application, the present embodiment of the invention can also be achieved by pressing the first slot set 1501 against the hook set 102 to support the hooks 102 .
[0020] Meanwhile, the first engaging surface 108 a of the first hook 102 a is pressed against a lower edge of the first upper slot 1501 a to provide the fastening component 101 with an upward force to support the display panel 120 . As the elastic element 107 is compressed, the second engaging surface 108 b of the second hook 102 b is pressed against the upper edge of the first lower slot 1501 b to provide the fastening component 101 with a downward force to match the force produced by the compressed elastic element 107 . The upward force and downward force enable the supporting structure 200 to support the display panel 120 even firmly.
[0021] When the display panel 120 and the casing 130 are divided by a second height H 2 , the hook set 102 passes through the second slot set 1502 , such that the supporting structure 200 has a second height H 2 as indicated in FIG. 2B . Meanwhile, the first engaging surface 108 a of the first hook 102 a is pressed against the lower edge of the second upper slot 1502 a to provide the fastening component 101 with an upward force to support the display panel 120 . The second engaging surface 108 b of the second hook 102 b is pressed against the upper edge of the second lower slot 1502 b to provide the fastening component 101 with a downward force to match the force of the elastic element 107 . The upward force and the downward force enable the supporting structure 200 to support the display panel 120 even firmly.
[0022] As indicated in the above disclosure, the supporting structure 200 of the present embodiment of the invention is a height-adjustable supporting structure. The height-adjustable supporting structure, when disposed in a display device, is able to support various display panels with different measures of thickness. Consequently, there is no need to develop different sets of charge cores to correspond to the display panels with different measures of thickness, not only reducing the production cost but also increasing the production efficiency of the display device.
[0023] Referring to FIG. 3 , a perspective of a supporting structure being disposed on a casing according to the first embodiment of the invention is shown. In FIG. 3 , the casing 130 comprises at least two connecting columns 180 a and 180 b . The two connecting columns 180 a and 180 b are respectively melted to pass through the two through slots 158 a and 158 b , such that the bottom surface 159 of the fixing part 156 is connected to the casing 130 . The connecting columns 180 a and 180 b are preferably melted and infused into the through slots 158 a and 158 b . However, anyone who is skilled in the technology will understand that the way of connection exemplified here is not for limiting the scope of the technology of the invention.
[0024] To summarize, the supporting structure 200 of the present embodiment of the invention is a height-adjustable supporting structure, which, when disposed in a display device, is able to support various display panels with different measures of thickness. Consequently, there is no need to develop different sets of charge cores to correspond to the display panels with different measures of thickness, not only reducing the production cost but also increasing the production efficiency of the display device.
Second Embodiment
[0025] Referring to FIG. 4 , a perspective of a supporting structure being disposed on a casing according to a second embodiment of the invention is shown. The sustaining component 450 of the present embodiment of the invention differs with the sustaining component 150 of the first embodiment in the connecting mechanism between the sustaining component and the casing. As for other similar elements, the same reference numbers are used and are not repeated here. As indicated in FIG. 4 , the sustaining component 450 further includes at least a positioning part 400 and an anti-slip bump 460 . The positioning part 400 is disposed at the peripheral of the sustaining component 450 , and the anti-slip bump 460 is disposed on one side of the sustaining component 450 . The casing 130 includes an opening 462 and an anti-slip hole 464 . When the sustaining component 450 is placed into the opening 462 , the positioning part 400 is engaged with the opening 462 . The anti-slip bump 460 is received in the anti-slip hole 464 for preventing the sustaining component 450 from rotating with respect to the casing 130 .
[0026] There is an alternative connecting mechanism in addition to the connecting mechanism between the sustaining component and the casing as disclosed in the first embodiment and the present embodiment of the invention. The alternative mechanism is achieved by disposing a metal piece (not illustrated in the diagrams) between the casing 130 and the liquid crystal the display panel (as indicated in the display panel 120 of FIG. 1 ) and further disposing an opening and an anti-slip hole on the metal piece for receiving the sustaining component 450 . In other words, the positioning part 400 of the sustaining component 450 is engaged with the opening disposed on the metal piece. Meanwhile, the anti-slip bump 460 is received in the anti-slip hole disposed on the metal piece for preventing the sustaining component 450 from rotating with respect to the metal piece.
[0027] According to the supporting structure and display device using the same disclosed in the above embodiments of the invention, the supporting structure is a height-adjustable supporting structure. The height-adjustable supporting structure, when disposed in a display device, is able to support various display panels with different measures of thickness. Consequently, there is no need to develop different sets of charge cores to correspond to the display panels with different measures of thickness, not only reducing the production cost but also increasing the production efficiency of the display device.
[0028] While the invention has been described by way of example and in terms of a preferred embodiment, it is to be understood that the invention is not limited thereto. On the contrary, it is intended to cover various modifications and similar arrangements and procedures, and the scope of the appended claims therefore should be accorded the broadest interpretation so as to encompass all such modifications and similar arrangements and procedures.
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A supporting structure applied in a display device is provided. The display device includes a casing and a display panel. The supporting structure comprises a fastening component and a sustaining component. The fastening component including a hook set is used for supporting the display panel. The sustaining component having a plurality of slot sets is disposed on the casing. The hook set separately presses against the slots for forming different distances between the display panel and the casing.
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This application claims priority under 35 U.S.C. §119 based on provisional application Ser. No. 60/074,544, filed Feb. 12, 1998 and provisional application Ser. No. 60/056,836, filed Aug. 22, 1997, which are both hereby incorporated by reference herein in their entireties.
BACKGROUND OF THE INVENTION
The present invention pertains to instruments and methods for use in delivery of compositions, such as therapeutic fluids, through a tissue while minimizing exposure of the tissue to the compositions. More particularly, the invention pertains to treatment of a targeted tissue within an area of healthy tissue, and more particularly, to a multi-body apparatus and method capable of delivering compositions to a target tissue mass, such as, for example, a tumor, in the otherwise healthy tissue of a body organ, with minimum loss or exposure of the composition to the healthy tissue. The invention is particularly directed to multi-body apparatus capable of delivering compositions to a target tissue, such as brain tumor, while minimizing or preventing the exposure of healthy brain tissue to compositions that could potentially harm the healthy tissue.
DESCRIPTION OF THE PRIOR ART
In a method of treating a target tissue, such as, for example, a tumor, located within an otherwise healthy body organ, a composition in the form of a chemical, a therapeutic fluid, a dye, a contrast agent, a drug or a “cocktail” of chemicals, compositions and/or drugs, is delivered directly to the target tissue by injection.
Although this method is well suited for injection of fluid compositions, it will be understood by those skilled in the art that other compositions, such as, for example, viscous compounds, semi-fluids, or solids in granular or powdered form may also be injectable. Furthermore, the compositions may be injected in a liquid state and, after injection, solidify under the influence of body heat or by the application of an external energy source, such as, for example, microwave, radio frequency or electromagnetic energy. Alternatively, a solid or semisolid composition may be injected, and, after injection, liquify under the influence of body heat or an external energy source.
In this treatment method, after the location of the target tissue in an organ has been determined by MRI or other mapping or imaging method, a treatment apparatus having, for example, a needle or cannula capable of transporting a composition preferably in a fluid or semi-fluid state and having an opening at or near the tip for delivering fluid, is passed through healthy organ tissue until the tip opening is located within the tissue targeted for treatment, e.g. a tumor. A composition for treating the target tissue is transported from a reservoir at a proximal end of the treatment apparatus, through a needle shaft, and out through an opening at the distal tip of the needle. The fluid is delivered directly into the target tissue. This method has the advantage of localizing the treatment by specifically targeting tissue mass to be treated and is extremely successful in delivering the majority of the transported composition to the targeted tissue. The injection method is far less invasive than more radical treatments, such as, for example, surgery to remove tumor tissue, which can damage large amounts of healthy tissue. It also has advantages over traditional chemotherapy and radiology, which expose significant amounts of healthy tissue to side effects and possible damage.
This method of delivering a composition to a targeted tissue mass is particularly effective in treating brain tumors, since brain tissue is especially sensitive and susceptible to damage. For this reason, in the case of brain tissue treatment, needles are used which have a closed, rounded tip to minimize damage to healthy tissue and to prevent tissue from “packing” in the needle end. It will be understood by those skilled in the art that a variety of tips are also suitable, such as, for example, open tips, or pointed needle tips which are not “cutting” tips, etc. In addition to the particularly sensitive nature of brain tissue, certain types of brain tumors are known to have a high incidence of regrowth or recurrence. Patients with regrowing or recurring brain tumors may require multiple therapeutic treatments in the same location in the brain and, it is therefore desirable to keep to a minimum cumulative damage by multiple treatments. Thus, therapies for brain treatments in general need to be minimally damaging to healthy brain tissue.
Although the method of directly injecting fluids has been shown to be effective in specifically targeting and treating tissues, particularly in the brain, certain drawbacks are known. Compositions that are best suited to destroy tumor tissue are also known to negatively effect and possibly damage healthy tissue. And, although the method delivers the majority of the composition to the targeted tissue, some fluid may escape the shaft opening near the tip prematurely as it is being transported through healthy tissue to be located in the targeted tissue mass. Also, if the composition is injected under pressure into the target tissue, the fluid may not be absorbed quickly enough by the target tissue. If the fluid is not absorbed in the target tissue as quickly as it is injected, the fluid will seek a path of least resistance to escape the area of injection. The fluid may flow back along a track in the tissue. The track may be a pre-existing track in the tissue made by, for example, a diagnostic or other surgical instrument, or the track may be made by the treatment apparatus passing through the tissue. Alternatively, the track may be a naturally occurring lumen in the tissue, such as, for example, a vascular lumen, or may comprise an element of a guiding or positioning apparatus or device through which the treatment apparatus passes to reach the target tissue. The tendency for compositions to flow back along a track in the tissue, either while the treatment apparatus is in place or after the apparatus is withdrawn, will hereinafter be designated as “flow-back” or, alternatively, “retro-grade flow”. In the case of either premature escape of fluid or flow-back of fluid, the effects are the same: healthy tissue is exposed to composition and may be damaged, and doses of composition intended for treating the target tissue may fail to be absorbed by or delivered to the target tissue. The problems of premature escape and flow-back are amplified by the fact that some of the most desirable compositions are low viscosity liquids with low surface tension characteristics. Due to their low viscosity, these fluids are highly likely to leak from the apparatus prematurely and/or flow back along the track to effect healthy tissue.
In view of the above-identified advantages and disadvantages, the present invention is directed to an apparatus and injection method for minimizing the adverse effects of compositions on healthy tissue in the tracks of surgical devices by minimizing or preventing premature escape and migration or flow-back of compositions during treatment
OBJECTS OF THE INVENTION
It is an object of the invention to provide a device and a method for treating target tissues, particularly brain tumors, by injecting a composition into the target tissue.
It is another object of the invention to provide a device and method for treating target tissues by injecting a composition while minimizing damage to healthy tissue caused by exposure to the composition.
It is another object of the invention to provide a multiple shaft apparatus capable of delivering composition to a target tissue without prematurely leaking the fluid onto the tissue of a patient or other person.
It is another object of the invention to provide a multiple shaft device with means capable of preventing premature escape of a composition.
It is another object of the invention to provide an injection device with a means to prevent flow-back of composition along an apparatus track.
It is another object of the invention to prevent flow-back of a composition so that the composition is more effectively delivered to the targeted tissue.
It is another object of the invention to prevent composition delivered to a target tissue from flowing back into the apparatus by providing a means of sealing the composition out of the apparatus to ensure full delivery to the target tissue.
The present invention is generally characterized in an apparatus with a body having multiple hollow coaxial shafts arranged to control the flow of compositions to a target. An inner shaft delivers a composition through a lumen extending from a reservoir at a proximal end of the inner shaft to an outwardly directed inner shaft opening near the distal end, or tip, of the inner shaft. A central shaft supports a flow control means in the form of a sleeve which is repositionable to selectively open and close the inner shaft opening. An outer shaft has an elastic portion on the distal end which can be temporarily radially expanded to form a dam to prevent fluid flow-back along the apparatus track.
These and further objects and advantages of the invention will become apparent from the following description of the preferred embodiment taken in conjunction with the accompanying drawings wherein identical reference numbers indicate identical parts or parts providing identical functions.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of an apparatus according to the present invention with the valve closing the tip opening and the flow-back dam in an unexpanded state.
FIG. 2 is an exploded view of the apparatus according to the present invention showing the three shafts that make up the body of the apparatus.
FIG. 3 is a side elevation view of the apparatus of the present invention with the valve at the apparatus tip closed and the flow-back dam retracted.
FIG. 4 is a cross-section view take along sectional line 4 — 4 in FIG. 3 .
FIG. 5 is a cross-sectional view of the distal tip of the apparatus taken along sectional line 5 — 5 in FIG. 1 .
FIG. 6 is a partial cross-sectional view of the control means of the apparatus of the present invention in a first position.
FIG. 7 is a partial cross-sectional view of the control means of the apparatus in a second position.
FIG. 8 is a side elevation view of the apparatus in use in a fluid supply mode.
FIG. 9 is a cross-sectional view the expanded dam.
FIG. 10 is a view of the apparatus as used in conjunction with a stereotactic frame.
FIG. 11 is an enlarged view of the tip of the apparatus in a target tissue.
FIG. 12 is a schematic diagram of another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to FIG. 1, an apparatus 10 is shown having a midsection 11 separating opposite proximal and distal ends 12 , 14 respectively, and having a longitudinal axis along the length of the body from the proximal to the distal end. The body 10 has a control means 16 at the proximal end 12 . The distal end 14 of the apparatus 10 may be steerable by conventional means, such as, for example, by providing a tip having a predetermined curved shape, or by providing a tip having a memory metal, such as nitinol. The preferred embodiment shown is intended for treatment of brain tumors, however, the inventor conteare addressed below.
The body 10 is comprised of three hollow shafts, as shown in FIG. 2, an inner shaft 28 , an central shaft 36 and outer shaft 40 , coaxially arranged along the longitudinal axis of the body 10 with each individual shaft having a tubular midsection and having proximal and distal ends substantially corresponding to the tubular midsection 11 and proximal and distal ends 12 , 14 , respectively, of body 10 . The hollow shafts are preferably fabricated by known techniques from a surgical quality material, such as, for example, type 304 stainless steel with a full hard temper. The use of other materials to fabricate the shafts is also contemplated. For example, other surgical grade metals may be used, or polymer materials suitable for surgical applications may be used to fabricate the hollow shafts. Type 304 stainless steel is preferred as it is a well known material for similar applications, and is readily available for fabrication in the forms required. Type 304 stainless steel has the required strength, toughness and elasticity modulus to allow it to function properly with stereotactic frames such as those used in practicing the present invention. And type 304 stainless steel is known to be compatible with at least some of the compositions intended for use in this invention.
The outside diameters of the body could range in size, for example, from 10 mm for use in laparoscopy, to 0.2 mm for micro-procedures. The length, depending on the location of the target tissue from the body surface, could be in the range, for example, of from 50 cm for laparoscopy to 2 cm for other procedures. In the nominal preferred embodiment, i.e. the apparatus for treating brain tissue, outside diameter for each shaft is: an inner shaft 28 having a diameter of 1.07 mm, a central shaft 36 having a diameter of 1.47 mm, and an outer shaft having a diameter of 1.83 mm. The suggested length of the preferred embodiment will be approximately 30 cm.
The inner shaft 28 has a central, longitudinally oriented lumen 30 , shown in FIGS. 4 and 5, which opens to a terminal fixture 49 , shown in FIGS. 1-3, at the proximal end of the inner shaft 28 . The terminal fixture 49 supports a connector means 47 , such as, for example, a Luer connector, for attaching a fluid reservoir 32 (FIG. 8 ). The inner shaft lumen 30 opens at the distal end 14 of the body 10 to a tip opening 22 proximal to a tip 20 of the shaft. In a fluid supply mode, the lumen 30 serves as a conduit for compositions from tip opening 22 to the reservoir 32 . For the purposes of this supply operation, the tip 20 and shaft tip opening 22 are temporarily immersed in an external fluid supply source such as, for example, bottle 45 (FIG. 8 ). Negative pressure is provided in reservoir 32 causing the composition to travel from the external fluid supply 45 through the tip opening 22 , up through the conduit and into the reservoir 32 . In a fluid delivery mode, the process is reversed, and lumen 30 serves as a conduit to transport compositions from the reservoir 32 , which is provided with positive pressure during in the delivery mode, to the tip opening 22 at the distal end 14 of the body 10 for delivery through the tip opening 22 to the targeted tissue. Positive or negative pressure may be selectively provided to the reservoir 32 by a barrel and plunger (not shown) of conventional design, such as, for example, those found in a conventional syringe device, or by other known means for fluid delivery, in communication with the composition reservoir 32 .
The preferred embodiment of the present invention is intended for treatment of tissue located in brain tissue. In treatments involving insertions through brain tissue, the tip 20 is preferably closed and blunt or rounded, to prevent excessive damage to the tissue and to prevent the brain tissue from blocking or plugging the tip opening 22 as it is being inserted. Alternatively, a pointed, “non-cutting” type tip may be used. In the preferred configuration, multiple tip openings 22 are located proximal to the tip 20 on a sidewall of the inner shaft 28 , so that each opening 22 is oriented in a radially outwardly facing direction relative to the longitudinal axis of the body. Although the preferred embodiment is for treatment of brain tissue, and has a tip arrangement with a blunt, closed tip and a side oriented tip opening, the inventor contemplates the use of this invention for delivering compositions to target tissue in other organs, such as, for example, the liver. Thus, tip configurations suitable for a variety of tissue conditions and medical procedures are contemplated, including, for example, a conventional open pointed “cutting” tip suitable for treatment of other organs.
The inner shaft 28 is slidably supported in a complimentarily sized lumen 37 centrally located along the longitudinal axis extending from the proximal to the distal end of central shaft 36 . Preferably, the outer dimension of the inner shaft 28 and the inner dimension of the lumen 37 of the central shaft 36 are sufficiently close to inhibit leakage of fluids between the shafts, while permitting the inner shaft to slide freely with respect to the central shaft. Alternatively, a seal or seals, such as, for example, an O-ring, a gasket, or a sealing material or compound may be provided to inhibit fluid leakage between the inner shaft and the central shaft. Similarly, a seal or seals are provided where necessary to other elements of the apparatus to prevent undesired flow of liquids between elements.
The inner shaft 28 has a length longer than central shaft 36 so that the proximal and distal ends of the inner shaft 28 can extend beyond the corresponding proximal and distal ends of central shaft 36 by a prescribed distance. The central shaft 36 is selectively repositionable to a limited degree relative to the inner shaft 28 , thus the distance of extension of the inner shaft 28 with respect to the central shaft 36 can be manipulated. A push paddle 52 mounted on the proximal end of the central shaft 36 provides a means for manipulating the central shaft 36 with respect to the inner shaft 28 and the outer shaft 40 .
A valve means 38 in the form of a sleeve 39 is securely mounted on the extreme distal end of central shaft 36 as an extension of the tubular form of shaft 36 , so that the sleeve 39 is positioned coaxially about a portion of the distal end of the inner shaft 28 . The sleeve 39 has a proximal end 58 , a distal end 59 and a lumen 57 . For reasons discussed below, the proximal end 58 of the sleeve 39 is provided with an outer diameter larger than the diameter of the central shaft 36 to which it is secured, thus forming an annular shoulder 62 with a bearing surface 63 directed towards the proximal end 12 of the body 10 . Preferably, the outer diameter of the sleeve 39 is substantially similar to the outer diameter of the outer shaft 40 , so that the outer surface of the body 10 is provided with a substantially smooth, obstruction free finish to facilitate the passage of the body through tissue during insertion and withdrawal operations. Between the proximal end 58 and the distal end 59 , the outside diameter of the sleeve 39 is preferably reduced to provide a suitable taper from the full outside diameter of the outer shaft 40 to the outside diameter of the inner shaft 28 . Thus, the tapered distal end 59 of sleeve 39 forms a smooth transition between the inner shaft 28 and the outer shaft 40 to facilitate insertion of the body 10 through tissue.
The diameter of the lumen 57 of the sleeve 39 is preferably the same as or slightly smaller than the diameter of the lumen 37 of the central shaft 36 so that the sleeve closely fits the circumference of the inner shaft 28 to form a slidable sealing engagement with the outer surface of the inner shaft 28 . The sleeve 39 is selectively repositionable on the inner shaft 28 along the longitudinal axis of the body 10 by longitudinal movement of the central shaft 36 . By moving the sleeve 39 longitudinally to its most distal position, about the portion of inner shaft tip 20 having the tip opening 22 , the inner shaft tip opening 22 is sealed and compositions are prevented from leaking from the opening 22 . By withdrawing the sleeve 39 longitudinally to a position proximal of the portion of the tip 20 having the tip opening 22 , the tip opening 22 is exposed, and composition is permitted to pass freely through it.
Alternatively, the sleeve 39 can be provided with an aperture (not shown) which in a first radial position aligns with the tip opening 22 to permit fluids to pass, and which in a second position is radially offset from the tip opening 22 , thereby blocking the tip opening 22 to prevent fluids from passing. Thus, the valve means may be selectively manipulated by radial movement of the central shaft 36 with respect to the inner shaft 28 . In this embodiment, radial movement of the central shaft is selectively controlled by the push paddle 52 or some other suitable means.
Alternatively, the valve means 38 could comprise a valve, such as, for example, a one-way flapper valve (not shown) or elastic “aortic” type valve (not shown) at the tip 20 of the body 10 .
The sleeve 39 may be made from any material which is capable of providing: a slidable sealing relationship with the inner shaft 28 ; a bearing surface, such as, for example, surface 63 on the shoulder 62 , capable of supporting the forces necessary to expand dam 81 ; and, a secure attachment to the supporting central shaft 36 . Metal, such as, for example, stainless steel, or polymer materials, such as, for example, Delrin or Polypropylene are suitable materials which can be fabricated to provide the proper sealing relationship with the inner shaft 28 and which can form a bearing surface capable of supporting the forces necessary to expand dam 81 . The sleeve formed from such materials can be bonded or adhered to a stainless steel or polymer shaft body with a suitable adhesive, a suitable welding process, or another suitable mechanical fastening means, such as, for example, and annular ring or a swaged shaft end, etc. Polymer materials have the advantage of being capable of being formed in place, about the shaft body, by molding with suitable structural anchors, such as, for example, tabs, clearances, annular rings, swaging or grooves, provided on the shaft to secure the molded sleeve on the shaft. Polymer materials also have the advantage of providing, depending on formulation of the polymer, a better sealing capability and the flexibility to close the distal end of lumen 37 . Alternatively, if the shaft and seal are formed of the same material, they could be formed as one integral unit.
In the preferred embodiment, the sleeve 39 is fabricated from stainless steel. Stainless steel has the advantage of providing excellent fabrication qualities, structural integrity and, for the purpose of attachment to a supporting shaft, extremely secure mounting options, such as, for example, welding, swaging, threading or bonding to the body 10 . Preferably, the ability of a stainless steel sleeve 39 to form a tight seal may be enhanced by providing a gasket 55 (FIG. 5) between the inner surface of the sleeve 39 and the outer surface of the inner shaft 28 .
The sleeve 39 may have a uniform lumen diameter through the length of the sleeve. Providing the sleeve with a uniform lumen diameter would be required if the sleeve were fabricated from metal. However, a sleeve 39 fabricated from a polymer or other similar material could be provided with elastic qualities capable of conforming, at least at the distal end 59 , to the shape of the inner shaft 28 as it curves to a rounded tip 20 . Furthermore, enough elasticity could be provided to the distal end 59 of the sleeve 39 so that the distal end 59 would substantially close the sleeve lumen 37 completely, as shown in FIG. 1 . Such a closure would be necessary in the case of an apparatus having an open, cutting tip instead of the rounded tip 20 and side opening 22 of the preferred embodiment shown in FIGS. 1-6.
The outer shaft 40 has a lumen 41 extending from the proximal to the distal end and sized to support in slidable engagement the central shaft 36 . Preferably, the outer dimension of the central shaft 36 and the inner dimension of the lumen 41 of the outer shaft 40 are sufficiently close to inhibit leakage of fluids between the shafts, while permitting the central shaft to slide freely with respect to the outer shaft. Alternatively, a seal or seals, such as, for example, an O-ring, a gasket or a sealing material or compound, may be provided to inhibit fluid leakage between the central shaft and the outer shaft.
The outer shaft 40 may have calibration marks 42 on its outer surface suitable for use with gaging instruments such as, for example, a stereotactic or other type of locator frame for use with MRI or other imaging means. A radially expandable dam 81 comprised of an elastic portion 80 is provided on the distal end of the outer shaft 40 to selectively prevent fluid flow-back along the track. The dam 81 has proximal and distal ends, 82 and 83 respectively, and a lumen 85 substantially corresponding in diameter to the outer diameter of the central shaft 36 . The dam 81 is positioned coaxially about a portion of the distal end of the central shaft 36 , and may “free-float” in this position about the central shaft 36 while “captured” between a distally directed surface of the distal end of the outer shaft 40 and the proximally directed bearing surface 63 of the sleeve 39 . Alternatively, the proximal end 82 of the dam 81 may be fixedly mounted on the distal end of outer shaft 40 as an extension of the tubular form of shaft 40 while the distal end 83 of the dam 81 engages but is not fixedly attached to the bearing surface 63 of the sleeve 39 . Alternatively, the distal end 83 of the dam 81 may be fixedly mounted on the bearing surface 63 of the sleeve 39 , while the proximal end 82 of the dam 81 engages but is not fixedly attached to the distal end of the outer shaft 40 . Alternatively, the dam 81 may be fixedly mounted on both the proximal and distal ends, 82 and 83 respectively. The secure attachment may be made by any known means, including but not limited to the mounting methods mentioned above. In the preferred embodiment, the proximal end 82 of the dam 81 is fastened to the distal end of the outer shaft 40 by an annular steel band 91 or swaged outer shaft end 92 . Preferably, the distal end 83 of dam 81 engages but is not secured to bearing surface 63 of shoulder 62 on the sleeve 39 . An annular steel band 93 , secured to the outer surface of the proximal end of the sleeve 39 such that the proximal end of the steel band 93 extends proximally beyond the proximal end of the sleeve 39 , forms an annular groove 94 in which the distal end 83 of the dam 81 is seated. The steel band 93 is preferably not secured to the distal end 83 of the dam 81 . The annular groove 94 formed by the steel band 93 prevents the unsecured distal end 83 of the dam 81 from riding up over the proximal end of the sleeve 39 when, as explained in more detail below, the bearing surface 63 engages the distal end 83 of the dam 81 to expand the dam.
The dam 81 is fabricated from an elastic material or materials suitable for surgical applications, such as, for example, a silicone or rubber elastomer. In a unexpanded position, the dam 81 has a uniform outer diameter substantially equal to the outer diameter of the outer shaft 40 . With the dam 81 in the unexpanded state, the body 10 carrying the dam 81 on outer shaft 40 can be readily inserted or withdrawn through healthy tissue to the tissue targeted for treatment. The dam 81 can be radially expanded by the longitudinal movement of the central shaft 36 with respect to the outer shaft 40 such that the bearing surface 63 on shoulder 62 of the sleeve 39 , bearing against the distal end 83 of the dam 81 , compresses the distance between the proximal end 82 and distal end 83 of the dam 81 , thus forcing the soft elastic portion 80 of the dam to expand radially outwardly.
Although in the preferred embodiment, the dam 81 in a unexpanded position has an outer diameter substantially equal to the outer diameter of the outer shaft 40 , it will be understood that the dam could also be constructed so that the elastic portion 80 is biased toward the radially expanded position, so that in the “unexpanded” state, the outer diameter of the dam 81 is substantially greater than the outer diameter of the outer shaft 40 . This construction would require the fixed attachment of the proximal end 82 of the dam 81 to the distal end of the shaft 40 and the fixed attachment of the distal end 82 of the dam 81 to the proximal end 58 of the sleeve 39 . The radially expanded position of the dam 81 could then be radially reduced to substantially the same outer diameter as the outer shaft 40 by longitudinal movement of the central shaft 36 relative to the outer shaft 40 such that the distance between the distal end of the outer shaft 40 and the proximal end 59 of the sleeve 39 is increased, thus forcing the elastic portion 80 to stretch and be reduced in diameter.
Alternatively, rather than simply expanding radially outwardly, the dam could be engineered such that compressing the distance between the ends of the dam 81 would cause the walls of the dam to fold back on themselves, the overlapping walls thereby providing an annular expanded portion about the body.
Alternatively, the dam 81 could have proximal and distal ends 82 and 83 respectively, fixed in a sealed relationship with the outer shaft and the central shaft such that fluid pressure provided to the lumen of the outer shaft would inflate and expand the dam. In another alternative embodiment, the dam could take the form of a passive plug. The outer shaft would have a portion near the tip with a permanent bulge biased radially outwardly only with sufficient bias so that the bulge is naturally compressed by the tissue during insertion and withdrawal of the apparatus body 10 . When the body 10 is stationary, however, the “passive-plug” would automatically expand to prevent flow-back.
In another alternative embodiment, substantially the entire length of the outer shaft which is located in the apparatus track comprises a dam made of a elastic material. The elastic wall outer shaft can be inflated by fluid pressure provided to the lumen of the outer shaft. In this embodiment, substantially the entire apparatus track would be sealed by engagement with the inflated elastic outer shaft.
In yet another embodiment, the entire outer shaft comprises an elastic material which is expanded by inserting an apparatus tube of a dimension slightly larger that the apparatus track dimension (disclosed in another context in U.S. Pat. No. 5,454,790).
As a means for inhibiting a migration of the composition along the track, the dam 81 creates a seal at an interface of the apparatus 10 and the track through which the apparatus 10 is inserted. In order for the seal to effectively inhibit the flow of composition between the apparatus 10 and the track, the seal must exert a pressure between the apparatus and the track which is equal to or greater than the pressure at which the composition is delivered through the tip of the apparatus into the target tissue. In the preferred embodiment, this pressure is provided by the outwardly expanding dam 81 . A similar sealing pressure between the track and the apparatus 10 can be provided by pulling the track against the apparatus 10 . This can be accomplished by providing sufficient negative pressure, or vacuum, to the surface of the apparatus outer tube. By way of the vacuum, the track will be drawn tightly into sealing engagement with the apparatus body to prevent flow-back of composition from the target tissue.
As an alternative means for inhibiting a migration of the composition along the track, a portion of the external surface of the apparatus which is in contact with the track can be mechanically or chemically altered to adhere to the track. For example, the surface tension of the apparatus surface or the track surface can be modified to enhance adhesion of the track surface to the apparatus surface, and thus inhibit a migration of the composition along the track.
Inner shaft 28 is preferably free relative to both the outer shaft 40 and central shaft 36 . The inner shaft 28 may thus be completely withdrawn from within the central shaft for exchange, maintenance or replacement during a therapeutic procedure.
A control mechanism 16 , preferably calibrated, located at the proximal end of the body 10 facilitates movement of the shafts with respect to each other. In the preferred embodiment, the outer shaft 40 and central shaft 36 are movably connected to one another by control mechanism 16 . A collar-like ring 96 is rigidly secured to the proximal end of the outer shaft 40 by any suitable means, but preferably by screw threads. The proximal end of central shaft 36 passes through the collar-like ring 96 , extending proximally from collar-like ring 96 . A collar-like knob 89 with a central aperture 98 is rigidly secured onto the proximal end of central shaft 36 by any suitable means, but preferably by screw threads. The collar knob 89 has a distally directed reduced diameter portion 88 . Inner shaft 28 is dimensioned to pass freely through the aperture 98 . Push paddle 52 has a central collar 97 with an aperture 87 which extends from a proximal to a distal end of the push paddle collar. The aperture 87 is dimensioned on the proximal end to receive the reduced diameter portion 88 of collar knob 89 . The push paddle 97 is movably supported on the reduced diameter portion 88 of knob collar 89 . An outwardly projecting annular lug 99 secured in the aperture 87 of the push paddle collar 97 rides in a corresponding suitably dimensioned inwardly facing helical groove 101 on the reduced diameter portion 88 of the knob 89 . The lug 99 serves to guide the movement of the central shaft 36 and outer shaft 40 with respect to each other. Similarly the aperture 87 of the push paddle collar 97 is dimensioned on a distal end of the push paddle collar 97 to receive and support the outer shaft collar 96 . A suitably dimensioned outwardly projecting annular lug 105 secured on the outer shaft collar 96 of the outer shaft 40 engages an inwardly facing annular slot 103 located inside the distal end of the push paddle collar 97 . Thus, the central shaft 36 is movably secured to the outer shaft 40 by way of the central shaft knob 98 connected to the push paddle collar 97 , which in turn is movably connected to the outer shaft collar 96 .
At least one of the respective slot and lug combinations has a slot with a pitch along its length which is capable of providing travel of 0.060 inch relative to the longitudinal axis of the apparatus shaft. This pitched slot translates the radial movement of the push paddle 52 to a longitudinal movement, or travel, of the central shaft 36 . The pitch of the slot is calibrated to provide a predetermined longitudinal movement of the shaft corresponding to specific radial movement of the push paddle. For example, movement of the push paddle through 180 degrees results in 0.060 inch travel for the central shaft 36 relative to the outer shaft 40 . In use, once the tip 20 has been located in the tissue to be treated, the outer shaft 40 is preferably fixed relative to the patient, or relative to the tissue being treated, by means of a stereotactic frame 195 (FIG. 10) or similar device. Movement of the central shaft 36 in a proximal direction relative to the outer shaft 40 along the longitudinal axis of the body 10 simultaneously opens the valve means 38 and expands the dam 81 at the distal end of the body 10 . This longitudinal movement of the central shaft 36 is controlled by radial movement of the push paddle which can be connected to the central shaft 36 and the terminal fixture 49 in any suitable way such that the necessary movement of the central shaft can be effected.
Embodiments of the apparatus having one, two, three, or more shafts are contemplated by the inventors. For example, instead of an apparatus having three coaxial shafts with one shaft controlling the dam expansion, an apparatus could be constructed having only one or two shafts with a radially expanded annular dam separately mounted on an external surface of the apparatus, and with thin pieces of a flexible member (not shown), such as a steel wire, provided inside or outside the shaft(s) to control dam expansion. In a single shaft apparatus, the elastic tube comprising the annular dam 81 could function as the valve means and the dam. A proximal end of the elastic tube would be rigidly fixed to the outside of the single shaft apparatus near the distal end of the shaft, at a point between the aperture 22 and the proximal end of the shaft, by a steel band, a collar or other attachment means. The distal end of the dam comprising the dam would have a steel band or other suitable collar capable of movably mounting the distal end of the elastic tube in a sealing relationship on the outside of the shaft at a point between the aperture 22 and the tip 20 . A steel wire attached at a first end to the band or collar of the distal end of the dam, and at an opposite end to the control means 16 , would be used to draw the movable distal collar of the dam toward the fixed proximal attachment point of the dam, thus simultaneously exposing the aperture 22 and expanding the dam 81 .
Alternatively, thin members, such as, for example, a steel wire, could be provided to push a proximal end of an elastic tube comprising a dam 81 , which proximal end is movably mounted to a shaft, toward a distal end of the elastic tube which is fixedly mounted to the shaft, thus expanding the dam 81 . Between the proximal and distal ends of the apparatus, the thin member could be positioned in an existing shaft lumen, or in a separate lumen dedicated to the thin member. Alternatively, the thin member could be positioned externally of the apparatus to run alongside the shaft in the apparatus track through the tissue. The thin member should be dimensioned to provide sufficient flexibility to permit the thin member to pass through the lumen of a shaft and possibly to bend sufficiently to pass through the shaft wall to connect to the elastic tube comprising the dam. The thin member would also be required to have rigidity sufficient to transmit the pushing force necessary to cause the expansion of the dam 81 .
As noted above, the valve means 38 may comprise a sleeve 39 with at least one aperture which corresponds to the tip aperture 22 . The corresponding sleeve aperture would be radially offset to inhibit flow of liquid from the aperture, and moved to a radially aligned position to expose the tip aperture 22 to permit the flow of fluid through the aperture. In this embodiment, the dam 81 could also be expanded by a the radial movement of at least one rotating member. For example, a cam mechanism could be provided inside the elastic tubing comprising the dam 81 to expand the dam. Rotation of a cam in the mechanism would cause expansion of the dam 81 .
Terminal fixture 49 may have a shoulder 72 with a surface 73 facing the distal end 14 of the body 10 , providing a reference for calculating the extension of inner shaft 28 from central shaft 36 . In addition to providing an extension reference, the surface 73 of shoulder 72 provides a stop to prevent over extension of the inner shaft 28 beyond the end of central shaft 10 .
In use, a target tissue must first be located and mapped in the brain by using MRI, or alternatively, computer tomography, ultrasound or other imaging method. The initial location and mapping of the target tissue and the subsequent manipulation of the apparatus of the present invention to direct it to the target tissue may be accomplished by any suitable targeting and/or manipulation apparatus, method or procedure including instruments or elements separate from or integral with the present apparatus. For example, tissue may be targeted and the apparatus guided by means of any energy source, such as, absorption, defraction, scatter, or radiation, including any energy spectra such as infrared, X-ray, or visible light, including CT (computed tomography), MRI (magnetic resonance imaging), PET (position emission tomography), SPECT (single position emission computed tomography), or ultrasound. Furthermore, tissue may be targeted and the apparatus of the invention manipulated through any instrumentation approach modality, such as, for example, a trocar for percutaneous procedures. The following are other examples of targeting and/or manipulation apparatus, methods or procedures, the principles of which may be applied, either alone or in combination, to any tumor or anatomical structure of interest:
1. Laparoscopic—e.g. for intra-abdominal injection of liver tumors, abdominal metastasis, or the delivery of agents to abdominal organs by direct injection through the use of laparoscopic instrumentation, with or without, for example, visualization by the use of a viewing wand or other viewing device.
2. Thoracoscopy—e.g. for the injection of lung tumors or pleural metastasis, through the use of thoracoscopic instrumentation, with or without, for example, visualization by the use of a viewing wand or other viewing device.
3. Percutaneous—e.g. the percutaneous injection of liver or other tumors using ultrasound guidance for needle positioning.
4. Stereotactic—e.g. the direct injection of a brain tumor, with or without a stereotactic frame, following tumor localization by MR imaging.
5. open cavity—e.g. the direct injection of a tissue or organ accessed by an open surgical procedure.
6. minimally invasive/microsurgical—e.g. use of the device with a neuro-endoscope and image guided surgery system such as Philip's EasyGuide™ Neuro.
The suggested apparatus, methods or procedures may require direct manipulation (by hand) or indirect manipulation, such as, for example:
1. mechanically aided—e.g. a fixed trajectory guidance device (Patel & Sandeman, Computer Aided Surgery, 1997, 2; 186-92, incorporated herein by reference).
2. robotically aided—e.g. a robotic laparoscope positioner (automated endoscope system for optimal positioning, a.k.a. AESOP), Computer Motion Inc.
In a preferred embodiment, a suitable stereotactic frame 195 is secured to the head of the patient 197 and images are created. These images are used to determine the best approach for a biopsy instrument to enter the target tissue 198 and retrieve a biopsy specimen. The images are also used to determine the precise location and the best approach for the treatment. A biopsy is often performed using the stereotactic frame 195 to support and guide the biopsy instrument. The biopsy specimen is removed and confirmed. The stereotactic frame 195 used for the biopsy may also be used to support the apparatus 10 and guide the tip 20 to the proper location in the target tissue 198 . The distal portion of the body 10 may be inserted through healthy tissue 193 to locate the tip 20 in a target tissue 198 . Alternatively, the distal portion of the body 10 may be inserted directly into the target tissue 198 , without the tip 20 or body 10 contacting healthy tissue, by passing the body 10 through a pre-prepared opening, such as, for example, a resection cavity. In either case, the valve means 38 of the present invention is expanded to prevent premature escape of composition which could potentially harm healthy tissue in a track created by the apparatus body 10 in healthy tissue or in healthy tissue exposed in a resection cavity. Furthermore, by preventing flow-back, either through a track in tissue or through a track in a guiding, targeting, position or manipulating device cooperating with the apparatus, the dam 81 assures that a maximum intended quantity of composition remains in the target tissue 198 until the composition has served its function by being absorbed or otherwise utilized.
When the tip 20 of the apparatus has been properly positioned in target tissue 198 to be treated, the inner shaft 28 and the outer shaft 40 are held stationary relative to the stereotactic frame, and thus, stationary relative to the target tissue 198 , i.e., the tissue being treated. The retracted dam 81 is positioned approximately at the outer periphery of the target tissue 198 . The central shaft 36 is then drawn longitudinally towards the proximal end 12 of the apparatus body 10 by radially rotating the push paddle 180 degrees. The sleeve 39 , which is fixed to and moves with the central shaft 36 , and which bears against the distal end 83 of the dam 81 , moves towards the distal end of the outer shaft 40 , thus compressing the distance between the distal end 83 and the proximal end 82 of the dam 81 . Compression of the distance between the ends 82 , 83 of the dam 81 causes the dam 81 to expand radially outwardly, and thus to exert pressure against the walls of the apparatus track thereby preventing flow-back of fluid along the apparatus track by sealing the apparatus track. As noted above, the apparatus track may be a track through tissue, created by the apparatus or another surgical instrument being forced through the tissue, or the apparatus track may be a track through an auxiliary surgical device, such as, for example, a lumen in a guiding, targeting, positioning or manipulating instrument in which the apparatus is cooperatively positioned to access the target tissue. A single apparatus track may also comprise a portion which passes through tissue and a portion which passes through an auxiliary surgical device. Thus, to prevent flow-back the radially outwardly expanded dam 81 may exert sealing pressure against tissue, i.e., in an apparatus track through tissue, or against the structure of an auxiliary surgical device, such as, for example, the inner walls of a lumen of an endoscopic, laproscopic or thoracospic instrument. Furthermore, where a single apparatus track passes through tissue and through an auxiliary surgical device, one or more dams 81 may be provided to seal both the portion passing through tissue and the portion passing through the auxiliary surgical device.
The components of the apparatus are preferably arranged so that when the central shaft 36 is moved longitudinally towards the proximal end of the body 10 relative to the outer shaft 40 to radially expand the dam 81 , the central shaft 36 also moves relative to inner shaft 28 . Longitudinal movement of the central shaft 36 relative to the inner shaft 28 causes the tip opening 22 to be exposed. Composition is then passed from the reservoir 33 through the lumen 30 of the inner shaft 28 , and through the exposed tip opening 22 to the tissue to be treated. The composition flows out of the tip openings 22 in the direction of arrow 190 , and because the dam 81 has been expanded at the periphery of the target tissue 198 , composition is prevented from flowing back up the apparatus track in healthy tissue 193 . The dam 81 is held in the expanded position to prevent flow-back for a period of time sufficient to permit the composition to be substantially absorbed or otherwise utilized in the target tissue. In addition to inhibiting flow-back of composition along the apparatus track, the dam serves to anchor and stabilize the body in the patient, thus preventing accidental withdrawal or hyper insertion of the body in a patient if the patient moves during the “holding” period of the treatment, e.g. while the dam is expanded so that composition can be absorbed by the tissue being treated. When the composition has been substantially absorbed or otherwise utilized in the target tissue 198 , the central shaft 36 is moved toward the distal end of the body 10 , which in turn moves the sleeve 39 to its position covering the tip openings 22 , preventing further passage of fluid, and causing the dam 81 to unexpand and contract to its original unexpanded position. Covering, i.e., closing, the tip openings 22 not only prevents further passage of composition from the apparatus which could damage healthy tissue as the apparatus is withdrawn, but also prevents delivered compositions in the targeted tissue from flowing back into the apparatus. The apparatus body can then be safely withdrawn from the patient.
Inasmuch as the present invention is subject to many variations, modifications and changes in detail, it is intended that all subject matter discussed above or shown in the accompanying drawings be interpreted as illustrative only and not be taken in a limiting sense.
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In a method and apparatus for delivering a composition to a targeted area of tissue, exposure of a non-targeted tissue to the composition is minimized. The apparatus has at least one needle-like shaft which is inserted through a track in the non-targeted tissue to deliver the composition to the targeted tissue through an opening in the shaft. The track may be a naturally occurring lumen in a tissue, such as a vascular lumen, or may be a track created surgically by a diagnostic instrument, or by the needle-like shaft of the present apparatus. A valve-like mechanism closes the opening in the shaft to prevent premature delivery of the composition during insertion of the shaft, and to prevent loss of composition during withdrawal of the shaft. The valve-like mechanism also prevents excessive delivery of the composition to targeted tissue. An annular dam is mounted on an exterior portion of the shaft near the opening. When the opening in the shaft has been suitably positioned in the targeted tissue, the dam is radially expanded to prevent quantities of composition intended for delivery to the targeted tissue from flowing away from the targeted tissue along the track though which the shaft is inserted.
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[0001] This is a 371 national phase application of PCT/FR2006/001224 filed 30 May 2006, claiming priority to French Patent Application No. FR 0505440 filed 30 May 2005, the contents of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a pistol for controlled injection of sealing products into local areas of structures having defects in water tightness, or in media to be stabilized. The injected product is generally a mixture of several chemical constituents in relative volumes which may be different. This mixture is injected by means of a pistol and a bicomponent pump, depending on the field of use, into non-watertight expansion joints, in cracks of concrete structures, such as tunnels, underground galleries, dams, cofferdams.
BACKGROUND OF THE INVENTION
[0003] Concrete structures, subject to water pressure or buried, often include defects in tightness such as cracks, teeming arrests, non-waterproof expansion joints, coating defects of metal building components, porosities, honeycombing, at which water tightness is not ensured and where water leaks occur.
[0004] In order to ensure water tightness of these local defective areas, particularly when the liquid leaks are subject to pressure and/or have a high flow rate, it is not possible to use cement or concrete for sealing the leaking areas. The bulk concrete or cement setting time is too long to allow such leaks to be sealed.
[0005] In the case when despite everything a sealing-off of the leaks would be obtained with these materials, this seal would be rigid and would rapidly break subsequently to ground movements, expansions or contractions due to temperature differences.
[0006] It is known how to use two chemicals mixed before injection into the concrete by means of injectors, either screwed into the concrete at right angles to the defect, or of the expansive type.
[0007] These injectors have the following significant defects:
[0008] These injectors after drilling the concrete must be screwed into the support, and require the use of tools, their length and diameter should be different depending on the thickness of the concrete and on the nature of the problem to be solved.
[0009] If the injector is too short or positioned too close to the surface of the concrete, there is a high risk that the support is pulled off and/or burst upon applying pressure.
[0010] After drilling in the horizontal or vertical planes, it is required that the drilling dust be removed by blowing or washing, otherwise the injector will not be able to fulfil its role, the cracks or joints being filled with drilling dust.
[0011] After injection, the injectors are most often stuck by the injection product and cannot be recovered, they are then left in place or cut to be level with the surface of the support where they will oxidize, thereby causing oxidization spots which are difficult to suppress.
[0012] Quasi-routine replacement of these injectors has a significant effect on the financial supply and labor position.
[0013] The injector which has remained in place, blocked by the injection product, cannot be re-injected; a new perforation is required.
[0014] If the injectors have to be removed from the support with a tool of the “hub extractor” type, the operation is likely to cause damages at the surface of the support: the latter will have to be repaired.
[0015] The pistol connected to the injector should be connected and disconnected at each injection, which promotes flows of resin onto the surroundings, the tooling, the operator.
[0016] The injector-pistol assemblies on the market allow the contact of different components of the injected resin and require constant cleaning and attention, the chemicals being polymerized in the injector-pistol assemblies.
[0017] The injectors on the market have to be connected to an injection pistol, a mandatory relay towards the pump, thereby complicating the injection procedure, the maintenance, the reliability with an increase of costs.
SUMMARY OF THE INVENTION
[0018] The object of the present invention is to propose an injection pistol which overcomes all or part of the aforementioned drawbacks.
[0019] This is a pistol for injecting through an injection hole, a sealing product formed by a mixture of at least two solutions, said injection pistol comprising in a way known from document FR.2.553.304, a tubular injection system which is fed, notably under pressure, with each of said solutions and which ends with an injection head capable of penetrating into the injection hole.
[0020] In a characteristic way, according to the present invention, the tubular system includes for each solution, an independent transfer conduit emerging from the end of the injection head, so that the mixing of the solutions is performed outside the injection head.
[0021] According to this particular arrangement, the mixing of the chemical solutions with which the sealing product may be formed, is performed not in the injection device but at the outlet of the latter, in the seal defect to be sealed. So there is no longer any risk of fouling the injection head with the polymerized sealing product.
[0022] According to an alternative embodiment, a first conduit for transferring a given solution is a tube with a circular cross-section and at least one other conduit for transferring at least another solution with an annular cross-section, which is delimited by at least a tube arranged concentrically around the first transfer conduit. Thus, at the outlet of the injection head, the solution conveyed by the first transfer conduit is necessarily in contact with the solution conveyed by the transfer conduit which surrounds it in an annular way.
[0023] According to an alternative embodiment, the injection head includes towards its end, a sleeve which is crossed by the transfer conduits and which is expansible, by expansion means, between a rest position in which the injection head may be introduced into the injection hole and an expanded position in which the sleeve is sealably applied onto the walls of the injection hole. With this arrangement, the sealing product cannot flow back towards the outside in the injection hole but remains necessarily localized in the defect to be sealed.
[0024] According to an embodiment of this alternative, the expansible sleeve is a flexible tube with elastic radial deformation. Further, the expansion means include a part with a frusto-conical shape which is crossed by the transfer conduits. Finally the frusto-conical part and the expansible sleeve may be displaced relatively to each other between a rest position in which the small base of the frusto-conical part is in proximity to an aperture of the sleeve and an active position in which the frusto-conical part has forcibly penetrated from said small base into said aperture, which causes the increase of the outer diameter of the sleeve.
[0025] It is understood that the injection head should be able to penetrate into the inside the injection hole until the expansible sleeve is placed at the walls of said injection hole. Thus, in its rest position, the sleeve should have an outer diameter less than the inner diameter of the injection hole. With the radial deformation of the flexible tube forming the expansible sleeve, the latter may press against the walls of the injection hole until it forms a seal gasket preventing the mixture of the solutions during polymerization from flowing back towards the outside around the injection head.
[0026] In one embodiment, the tubular system comprises a protective tube containing the transfer conduits and at the end of which the expansible sleeve is attached, notably via a receiving ring. The protective tube forms a somewhat protective sheath for the transfer conduits. It also provides attachment of the expansible sleeve. With the presence of the receiving ring, it is possible to form a rigid attachment point for the sleeve during its expansion.
[0027] According to one embodiment, the injection pistol of the present invention comprises a dual action actuator, the actuation of which controls the dual relative displacement of the frusto-conical part and of the sleeve. Therefore, the operator after having introduced the injection head into the injection hole, may quite simply control the expansion of the sleeve by actuating the cylinder, and next, after injecting the mixture of the solutions, the passing of the sleeve into the rest position so as to be able to remove the injection head from the injection hole.
[0028] According to one embodiment, the body of the dual action actuator is connected to the frusto-conical part via the transfer conduits.
[0029] According to an alternative embodiment of the present invention, the injection pistol includes a compressed air supply. In the case when the dual action actuator is of the pneumatic type, this compressed air supply may be connected onto the cylinder of the actuator.
[0030] Further, provision may be made for sending the compressed air into the space between the protective tube and the transfer conduits right up to the end of the injection head.
[0031] The operator by actuating the compressed air supply, may therefore achieve by blowing, removal of the dusts from the bore of the injection hole. He/she may also at the end of the operation and after removing the injection head from the hole, remove by blowing, the sealing product which might be found on the surface of the frusto-conical part.
[0032] In a preferred embodiment, the injection pistol of the present invention includes two subassemblies jointed with each other, i.e.:
a) a first subassembly comprising the ducts for introducing the solutions, the transfer conduits, the frusto-conical part and the dual action actuator body and b) a second subassembly comprising a carrying handle, the protective tube, the sleeve and the cylinder of the dual action actuator.
[0035] Both of these two subassemblies are connected together through a hinged connection allowing relative longitudinal displacement without any rotation of both subassemblies relatively to each other upon actuating the actuator.
BRIEF DESCRIPTION OF THE DRAWINGS
[0036] The present invention will be better understood upon reading the description which will be made of a preferred exemplary embodiment of an enhanced injection pistol, illustrated by the appended drawing, wherein:
[0037] FIG. 1 is a very schematic illustration of the different components of the pistol,
[0038] FIG. 2 is a side view of the pistol of FIG. 1 ,
[0039] FIG. 3 is a bottom view of the pistol of FIG. 1 and
[0040] FIG. 4 illustrates both the rest and expanded positions of the sleeve fitting out the injection head of the pistol of FIG. 1 .
DETAILED DESCRIPTION
[0041] In the injection pistol 30 which will be described hereafter, the sealing product is made from a mixture of two chemical solutions. This is not exclusive of the present invention; the number of chemical solutions to be mixed may be larger than two.
[0042] In the present case, this may notably be a mixture of an aqueous acrylic solution and an aqueous solution containing a polymerization initiator, of the type of that described in document FR.2.630.743.
[0043] With reference to FIG. 1 , the injection pistol 30 includes an injection head 31 which is fed with each of both chemical solutions from a first intake 8 for the solution corresponding to the resin and from a second intake 11 as for the solution containing the polymerization initiator. At least the first intake 8 is fitted out with a non-return valve and a fast coupler 9 . Each of these intakes opens out onto the transfer conduit which is specific to it. In FIG. 1 , at the injection head 31 , transfer conduits 3 , 4 may be seen, which are positioned concentrically along the longitudinal axis of the injection head. The transfer conduit 4 is a tube with a circular section. It is intended to convey the solution containing the polymerization initiator, supplied from the intake 11 . The transfer conduit for the resin, from the intake 8 , is conveyed in an annular transfer conduit, internally delimited by the first tube 4 and externally delimited by the second tube 3 .
[0044] The pistol 30 includes a dual action actuator 15 which may be pneumatic, electric, electro-mechanical or hydraulic.
[0045] Its connection 2 is adapted to its operating mode. In the present case, this may be a compressed air supply 1 .
[0046] Both tubes 3 , 4 , notably made in stainless steel 316L, are contained in a protective tube 20 which may also be in stainless steel 316L or in aluminium. Both tubes 3 , 4 , are firmly attached to the actuator 15 and at their other end, to a frusto-conical part 7 , through which the tubes 3 , 4 pass. In FIG. 1 , the end 17 of the first tube feeding the solution containing the polymerization initiator opens out beyond the second tube 3 .
[0047] At the distal end of the protective tube 20 , a receiving ring 5 is provided allowing an expansible sleeve 6 to be attached thereto. In the present case, this is a flexible tube which may be elastically deformed radially.
[0048] The proximal end of the protective tube 20 is firmly attached to the cylinder of the dual action actuator 15 .
[0049] Overall the injection pistol 30 consists of two subassemblies which are jointed with each other by a hinged connection 19 so as to allow the expansible sleeve 6 and of the frusto-conical part 7 to be relatively displaced with respect to each other.
[0050] The first subassembly comprises the ducts for introducing the solutions, the transfer conduits, i.e. both tubes 3 , 4 , the frusto-conical part 7 and the body of the dual action actuator. The second subassembly comprises the protective tube 20 , the sleeve 6 and the cylinder of the dual action actuator. This second subassembly also comprises a structural component on which a carrying handle 23 is attached.
[0051] Both positions are illustrated schematically in FIG. 4 , the rest position on the one hand ( FIG. 4A ) and the expanded position on the other hand ( FIG. 4B ).
[0052] First of all, the operator has proceeded with drilling an injection hole 32 of a determined diameter D 0 . He/she positions the injection head 31 so as to cause the frusto-conical part 7 to penetrate into the injection hole and the expansible sleeve 6 in the rest position, having in this condition an outer diameter D 1 , which substantially corresponds to the outer diameter of the protective tube 20 . He/she then actuates from the handle 16 , the dual effect actuator 15 , so as to displace the cylinder relatively to the body of the actuator in the direction of the arrow F ( FIG. 4B ). This backward displacement relatively to the carrying handle 23 will correlatively cause backward motion of the frusto-conical part 7 inside the injection hole 32 . During this displacement, the small base 7 a of the frusto-conical part 7 which was in proximity to the distal aperture of the sleeve 6 penetrates into the inside of said aperture. At the end of the displacement, in the example illustrated in FIG. 4B , the frusto-conical part 7 has totally penetrated inside the sleeve 10 , which is therefore deformed radially, consequently increasing the diameter D 1 . This radial deformation is provided so that the sleeve in the expanded position will be strongly applied against the inner walls of the injection hole 32 , forming a sealed barrier.
[0053] It is in this spread position of the sleeve 6 that the operator may accordingly control the arrival of two chemical solutions which both emerge through transfer conduits right up to the end of the injection head, directly into the injection hole 32 and into the cavity to be sealed, without any possible backward flow around the injection head 31 .
[0054] Actuation of the dual effect actuator 15 causes, as described above, the backward motion, relatively to the handle 23 of the first subassembly. In order to allow this backward motion, the injection pistol 30 is fitted out with a joint hinge 19 , which is able to connect both subassemblies and withstand by angular pivoting the relative displacement of both of these subassemblies.
[0055] This hinge 19 consists of two plates 33 , 34 , connected to each other by a transverse pivot axis 35 . Each plate 33 , 34 is itself connected to a subassembly by a transverse pivot axis 36 , 37 . In the rest position of the injection pistol ( FIG. 4A ), both plates 33 , 34 together form an angle α. At the end of the backward motion, the sleeve 6 being in the expanded position ( FIG. 4B ), both plates 33 , 34 together form an angle β larger than the angle α.
[0056] With this hinge mounted on three parallel transverse axes 35 , 36 , 37 , both subassemblies may be displaced without any rotation.
[0057] When the sealing operation is finished, it is sufficient for the operator to actuate the handle 16 so as to perform the displacement of both subassemblies in the opposite direction, in order to put the sleeve 6 back into its rest position and to perform extraction of the injection head from the hole 32 .
[0058] It is then sufficient for the operator to fill the portion of the hole 32 occupied by the sleeve 6 with a mortar without any shrinkage. Thus, it will subsequently be possible to reuse the same injection hole if necessary.
[0059] Notably in the case when the injection pistol includes a compressed air supply, for actuating the air actuator, this compressed air supply may also be used for removing the dusts caused by the drilling of the injection hole on the one hand and for cleaning the frusto-conical part 7 from possible deposits of sealing product which might have occurred, on the other hand. In this case, the compressed air supply is directed into the space between the protective tube 20 and the second tube 3 right up to the end of the injection head 31 . This compressed air emerges through the injection head at the distal end of the sleeve and directly arrives on the outer surface of the frusto-conical part 7 .
[0060] This frusto-conical part 7 may be in stainless steel or in a synthetic material. The flexible tube acting as a sleeve may also be in a synthetic material but which is flexible and sufficiently deformable so as to lead to the result as described earlier.
[0061] The intakes 8 , 11 for the chemical solutions are connected to a pump connected to a hydraulic unit on the one hand and to the containers containing said solutions on the other hand. It is this pump which provides the chemical solution supply. It is connected to the injection pistol 30 at the beginning of the operation and disconnected at the end of the operation. Therefore, there is no loss of product or tedious cleaning. Connection and disconnection are achieved in a very simple and fast way.
[0062] Provision may also be made for a discharge handle 10 .
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The pistol is used for injecting through a hole a sealing product formed by a mixture of at least two solutions. It comprises a tubular injection system which is fed, notably under pressure, with each of said solutions, and which ends with an injection head capable of penetrating into the injection hole. The tubular system includes for each solution, an independent transfer conduit emerging from the end of the injection head, so that the mixing of the solutions is performed outside the injection head. Preferably, the first transfer conduit is a tube with a circular cross-section and the other transfer conduit(s) has(have) an annular cross-section, being delimited by one or several tubes arranged concentrically around the first transfer conduit.
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FIELD OF THE INVENTION
The present invention relates to a control magnet assembly for a pattern apparatus in knitting machines for electrically controlled needle selection. The control magnet assembly has at least one selection magnet, which is provided with at least one permanent magnet retainer pole zone and at least one control pole zone, with which at least one control coil, which is triggerable in accordance with the pattern, is associated, and against which armature elements that are operatively connected to the needles can be moved.
BACKGROUND OF THE INVENTION
In control magnet assemblies of this kind, which are known in both flat-bed knitting machines and circular knitting machines (for example, see German Auslegeschrift No. 15 85 206, German Patent No. 20 10 973, German Offenlegungschrift No. 21 50 360 and German Offenlegungschrift No. 25 19 896), a variably large number of armature elements are retained on the selection magnet, in accordance with the triggering by the pattern apparatus in the through travel direction following the control pole zone. These armature elements form magnetic short-circuits with respect to the armature element that at a given time is actually in the control pole zone. As a result the retaining force with which that particular armature element is retained in the control pole zone is varied, and hence also the magnitude of the counter field that is to be built up relative to the permanent magnetic field, so as to reduce the retaining force to zero or to the vicinity of zero in the control pole zone for "throwing off" an armature element. In other words, the magnetizing current to be expanded to generate the counterforce and which is to flow through the control coils is dependent in its magnitude on how many armature elements remain attracted immediately previously. The fewer armature elements continue to adhere, the greater must the magnetizing current be that must flow through the control coil. This problem arises to an even greater extent in multi-system knitting machines or selection magnet systems, because the neighboring pole zones "throw off" in various ways. The same applies to flat-bed knitting machines, in contrast to circular knitting machines; in circular knitting machines, armature elements are always presented, while in the case of flat-bed machines this is not the case in the stroke reversal zones, where quite variable magnetic conditions therefore prevail.
In the known control magnet assemblies, optimal throwing off by the particular armature elements does not take place because the magnetic counterforce generated by the always-constant magnetizing flow through the control coil may possibly be too large or too small, which in either case can cause an armature element that should be thrown off to remain stuck. Although it is known from German Offenlegungschrift No. 21 50 360 to provide the selection magnet with an adjustable magnetic shortcircuit, nevertheless all this means is that manufacturing tolerances and material deviations which affect the magnetic circuit can be compensated for. The above-described problem or disadvantage still exists, however.
OBJECT AND SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved control magnet assembly for a pattern apparatus in knitting machines for electrically controlled needle selection of the above generic type such that optimal magnetic conditions in the control pole zone are furnished in such away that uniform and reliable throwing off of the particular armature elements is always attained.
This object is attained, in a control magnet assembly as described above, by providing a measuring head for detecting the magnitude of the magnetic field in the control pole zone and by providing a circuit layout between the measuring head and the control coil.
Since the measuring head can measure the instantaneous magnetic field intensity in the control pole zone at any time, the value of this magnetic field intensity being used via the circuit layout for determining the optimal countermagnetization, the retaining force can always be brought accurately to the predetermined value, for instance zero, for throwing off following armature elements, regardless of the number of existing short circuits caused by adhering armature elements. As a result, uniform dropping off is attained for all the armature elements, without the danger that one or another armature element that should be thrown off will stick. An always constant and accurate compensation for the existing permanent magnetic field in the control pole zone for throwing off of armature elements is thus assured. At the same time, any manufacturing tolerances and differences in the properties of the material that affect the magnetic circuit or circuits are also compensated for.
The measuring head may inherently be embodied by arbitrary elements for measuring the field intensity. Suitably, however, a Hall generator is used for the measuring head, because such an element is a reliable and small-sized component.
In order to obtain the most accurate possible measurement of the field intensity in the control pole zone, the measuring head is disposed near the control pole zone pole face opposite the armature elements.
From German Offenlegungschrift No. 21 50 360 it is known to provide pole pieces on both sides of the selection magnet, with the ends of the pole pieces that have the pole faces leaving a gap open between them. In an exemplary embodiment of the present invention, this gap between the pole pieces in the vicinity of the ends is utilized for accommodating the measuring head, by displacing the measuring head in the gap formed between the pole ends. This also provides an optimal disposition of the measuring head. It is also suitable for the measuring head to be set back with respect to the pole faces and to dispose a nonmagnetic strip of hard material in the qap, adjoining the measuring head, the free end face of this strip protruding somewhat beyond the pole faces. As a result the measuring head is not only brought close to the pole faces, but central guidance of the particular armature elements is also provided.
According to the present invention it is also advantageous to surround each of the pole pieces with a control coil, both control coils being triggerable in parallel uniformly in the same direction, so that on both sides of the measuring head and of the nonmagnetic strip an identical magnetic field, in the opposite direction from the permanent magnetic field, is generated. The effective inductance is also reduced thereby, resulting in a quick rise in current and thus in an accelerated and improved control (that is, more-rapid compensation for the permanent magnet field).
In another exemplary embodiment of the present invention, the circuit layout has a control circuit, which is coupled to a comparator circuit having a measuring resistor connected in series with the control coil or coils; the output of the comparator circuit is equal to the difference between the voltage derived from the magnetizing current at the measuring resistor and the Hall voltage. As a result, very simple regulation based on the pertinent comparison is attained. This circuit layout also makes it possible to apply a relatively high feed voltage U M of 40 V for instance, so that by this means as well very short current rise times and thus a very rapid compensation for the permanent magnet field are attainable. This circuit layout is also short-circuit-proof if there is a defective sensor or even if there is no sensor at all.
The control circuit suitably has an adjustable level adaptation circuit, by means of which calibration, based on manufacturing tolerances and deviations due to the particular design, can be attained before the apparatus is placed in service.
It is suitable if both the selection magnet and those parts of the circuit layout that serve to calibrate the magnetic system are received by a circuit board and disposed inside a common housing. If the housing is detachably secured to the front panel of the cam carriage, then this component unit can be removed and replaced as a unit, without requiring further assembly work and calibration operations.
If the control magnet assembly for a multi-system knitting machine is provided with a number of selection magnets corresponding to the number of needle selection systems, then it is particularly advantageous if a common permanent magnet is used for the permanent-magnetic retaining pole zones of the selection magnets.
Further details of the invention will become apparent from the ensuing detailed description of an exemplary embodiment shown in the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal section taken through a needle bed of a flat-bed knitting machine and a control magnet assembly, located movably above this needle bed, in accordance with a preferred exemplary embodiment of the present invention;
FIG. 2, on a larger scale, is a plan view of the control magnet assembly in the direction of the arrow II in FIG. 1;
FIG. 3 is a longitudinal section, selected in accordance with FIG. 1, taken through the control magnet assembly along the line III--III of FIG. 2;
FIG. 4 is a section rotated by 90° as compared with FIG. 3 through the control magnet assembly along the line IV--IV of FIG. 2; and
FIG. 5 is a schematic diagram of a circuit layout such as is used in the control magnet assembly according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The control magnet assembly 10 shown in the drawings, in accordance with a preferred exemplary embodiment of the present invention, which is connected via a control cable 11 to a pattern apparatus, not shown, of a flat-bed knitting machine, is secured to the back side of a front panel 13 of a carriage 12 not shown in detail, and a head portion 14, in this case containing two measuring heads 15, 25, which penetrates the front panel 13 through a slit-like recess 16 and protrudes beyond the front side, facing a needle bed 17, on the front panel 13. The carriage 12 provided with the control magnet assembly 10 is movable back and forth along the needle bed 17, in which a multiplicity of knitting needles 18 are supported in needle slots 20 such that they are movable back and forth (to the left and right as seen in FIG. 1) crosswise to the direction of carriage travel. The needles 18 are connected in a manner not shown in detail to a needle pusher 19, which can be acted upon by a selection jack 21. The selection jack 21 is substantially embodied as a two-armed lever, and is held movably in the direction of movement of the needles 18 in the needle slot 20 associated with the particular knitting needle 18. The selection jack 21 is mounted pivotably on the bottom of the needle slot 20, has a butt 23 on its rearward arm, remote from the needle pusher 19, and an armature element 26 of magnetic material on its forward arm 24, oriented toward the needle pusher 19. The rearward arm 22 of the selection jack 21 is acted upon by a leaf spring 27 such that the selection jack 21 in the position of repose is pivoted away so that its armature element 26 is located inside the needle slot 20 and its rearward butt 23 is located outside the needle slot 20.
In the usual manner, upon the transit of the carriage 12, the selection jacks 21 are pivoted counter to the action of the leaf spring 27 (as shown in FIG. 1) by means of cams, not shown, disposed on the carriage 12 and are thus presented to the control magnet assembly 10 and are held thereby in the presented position, and upon further movement of the carriage 12 are either retained further or let loose or "thrown off", by reduction of the magnetic retention force to zero, so that the particular selection jacks 21 can move into their position of repose, under the influence of the leaf spring 27. In the exemplary embodiment, in this position of repose, the selection jack 21 and thus the associated knitting needle 18 is selected, because it is movable toward the needle pusher 19, by means of a feeder element secured to the carriage and on which the butt 23 comes to rest, so that the needle 18 can be moved into a working position.
The control magnet assembly 10, according to the exemplary embodiment of FIGS. 2--4, has two selection magnet systems 29 and 30 which come into action in succession and which together have a strip-like permanent magnet 31, which extends oriented longitudinally upright on both wide side faces 32, 33 of the permanent magnet 31, pole pieces 34, 35 extend and rest in platform-like fashion. While in the longitudinal extension of the permanent magnet 31 the two pole pieces 34 and 35 protrude only slightly at both ends, in the direction of the transverse extension of the pole pieces 34 and 35 are substantially wider than the permanent magnet 31, although the upper long side 36 of the permanent magnet 31 protrudes somewhat beyond the upper long sides of the pole pieces 34, 35. Viewed in the longitudinal direction, the pole pieces 34 and 35 are divided into a plurality of elements 37-41 and 47-51 (see FIG. 2), which as shown in FIG. 4 are each separated from one another by a small gap. Reference numerals 37, 47 or 39, 49 or 41, 51, for pole pieces 34 and 35, identify the outer (on the left in FIG. 2) or inner or outer (on the right of FIG. 2) retaining pole piece elements of the pole pieces 34 and 35, that is, those which define the retaining pole zones of the two selection magnet systems 29, 30 of the control magnet assembly 10. In contrast, referenece numerals 38, 48 and 40, 50 designate the control pole piece elements of the pole pieces 34 and 35, that is, those which define the control pole zones of the two selection magnet systems 29, 30 of the control magnet assembly 10. The retaining pole piece elements and the control pole piece elements are identical among themselves, the control pole piece elements being substantially narrower than the retaining pole piece elements. A division of the control magnet assembly 10 into the two selection magnet systems 29 and 30 is effected by the plane 55 shown in FIGS. 2 and 4. The control pole piece elements 38 and 48 or 40 and 50 are each surrounded by a control coil 42 and 52 or 43 and 53. The control coils 42, 52 and 43, 53 are located with their top surfaces spaced apart by a short distance from and facing the lower long side of the permanent magnet 31 and across a further portion of the widthwise extension of the pole pieces 34, 35 as far as the head portion 14. The control coils 42 and 52 or 43 and 53 each belonging to one pair of the control pole piece elements 38 and 48 or 40 and 50 facing one another are wound in the same direction and substantially fill up the gap 44, formed with approximately the same thickness as the permanent magnet 31, between the two pole pieces 34 and 35 (FIG. 3) and the gap 44 or 46 with respect to the adjoining retaining pole piece elements 37, 47 or 39, 49 or 41, 51 (FIG. 4). The gaps 45, 46 between the retaining pole piece elements and the control piece elements taper as shown in FIG. 4 and in the vicinity of the ends 56 and 57 of the pole pieces 34 and 35 disposed in the head portion 14 form a very small air gap 58 or 59, which are offset inward and parallel with respect to the gaps 45 and 46. The control pole piece elements are thus narrower in the vicinity of their free ends than in the vicinity surrounded by the control coils, so that in the direction of travel X or Y of the carriage 12, narrow control pole face sections 61 result, corresponding to the thickness of the armature element 26. In the same plane as the control pole face sections 61 are the retaining pole face sections 62, which are defined by the retaining pole piece elements.
Displaced in the head portion 14 of the control magnet assembly 10, on the lower side of the corresponding pair of control coils 42, 52 or 43, 53 and in the gap 44 between the associated two control pole piece elements of the pole pieces 34 and 35 of each selection magnet system 29, 30 is the measuring head 15 or 25 for measuring the magnetic field intensity in each of the control pole zones. The measuring head 15, 25 is a Hall generator, in the preferred exemplary embodiment of the present invention shown. It will be understood that other elements which measure the magnetic field intensity may also be used. The Hall generator 15, 25 is disposed in the respective intermediate zone 54 along which the gaps 45, 46 taper to the air gaps 58 and 59. Immediately adjacent to the underside of the measuring head 15, 25, a slide strip 63 is provided in the gap 44, which comprises a hard material such as sapphire and along the sliding face 64 of which the armature elements 26 of the selection jacks 21 slide. The sliding strip 63 has approximately the same length as the permanent magnet 31 and is likewise embodied in one piece. Its sliding face 64 protrudes beyond the pole face sections 61 and 62 by a slight amount, for example 0.05 mm, so that a correspondingly small air gap is formed between the armature elements 26 and the pole faces 61, 62.
The two selection magnet systems 29 and 30, forming a unit, are inserted into a rectangular recess 67 of a housing 66, with an interposed elastic filling composition 68. In the vicinity of the recess 67, the housing 66 has an extension 69 on its open front side, in the form of two parallel side walls in which the head portion 14 of the two selection magnets 29 and 30 is received. Adjoining the rectangular recess 67, remote from the extension 69, is a wider, approximately rectangular hollow space 71, which is subdivided by means of a circuit board 72 that is detachably secured in the hollow space 71. The circuit board 72, with components shown in the form of boxes 70 in FIGS. 3 and 4, forms a control circuit 74 for each selection magnet system 29, 30; this control circuit 74 is connected, in a manner shown in greater detail in FIG. 5, via lines 76, 77, 78 and 79 to the respective measuring head 15 or 25, to the respective control poles 42, 43 or 52, 53 and to a level control circuit 86 and a comparator circuit 73, which are for example accommodated in a cabinet next to the machine. The circuit board 72 also carries a plug-in bushing 81, into which the cable 11, for example for both selection magnet systems, leading to the pattern apparatus and to the circuits 73, 86 can be plugged. The hollow space 71 is covered by a detachably secured cap 82. The substantially approximately rectangular housing 66 has cooling fins 83 on its long sides. The housing 66 is secured via connecting screws that are inserted into bores 84 to the front panel 13 of the cam carriage 12 such that it is detachable from outside, so that it is replaceable on its own, as a component containing the selection magnet systems, without requiring further assembly or disassembly.
From FIG. 5, the circuit layout of the control magnet assembly 10 according to the invention, having the electrical circuits 73, 74, 86, can be seen. Each pair of control coils 42 and 52 or 43 and 53 is connected in parallel with one another and near the trigger circuit 86, which is supplied with direct current U M (of 40 V, for example), is connected to the pattern apparatus, not shown, of the knitting machine for the pattern-dependent triggering via a line 87. Connected to the trigger circuit 86 is the comparator circuit 73, which contains a measuring resistor 88 and a voltage comparator 89, one input of which is connected to the measuring resistor 88, the other input of which is connected to the control circuit 74, and the output of which is connected to the trigger circuit 86. The control circuit 74, which on its output side is connected to the comparator circuit 73, is connected on its input side to the associated measuring head or Hall generator 15, 25. The control circuit 74 contains an adjustable calibration element 91, an adjustable amplifier and level adaptation element 92 and a threshold value limiting element 93, which are connected in series. Thus each selection magnet can be calibrated and adjusted on its own, regardless of where it is used.
The function of the control magnet assembly 10 according to the invention is as follows: If a presented armature element 26 of a selection jack 21, after sliding along the retaining pole zone of a selection magnet system 29 or 30, is supposed to be "thrown off" in the control pole zone of this system, then in accordance with the pattern a magnetizing current is supplied to the appropriate control coil pair, such that a magnetic field is built up very rapidly in the control pole zone, this field being opposite to the permanent magnet field in the control pole zone and having the same magnitude, so that the magnetic retaining force is reduced to a predetermined value that is less than the force of the leaf spring 27 acting upon the selection jack 21. Preferably the magnetic retaining force should be reduced to zero. In order to attain this value for the resultant magnetic retaining force accurately, regardless of how many of the selection jacks preceding this selection jack 21 that is to be thrown off are sticking to the following retaining pole zone, the instantaneously prevailing field intensity is measured in the control pole zone by means of the field intensity sensor 15 or 25, embodied as a Hall generator, and processed in the control circuit 74 and delivered to the input of the comparator circuit 73. The comparator circuit 73 is also supplied with the magnetizing voltage picked up at the measuring resistor 88, which is proportional to the magnetizing current supplied to the control coil pair. The differentiating output of the comparator circuit 73 determines the magnetizing current to be supplied to the pair of control coils, and this current is the input signal for the trigger circuit 86. If the difference between the two voltages to be compared is greater than zero, then the magnetizing current is increased until because of the reduction of the magnetizing field intensity the differential output is equal to zero. In this process, a triggering of the associated pair of control coils takes place by means of the trigger circuit 86 only whenever a trigger signal arrives in accordance with the pattern via the line 87.
It will be understood that one suitable electrical circuit layout is associated with each selection magnet 29 or 30, each of which is triggered separately in accordance with the pattern. It will also be understood that the control magnet assembly 10, in the event that instead of a two-system knitting machine, a onesystem machine is being used, will have only one selection magnet 29 or 30. Correspondingly, with multi-system arrangements a plurality of selection magnets may also be secured as a unit on a carriage 12, and preferably one common permanent magnet is provided (this is known as the three-way technique).
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A control magnet assembly (10) for a pattern apparatus in knitting machines, for electrically controlled needle selection, has selection magnets (29, 30), which are provided with permanent magnetic retaining pole zones and with control pole zones with which control coils (42, 43; 52, 53) that are triggerable in accordance with the pattern are associated, and against which armature elements (26) operatively connected with the needles (18) can be brought. In a control magnet assembly (10) of this kind, optimal magnetic conditions in the control pole zone are to be provided such that a uniform and reliable throwing off of the appropriate armature elements (26) is always attained. To this end, a measuring head (15, 25) is provided for detecting the magnitude of the magnetic field in the control pole zone, and a circuit layout is provided between the measuring head (15, 25) and the control coil (42, 43, 52, 53).
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FIELD OF THE INVENTION
The present invention relates to film growth technology. Specifically the present invention relates crystalline surface structures and to methods for fabricating crystalline structures on the surface of a template.
BACKGROUND OF THE INVENTION
Examples of so called monolayer crystalline surface (MCS) structures include essentially two-dimensional lattices of carbon (e.g. graphene), nitrogen and boron. When many parallel monolayers are present, such structures constitute a bulk material (as opposed to a film). Layered structures of 1 to 10 layers of essentially coplanar MCS-structures can be termed as few-layered crystalline surface (FCS) structures and they can still be termed films. Bulk or many-layered material containing tens of layers of essentially coplanar FCS-structures, when containing carbon, are termed graphite. FCS-structures can be distinguished from bulk also in that quantum effects are still important when the number of layers is small.
Graphene-based components have wide ranging applications for example in conductive pathways, transistors and sensors. FCS-structures are of great interest due to their unique and useful physical and chemical properties. FCS-structures in, for instance, polymers allow for the creation of flexible and transparent electronic devices.
Ideally, even an individual ribbon of an FCS-structure (containing one or a few monolayers) with a well defined property and in a specific location is sufficient for many applications. An example of such a structure is a Graphene Nano Ribbon (GNR). When these structures are narrow (on the order of a few nanometers wide) or thin (on the order of a few atomic layers thick) they exhibit quantum effects useful for many applications.
The high conductivity of certain FCS-structures, such as graphene, together with the ability to form these structures into 2D structures having extremely high aspect ratios, e.g. into graphene (carbon) nano-ribbons, allow for the production of high performance electronic components. The FCS-structures or the high aspect ratio structures fabricated from them may be utilized, for instance, as the conductive or semi-conductive channel of a transistor or sensor, or as a conductive element in a transparent electrode.
Graphene and carbon nano-ribbon based devices have already been successfully used as gas detectors, transistors, and transparent conductive coatings. Also, they are considered to be strong candidates for the replacement of ITO in transparent electrodes where the high costs of raw materials and production processes, together with performance barriers related to brittleness and coloring, are limiting their commercial lifetime.
For many purposes, the controlled synthesis of FCS-structures wherein the geometry and/or the location of the FCS-structure can be controlled is required. Moreover, FCS-structures already integrated on a substrate can be easier to manipulate, to assemble and to integrate into devices than randomly produced “stand-alone” fragments e.g. in a solution. Moreover, free fragments tend to fold or roll-up, thus reducing or negating many of their useful properties.
To date, manufacturing of FCS-structures in general and of devices based on individual FCS-structures has been too difficult, time-consuming and expensive to be commercially viable. For instance, in the case of graphene, only physical or chemical exfoliation from graphite has been shown to produce carbon MCS-structures (graphene). An example of an exfoliation method is disclosed in “Novoselov K. S., Electric Field Effect in Atomically Thin Carbon Films, Science, Vol. 306, no. 5696, pp. 666-669, 2004”. The drawbacks of such methods include e.g. lack of control of the end-product in terms of both quality and location, and a typically random and fragmented distribution of the MCS sheets on a substrate or in a solution. The problems associated with the prior art methods, the difficulty in producing consistent product, controlling the location of the product on substrates and patterning the product, together lead to complex and expensive manufacturing processes.
PURPOSE OF THE INVENTION
The purpose of the present invention is to reduce the aforementioned technical problems of the prior-art by providing a new type of method for fabricating crystalline surface structures, especially few-layered crystalline surface structures (FCS-structures) on a template.
SUMMARY OF THE INVENTION
The method according to the present invention is characterized by what is presented in claim 1 .
The product according to the present invention is characterized by what is presented in claim 12 .
The use according to the present invention is characterized by what is presented in claim 13 .
A method according to the present invention, for fabricating crystalline surface structures on a template, comprises the steps of providing a template into a reaction environment, wherein one or more elements required for the formation of the crystalline surface structure are contained within the template, heating the template inside the reaction environment to increase the mobility of the element within the template, and to increase the surface diffusion length of the element on the template-environment interface, and activating the template by altering the conditions within the reaction environment, to make the mobile element slowly migrate towards the template-environment interface and to make the element organize on the surface of the template as a crystalline structure. Furthermore, the crystalline structure is a monolayer crystalline surface (MCS) structure or a few-layered crystalline surface (FCS) structure.
A crystalline surface structure according to the present invention is fabricated by a method according to the present invention.
According to the present invention a method according to the present invention is used in the fabrication of a product.
According to one embodiment of the present invention, activating the template by altering the conditions within the reaction environment comprises releasing the element from the bulk of the template by a chemical reaction and/or by supersaturation of the template.
According to one embodiment of the present invention, activating the template by altering the conditions within the reaction environment comprises altering the temperature of the template and/or altering the partial pressure of the element in the reaction environment.
A few-layered crystalline structure (FCS) is a structure in which individual atomic layers are not covalently bonded to each other but are able to glide in plane with respect to each other.
Heating the template containing one, some or all of the elements required for the formation of the crystalline surface structure over the template, increases the mobility of the atoms or molecules of these elements both inside the template and at the template-environment interface. When the conditions of the template and/or of the reaction environment holding the template are suitably altered, at least a fraction of the elements migrate from inside the template onto the template-environment interface. Ensuring that the migration rate is sufficiently low and that the surface diffusion length of the element(s) on the surface of the template is sufficiently high, the atoms of the migrated elements will have sufficiently high mobility on the surface of the template to nucleate on an energy minimum. The surface diffusion length of the element(s) on the surface of the template can be controlled by controlling the temperature of the template and the pressure of the reaction environment. These parameters have to be adjusted so that the surface diffusion length is high enough to enable two-dimensional crystalline growth, at the same time ensuring that the elements do not become volatile on the surface of the template. As some materials possess a local energy minimum in a two dimensional configuration, a method according to the present invention may be used to produce crystalline surface structures with even a monolayer thickness, i.e. MCS (Monolayer Crystalline Surface)-structures.
A method according to the present invention provides a simple way to easily and efficiently synthesize FCS-structures on metal, insulator, polymer or other useful substrates, without the need for unreliable exfoliation techniques which furthermore are difficult to control. The method enables the production of a non-fragmented continuous crystalline surface structure on the surface of a template. The resulting structure commonly conforms to the shape of the template. Thus, by using a template of a suitable shape with a long or virtually infinite radius of curvature, essentially planar sheets of crystalline material may be produced on the template. The template may be e.g. solid, vitreous or liquid material.
According to one embodiment of the present invention, the method comprises the step of impregnating a heated template by the element by introducing the element into the reaction environment in a gas or in a liquid flow over the template, and by letting the element diffuse into the heated template.
According to one embodiment of the present invention, impregnating the heated template comprises introducing the element into the reaction environment as part of one or more precursors which thermally or chemically decompose inside the reaction environment to release the element to be diffused inside the template.
According to one embodiment of the present invention, impregnating the heated template comprises introducing carbon monoxide (CO) precursor into the reaction environment into contact with the template, for making carbon diffuse into the template.
The impregnation of the template may be simply carried out by placing the template in a reaction environment, and by exposing the template to a gaseous composition incorporating the element with which the template is to be impregnated. The one or more elements in the gaseous composition may be in elemental form or as part of precursor molecules.
According to one embodiment of the present invention, the element is selected from the group of carbon, nitrogen and boron.
According to one embodiment of the present invention, the crystalline surface structure is graphene.
Carbon, nitrogen and boron are elements that are known to possess crystalline structures which have a local energy minimum in a two dimensional configuration. Carbon, nitrogen and boron are therefore suitable materials for FCS-structures obtainable with a method according to the present invention. Specifically graphene, possessing interesting electrical, chemical and mechanical properties may be fabricated by using carbon monoxide (CO) as a precursor for impregnating the template with carbon. The carbon may be made to migrate onto the surface of the template from inside the template in a method according to one embodiment of the present invention. On the surface of the template the carbon atoms may self organize as graphene by surface diffusion, to minimize the energy of the crystalline lattice.
According to one embodiment of the present invention, the material of the template comprises transition metal, oxide, nitride or carbide. These template materials are suitable for impregnation with carbon, nitrogen or boron, as the diffusion rate of these elements into (and migration rate out of) the aforementioned template materials, is inherently relatively quick even at low template temperatures and at small concentration differences between the template and its environment. The inherently high rate of diffusion and migration enables to more efficiently control these processes by external process parameters, which is beneficial for homogeneous impregnation of the template and for reliable fabrication of an FCS-structure onto the surface of the template.
According to one embodiment of the present invention, the method comprises the step of positioning the template on a substrate. The substrate is commonly solid or vitreous.
According to one embodiment of the present invention, the template is liquid whose surface tension and wetting angle on the substrate are small enough that the liquid template forms a continuous film over the substrate.
When the template material is in liquid phase (or becomes liquid during a method according to the present invention), a substrate may be needed to mechanically support the template. Use of a liquid template material may be beneficial e.g. due to inherently more rapid migration and diffusion processes compared to solid templates, which enables to more efficiently control the migration and diffusion processes by external process parameters. Such process parameters include the temperature, the pressure and/or the chemical composition of the reaction environment.
A further advantage of the present invention is that it provides a method for fabricating crystalline structures, specifically FCS-structures, on a template from which the FCS-structures can be easily transferred onto secondary, e.g. polymer, substrates or integrated into electronic devices. By impregnating the template with different elements the resulting FCS-structures can be fabricated in different compositions comprising these different elements. The method according to the present invention allows for simpler, cheaper and more versatile method for fabricating FCS-structures than prior art techniques, thus allowing reduced cost and better performance.
The invention is particularly useful in, for example, the manufacturing of homogeneous or patterned transparent, conductive, and flexible polymer films comprising graphene or other FCS-structures. The invention may also be used in the fabrication of e.g. coated and multi-layered or three-dimensional structures, which are suitable for many optical and electronic applications such as opaque or transparent electrodes, interconnects, transistors, memory elements, diodes, lasers, filters, optical absorbers, saturable absorbers, field emitters, photo receptors, logic gates, inverters, probes; electrochemical devices such as supercapacitors, hydrogen storage (e.g. in fuel cells); analytical applications such as gas sensors, electrode materials and/or modifiers for analytical voltammetry, biosensors; chromatographic applications; mechanical applications such as conducting composites for antistatic shielding, transparent conductors for shielding of electromagnetic interference; electron guns for microscopes, field emission cathodes in, for instance, microwave amplifiers and/or field emission displays, gas storage, field-effect transistors, nanoribbon electromechanical actuators, electrodes in lithium batteries, light sources, saturable absorbers, nanosensors, solar cells, fuel cells, ultracapacitors and/or thermionic power supplies.
The embodiments of the invention described hereinbefore may be used in any combination with each other. Several of the embodiments may be combined together to form a further embodiment of the invention. A method, a product or a use to which the invention is related, may comprise at least one of the embodiments of the invention described hereinbefore.
DETAILED DESCRIPTION OF THE INVENTION
In the following, the present invention will be described in more detail with exemplary embodiments by referring to the accompanying figures, in which
FIGS. 1 a -1 d are a series of figures schematically illustrating a method according to one embodiment of the present invention,
FIGS. 2 a -2 d are a series of figures schematically illustrating a method according to one embodiment of the present invention,
FIGS. 3 a -3 d are a series of figures schematically illustrating a method according to one embodiment of the present invention,
FIG. 4 is a flow-chart presentation of methods according to some embodiments of the present invention and
FIG. 5 is a flow-chart presentation of methods according to some embodiments of the present invention.
For reasons of simplicity, item numbers will be maintained in the following exemplary embodiments in the case of repeating components.
The flow-chart of FIG. 4 presents in more detail the process steps of the embodiments of the invention presented by the series of FIGS. 1 a -1 d and of FIGS. 2 a - 2 d.
FIGS. 1 a to 1 d schematically illustrate a fabrication process of a crystalline structure according to one embodiment of the present invention. Each figure presents a schematic cross sectional view of the template 1 and the substrate 2 supporting the template 1 , in one step of the manufacturing process. The order of the figures corresponds to the order of the process steps in the manufacturing process.
The first step S 1 in the embodiment shown by FIGS. 1 a to 1 d is to introduce a template 1 into a reaction environment. The reaction environment may possibly be also pumped into vacuum. After this, in step S 2 , the reaction environment is heated to a suitable process temperature, which also heats the template 1 and a supporting substrate 2 . The template 1 , placed in the reaction environment, is impregnated with one or more elements 3 in step S 3 . These elements 3 will constitute the crystalline structure 4 on the template at a later stage of the method. During this step S 3 , illustrated by FIG. 1 a , the template 1 is heated and exposed to the molecules or atoms of the element(s) 3 . The impregnation may be carried out by e.g. supplying the elements 3 in a gas flow in the reaction environment. Heating the template 1 increases the rate of diffusion of the elements 3 from the gas phase into the template 1 ( FIG. 1 b ). The template 1 in FIGS. 1 a -1 d is supported by a solid substrate 2 and the template 1 may be homogeneous or patterned.
As the template 1 is exposed sufficiently long to the gas-phase elements 3 , the template 1 may become saturated from the elements 3 at which point no more net diffusion of the elements 3 into the template 1 occurs. After the template 1 has been impregnated ( FIG. 1 b ), conditions in the reaction environment are altered (step S 4 ) such that the elements 3 inside the template 1 begin to migrate onto the surface of the template 1 ( FIG. 1 c ), i.e. the template 1 is “activated”. Suitable alterations in the conditions inside the reaction environment for the migration to take place include e.g. a decrease in the temperature of the template 1 causing supersaturation of the template 1 by the elements 3 , a decrease in the partial pressure of an element 3 in the reaction environment, or an increase in the temperature of the template 1 causing a thermally assisted chemical reaction to take place inside the template 1 . This chemical reaction may lead to segregation of the template 1 material releasing elements 3 from within the template 1 . It has surprisingly been observed that when the rate of migration is sufficiently small and the surface mobility of the elements 3 on the template 1 is sufficiently high the elements 3 prefer to self-organize in a two-dimensional crystalline surface structure 4 conforming to the shape of the template 1 (step S 5 and FIG. 1 d ). This occurs on the condition that the particular formed crystalline structure 4 has a local energy minimum in a two-dimensional configuration.
As the crystalline surface structure 4 conforms to the shape of the template 1 the aforementioned mechanism for the synthesis of a crystalline surface structure 4 enables controlling the size and shape of the resulting crystalline surface structure 4 by controlling the size and shape of the surface area of the template 1 . Additionally the disclosed method is particularly suitable for the fabrication of FCS-structures due to the fact that growth of the structure 4 takes place from within the template as opposed to conventional, possibly epitaxial, film deposition methods (e.g. CVD, MOCVD, sputtering, PVD etc.) in which a structure is synthesized on a substrate from the side of the environment, i.e. the structure is deposited on the substrate. By letting the elements 3 migrate onto the surface of the template 1 from within the template 1 , the formed crystalline structure 4 itself efficiently acts as a migration barrier against the elements 3 . This prevents buildup of the elements 3 onto the already formed crystalline surface structure 4 , which causes the thickness of the crystalline surface structure 4 to remain small, preferring a two-dimensional structure 4 . By suitably choosing the elements 3 , e.g. from the group of carbon, nitrogen and/or boron, such that the elements 3 are known to form crystalline structures 4 that have a local energy minimum in a two-dimensional configuration, MSC-structures of these elements 3 can be easily synthesized with the disclosed method.
FIGS. 2 a to 2 d schematically illustrate a fabrication process of a crystalline structure according to one embodiment of the present invention. Each figure presents a schematic cross sectional view of the template 1 and the substrate 2 supporting the template 1 , in one step of the manufacturing process. The order of the figures corresponds to the order of the process steps in the manufacturing process. The method schematically illustrated by FIGS. 2 a -2 d is different from the one illustrate by FIGS. 1 a -1 d in that an element 3 is supplied into the reaction environment as part of a precursor molecule 5 in step S 3 (FIG. 2 a ). The precursor 5 contains element 3 of the material of the crystalline surface structure 4 , for instance in liquid or gaseous state. Conditions in the reaction environment can be adjusted so that the precursor 5 reacts and/or decomposes in contact with the surface of the template 1 to release the element 3 at the interface between the reaction environment and the surface of the template 1 . When the precursor molecules 5 reach the heated reaction environment and decompose, the precursor molecules 5 release the element 3 that diffuses into the template 1 and impregnates it ( FIG. 2 b ). The template 1 may catalytically participate in the decomposition of the precursor 5 . The remaining part 6 of the precursor 5 molecule gets flushed away from the reaction environment through an output path. When e.g. the temperature of the reaction environment and the template 1 is subsequently altered (decreased or increased depending on whether a supersaturation or a chemical reaction possibly leading to segregation is targeted within the template 1 , respectively) in step S 4 the element 3 remaining inside the template starts to migrate towards the surface of the template ( FIG. 2 c ) forming a crystalline surface structure 4 (step S 5 , FIG. 2 d ), e.g. an FCS-structure, as discussed above.
FIGS. 3 a to 3 d schematically illustrate another fabrication process of a crystalline structure according to one embodiment of the present invention. Each figure presents a schematic cross sectional view of the template 1 and the substrate 2 supporting the template 1 , in one step of the manufacturing process. The order of the figures corresponds to the order of the process steps in the manufacturing process. In the FIGS. 3 a -3 d the template 1 is already impregnated with precursor molecules 5 upon insertion to the reaction environment ( FIG. 3 a ). The precursor molecules 5 in this embodiment may be understood as structural entitles inside the template 1 that comprise other molecules bonded to the elements 3 . When the reaction environment and the template 1 are heated the remaining part 6 of the precursor molecules 5 is released from the template 1 into the reaction environment leaving the elements 3 inside the template 1 ( FIG. 3 b ). When the temperature of the reaction environment and the template 1 is subsequently decreased the elements 3 remaining inside the template start to migrate towards the surface of the template ( FIG. 3 c ) forming a crystalline surface structure, e.g. an FCS-structure, as discussed above ( FIG. 3 d ).
In one embodiment of the invention fabrication of crystalline surface structures 4 thicker than one monolayer may be realized by staging the activation of the template 1 . In this embodiment e.g. multi-layered FCS-structures may be fabricated by causing a staged transport of the one or more elements 3 to the surface of the template 1 . For example, the temperature of an impregnated template 1 or the partial pressure of an element 3 in the reaction environment can be dropped in discrete steps, after each of which the template 1 becomes supersaturated and produces a single layer of FCS-structure on the template 1 ; once a layer is formed, the temperature is dropped again to form an additional atomic layer. This additional layer is formed in between the previously formed layer and the template 1 , the new layer causing the previous layer to move away from the surface of the template 1 . The staging can be continued until a desired number of layers is obtained, the template 1 is exhausted of an element 3 , or the mobility of an element 3 is too low to self-organize into additional FCS-structures on the template 1 . The flow chart of FIG. 5 illustrates an embodiment of the method where staging is used to fabricate two layers of FCS-structures. The method of FIG. 5 is identical to the method of FIG. 4 with the only difference being that steps S 4 and S 5 are respectively repeated in steps S 6 and S 7 to realize the staging.
In one embodiment of the invention the reaction environment may be e.g. a chamber comprising an input path for introducing the elements 3 or precursors 5 from their sources in a gas flow and onto the template 1 , and an output path connected to a vacuum pump for guiding the exhaust gases out of the reaction environment. The temperature, pressure and chemical composition of the reaction environment may be controlled by heaters, by the pumping speed of the pump, and by feeding of the elements 3 and/or other gases into the reaction environment.
The template 1 can be fabricated on a substrate 2 in many ways. It may be obtained e.g. as a part of a method according to an embodiment of the present invention, or the template 1 on the substrate 2 can alternatively be fabricated in advance as a step separate from the invention. A suitable template 1 can then be chosen for a specific application.
The template 1 can be formed e.g. by depositing the template material on the substrate 2 . The deposition can be performed, for example, by sputtering, by chemical vapor deposition (CVD) or by condensation. After deposition the template 1 may be patterned into a desired shape by common film patterning techniques such as chemical etching or laser patterning.
If required for some applications, the crystalline surface structure 4 , e.g. an FCS-structure, can be transferred to another substrate (a transfer substrate). To accomplish this, the template 1 , having a crystalline surface structure 4 grown on the interface of the reaction environment and the template 1 , is placed in close proximity to, or in contact with, a suitable transfer substrate. The initially obtained crystalline surface structure 4 can be homogeneous or inhomogeneous. It can e.g. be patterned, aligned and/or oriented and/or be of varying composition.
EXAMPLES
Example 1 pertains to graphene nanoribbons synthesized from a gaseous carbon precursor on an iron template 1 , according to one embodiment of the invention. In this example, iron is deposited on a substrate 2 by, for instance, sputtering in the desired pattern, for instance in a ribbon. The iron deposit template 1 on the substrate 2 is then placed in a reaction environment into which a gaseous carbon source, CO precursor in this case (an organic precursor or a hydrocarbon, such as alcohol vapor or methane are also suitable), is introduced. The conditions in the reaction environment are then modified by elevating the temperature such that the carbon element 3 from the carbon precursor is released from the precursor 5 and diffuses into the iron ribbon template 1 for a period of time, such that the template 1 becomes saturated with carbon. The carbon (the element 3 ) can be released in the gas phase and then diffuse or migrate into the iron deposit as would be the case for, for instance, methane. The carbon can also be released directly into the iron template 1 due to a catalytic decomposition of the precursor 5 at the surface of the iron template 1 , as is the case with, for instance, a CO precursor 5 . The iron template 1 can be saturated by a continued introduction of carbon. By changing a process parameter, such as lowering the temperature in the reaction environment which also lowers the temperature of the iron template 1 , supersaturation of the template 1 from the carbon element 3 is achieved. Once supersaturation occurs, the carbon migrates to the surface and begins to self organize in a complete or partial graphene layer 4 with the geometrical bounds of the iron template 1 thereby determining the geometrical bounds of the graphene layer 4 .
According to example 1 an FCS-structure 4 was produced by preparing an iron template 1 material approximately 10 microns wide, approximately 100 microns long and approximately 1 micron thick on a silicon or silica substrate 2 by traditional sputtering and lift-off techniques. The iron template 1 was then placed in a tubular furnace held at approximately 800° C. into which CO was introduced at a pressure of approximately 1 atm with a flow rate of CO of approximately of 0.1 liters per minute. The iron template 1 was held in the reaction environment (the tubular furnace) for approximately 10 minutes at the furnace temperature. The iron template 1 was then slowly cooled down by gradually withdrawing it from the heated zone or cooling the heated zone of the reactor so that the temperature of the template 1 dropped at a rate of approximately 1° C./sec until the substrate 2 was cooled down to approximately 25° C. During the cooling process an FCS-structure 4 conforming to the shape of the template 1 formed at the template-environment interface.
Also according to example 1, an FCS-structure 4 was produced by preparing an iron template 1 material approximately 10 microns wide, approximately 100 microns long and approximately 1 micron thick on a silicon or silica substrate by traditional sputtering and lift-off techniques. The iron template 1 was then placed in a tubular furnace held at approximately 800° C. into which methane was introduced at a pressure of approximately 1 atm with a flow rate of methane of approximately of 0.1 liters per minute. The iron template 1 was held in the reaction environment (the tubular furnace) for approximately 100 minutes at the furnace temperature. The iron template 1 was then slowly cooled down by gradually withdrawing it from the heated zone or cooling the heated zone of the reactor so that the temperature of the template 1 dropped at a rate of approximately 1° C./sec until the substrate 2 was cooled down to approximately 25° C. During the cooling process an FCS-structure 4 conforming to the shape of the template 1 formed at the template-environment interface.
Also according to example 1, an FCS-structure was produced by preparing a silica template 1 material approximately 10 microns wide, approximately 100 microns long and approximately 1 micron thick on a nickel substrate 2 by traditional silica growth and lift-off techniques. The silica template 1 was then placed in a tubular furnace held at approximately 600° C. into which acetylene and H 2 gases in equal amounts were introduced at a pressure of approximately 1 atm with a combined flow rate of the gases of approximately 0.1 liters per minute. The silica template 1 was held in the reaction environment (the tubular furnace) for approximately 20 minutes at the furnace temperature. The silica template 1 was then slowly cooled down by gradually withdrawing it from the heated zone or cooling the heated zone of the reactor so that the temperature of the template 1 dropped at a rate of approximately 1° C./sec until the substrate 2 was cooled down to approximately 25° C. During the cooling process a multi-layered FCS-structure 4 conforming to the shape of the template 1 formed at the template-environment interface.
Example 2 pertains to graphene nanoribbons synthesized from a cementite template 1 , according to one embodiment of the invention. In this example, a cementite template 1 is prepared on a substrate 2 by sputtering iron in the desired pattern, for instance in a ribbon, and converting the iron deposit into cementite by exposing the iron deposit to CO gas. The cementite template 1 is then placed in a reaction environment. The conditions inside the reaction environment are then modified by elevating the temperature of the reaction environment such that the carbon in the cementite is released from the template 1 by a chemical reaction causing segregation of the template material. The carbon then migrates onto the surface of the cementite template 1 and begins to self organize in a complete or partial graphene layer with the geometrical bounds of the cementite template 1 thereby determining the geometrical bounds of the graphene layer.
According to example 2 an FCS-structure 4 was produced by preparing an iron template material approximately 10 microns wide, approximately 100 microns long and approximately 1 micron thick on a silicon or silica substrate by traditional sputtering and lift-off techniques. The iron template 1 was then heated in a CO environment in a reaction chamber to approximately 650° C. for approximately 10 minutes to transform the iron template 1 into cementite. The CO gas was then flushed, for example, with argon or nitrogen, or evacuated from the reaction environment. After flushing of the CO the template 1 was heated and held for approximately 1 minute in approximately 750° C. to transform (segregate) the cementite into iron and carbon. During the transformation process an FCS-structure 4 conforming to the shape of the template 1 formed at the template-environment interface.
In the following the meaning for some of the terms used in this document is further clarified.
By a monolayer crystalline surface (MCS) structure is meant a graphene-like crystal having one or more layers largely in parallel to one another. The term FCS-structure (few-layered crystalline surface structure) is meant to include, but not be limited to, layers of two-dimensional crystals of carbon, boron, nitrogen and/or silicon containing sheets, filaments and/or ribbons and/or any other largely two-dimensional crystalline structures, where “few” preferably means a number between 1 . . . 10 layers.
By a template is meant a layer of material which can be used to activate material inside the template for forming crystalline surface structures so that the material self-organizes on the template-environment interface. A property of the template is that it maintains itself as a layer under the synthesis conditions for the crystalline surface structure and does not spontaneously form islands or droplets or otherwise significantly change its topology. In the case of a liquid or molten layer as a template, this implies that the layer is thick enough and the effective wetting angle is small enough such that surface tension does not favor or promote the separation of the layer into individual droplets so as to maintain a long radius of curvature for the surface of the template. The template can comprise, as an example only, transition metals such as iron, nickel or cobalt. Other materials, for instance, nitrides or carbides of transition metals such as cementite are also possible template materials. Such materials have an advantage in that they can withstand higher temperatures before a layer separates into droplets.
By a long radius of curvature is meant that the radius of curvature of the face of the template belonging to the template-environment interface is greater than approximately 30 bond lengths of the crystalline surface structure.
By the template-environment interface is meant the surface of the template which is in contact with the environment, e.g. the reaction environment.
By environment is meant the liquid, gaseous or vacuum environment in contact with the surface of the template.
By activation is meant that a material forming the crystalline surface structure (i.e. the element(s) 3 ) is released from the bulk of the template and migrates onto the surface of the template on the template-environment interface. The release can be obtained by, for instance, chemical reaction and/or supersaturation.
By a substrate is meant any desired substrate, which is suitable for a specific application. Examples of suitable substrates are numerous. A condition for the substrate used as the substrate for the template is that the substrate must withstand the conditions used for the synthesis of the crystalline surface structure on the template.
As is clear for a person skilled in the art, the invention is not limited to the examples described above but the embodiments can freely vary within the scope of the claims.
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A method for fabricating crystalline surface structures ( 4 ) on a template ( 1 ). The method comprises the steps of providing a template ( 1 ) into a reaction environment, wherein one or more elements ( 3 ) required for the formation of the crystalline surface structure ( 4 ) are contained within the template ( 1 ); heating the template ( 1 ) inside the reaction environment to increase the mobility of the element ( 3 ) within the template ( 1 ), and to increase the surface diffusion length of the element ( 3 ) on the template-environment interface; and activating the template ( 1 ) by altering the conditions within the reaction environment, to make the mobile element ( 3 ) slowly migrate towards the template-environment interface and to make the element ( 3 ) organize on the surface of the template ( 1 ) as a crystalline structure ( 4 ).
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This is a continuation of U.S. patent application Ser. No. 11/124,743, filed May 9, 2005, which is incorporated herein by reference in its entirety and to which priority is claimed.
FIELD OF THE INVENTION
[0002] Embodiments of this invention relate to delay- or phase-locked loops, and particularly to circuits of that type with increased stability.
BACKGROUND
[0003] It is often desired in an integrated circuit to delay a signal. In the context of a periodic signal like a clock signal, adjustment of delay can be understood as an adjustment of the phase of the signal. Such phase shifting of a clock signal can be achieved by use of delay lock loops (DLLs) or phase lock loops (PLLs) that are used to generate internal clock signals for an integrated circuit from a master clock signal. Because of the complexity of modern-day integrated circuits, the ability to finely shift the phase of clock signal is particularly important to ensure proper timing within the circuit. For example, DLLs or PLLs are used to set the data output timing in high speed Dynamic Random Access Memories (DRAMs).
[0004] A typical analog DLL 10 is shown in FIG. 1 . As shown, the DLL 10 derives an output clock signal (ClkOut) from an input clock signal (ClkIn), in which the phase between the two can be tightly controlled. The DLL comprises a variable delay line (VDL) whose delay (tVDL) is controllable given the analog value of a control signal (VDLctrl), and a fixed delay circuit, namely Delay Module (or DM). The output of the delay module (ClkOut_DM) and the ClkIn signals are compared at a phase detector (PD), which essentially determines whether one of the two input signals (ClkIn; ClkOut_DM) are lagging or leading the other, and seeks to bring these two phases into alignment. For example, if ClkOut_DM leads ClkIn, then the phase detector outputs a “down” signal (DN) to reduce the value of VDLctrl, which increases tVDL; if ClkOut_DM lags ClkIn, then the phase detectors outputs an “up” signal (UP) to increase the value of VDLctrl, which decreases tVDL. The bandwidth of the loop is determined in accordance with a loop filter (LF), which in an analog circuit can comprise resistor-capacitor circuits (e.g., an R-C filter). Moreover, and although not shown, the loop filter may comprise a charge pump. In any event, by virtue of the delay module, the output clock signal ClkOut will precedes the input clock signal ClkIn by its delay (tDM). Of course, the DLL circuit 10 , may also be digital in nature, with the loop filter being replaced by a digital control, and wherein VDLctrl comprises digital outputs to the VDL (not shown).
[0005] In general, and assuming the period of ClkIn is tCK, the loop in DLL circuit 10 establishes a relationship of tVDL+tDM=N*tCK, where N equals the smallest possible integer. Because tVDL is usually not larger than tCK, N is primarily determined by tDM, i.e., the delay through the delay module. Though tDM is a fixed value at given conditions, N is still variable inversely proportional to tCK.
[0006] When the delay of the delay module, tDM, is larger than the clock period, tCK, the transfer function of the loop increases in complexity, and instability can result, as will be shown below. Moreover, such problems are worse as the clock frequency increases (i.e., tCK decreases), or as tDM increases. Furthermore, because tDM can vary as a result of process, temperature, or voltage variations, such instability can be particularly hard to control from device to device.
[0007] FIGS. 2 and 3 shows Z-domain modeling of analog DLL circuit 10 with ( FIG. 2 ) and without ( FIG. 3 ) a delay module (DM). Kd is the gain for the VDL, and L(z) is the transfer function of charge pump and loop filter. The z −1 block represents the fact that the phase detector compares the current input clock edge with the VDL output derived from the previous input clock edge. In other words, the z −1 block represents one clock cycle delay (tCK). The DM, by contrast, is represented by a z −m block ( FIG. 3 ), meaning that the DM delays by m cycles.
[0008] As seen in the figure, the transfer function of FIG. 2 (without the delay module) is a first order system of z, and optimal parameters (Kd, R, C, etc.) for the circuit can be solved with ease. However, the addition of the delay module, as shown in FIG. 3 , causes a significant difference. Here, the resulting transfer function is represented by the (m+1)th order of z. It is very difficult to achieve an analytic solution such a high-order system.
[0009] As a result, and as alluded to above, a DLL circuit 10 with a relatively high tDM can be unstable, as shown in FIG. 4 . As shown, the total delay time of propagation through the loop, tLooP, is about four cycles for an example, and equals the sum of tF and tB, where tF equals the propagation delay though the phase detector (tPD) plus the propagation delay through the loop filter (tLF), and tB=the propagation delay through the VDL (tVDL) plus the propagation delay through the delay module (tDM) (i.e., tF=tPD+tLF; tB=tVDL+tDM). tVDL is generally not larger than tCK, and tF is usually negligible for an analog DLL design, and is shown exaggerated in FIG. 4 . (tF may however not be negligible for digital filters). In short, it is largely due to tDM that the delay through the loop can be longer than a single clock cycle.
[0010] In FIG. 4 , a timing error (tER) between ClkIn and ClkOut_DM is shown. Because initially ClkIn leads ClkOut_DM, UP pulses are needed to try and bring them into alignment. Each UP pulse increases an analog value of the VDL's analog control signal, VDLctrl, which decreases tVDL; each down pulse (DN) achieves the opposite effect. (Fixed pulse widths for UP and DN are assumed for simplicity of explanation).
[0011] However, notice that it takes significant time (i.e., tLooP) for the output of the phase detector (UP; DN) to take effect through the loop so as to update the phase at the input of the phase detector. In the mean time, before this change in phase is effected, the phase detector continues to generate the same signals (initially, UP in FIG. 4 ) and does so at every clock period, regardless of whether they are needed or not, and despite that the fact that any phase shift wrought by earlier signals is not yet known. Thus, in the example of FIG. 4 , four UP pulses are output before any change in phase (tER) is registered. This discrepancy in frequency between the clock frequency (1/tCK) and the loop frequency (1/tLooP) causes the loop to overreact and become unstable. Specifically, the timing error, tER, does not converge but oscillates. The amplitude and period of the oscillation depends on the loop gain and the loop delay (tLooP).
[0012] The conventional solution to this problem involved decreasing the loop's gain and/or reducing the loop's bandwidth. This can be accomplished by increasing loop filter's resistance-capacitance values (assuming an analog circuit), reducing the charge pumping current, or increasing the size of the loop filter. But these solutions can consumes larger layout areas and can considerably decreases the tracking bandwidth (i.e., loop gain divided by loop delay), resulting in a longer time to achieve a phase “lock.” In short, such previous approaches involved undesirable trade offs between maximum frequency performance, stability, tracking bandwidth, and layout area. A better solution is therefore needed.
SUMMARY
[0013] A method and circuitry for a Delay Locked Loop (DLL) or a phase Locked Loop (PLL) is disclosed, which improves the loop stability at high frequencies and allows maximum tracking bandwidth, regardless of process, voltage, or temperature variations. Central to the technique is to effectively operate the loop at a lower frequency close to its own intrinsic bandwidth (1/tLoop) instead of at the higher frequency of the clock signal (1/tCK). To do so, in one embodiment, the loop delay, tLoop, is measured or estimated prior to operation of the loop. The phase detector is then enabled to operate close to the loop frequency, 1/tLoop. In short, the phase detector is made not to see activity during useless delay times, which prevents the loop from overreacting and becoming unstable. Thus, a loop with the proposed method can operate stably at any frequency, and without increasing the loop filter resistance-capacitance values or decreasing loop bandwidth, such that tracking bandwidth and layout area are not sacrificed. In short, use of the disclosed technique requires no trade off between maximum frequency, stability, and tracking bandwidth.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] Embodiments of the inventive aspects of this disclosure will be best understood with reference to the following detailed description, when read in conjunction with the accompanying drawings, in which:
[0015] FIG. 1 illustrates a prior art delay locked loop (DLL) with a delay module among other components.
[0016] FIGS. 2 and 3 illustrate the transfer functions of the DLL of FIG. 1 with and without consideration of the delay module.
[0017] FIG. 4 illustrates instability and oscillation that can result in use of the DLL of FIG. 1 when long delays are used in the delay module.
[0018] FIG. 5 illustrates an embodiment of the improved DLL, including use of a phase detector controller.
[0019] FIG. 6 illustrates timing diagrams used during a measuring period, in which the loop delay for the improved DLL circuit of FIG. 5 is measured or estimated.
[0020] FIG. 7 illustrate timing diagrams for the DLL circuit of FIG. 5 , showing selective enablement of the phase detector in accordance with the loop frequency, and no oscillations or instabilities.
[0021] FIG. 8 illustrates an embodiment of the invention in the context of a phase-locked loop (PLL).
[0022] FIG. 9 illustrates exemplary circuitry for selectively enabling the phase detector using an enable signal (PDen).
DETAILED DESCRIPTION
[0023] The disclosed scheme uses smart filtering to remove the discrepancy between the loop frequency (1/tLoop; delay in propagation through the loop) and the higher clock frequency (1/tCK) by activating the phase detector to work at a rate closer to the loop frequency. FIG. 5 shows one embodiment for achieving this goal in the context of an improved analog DLL circuit 100 . However, the improvements are equally applicable when applied to digital DLL, or to PLL 100 ′ ( FIG. 8 ), which uses a variable oscillator (VCO) to generate a clock signal whose phase and frequency are locked to those of the input clock, ClkIn.
[0024] As shown in FIG. 5 , a phase detector control block, PDctrl 105 , has been added to the DLL circuit. It includes a counter 112 , register 114 , and a controller 116 which together are useful in measuring the loop frequency and ultimately in controlling the phase detector in accordance with the loop frequency.
[0025] In a preferred embodiment, the loop frequency, 1/tLoop, is measured prior to operation of the DLL circuit 100 . This is preferred, because the loop frequency can vary with process, voltage, and temperature variations, and can also vary in accordance with the input frequency. Thus, by measuring the loop frequency, a reliable value is acquired which is tailored to the unique environment in which the DLL circuit 100 is used. However, it is not strictly necessary in all useful embodiments to first measure the loop frequency prior to using the same to control the DLL circuit. Instead, if the loop frequency is known or otherwise ascertainable, it can merely be used without the measuring step.
[0026] FIG. 6 shows the timing diagrams used during the loop frequency measuring step. Basically, this step measures the time it takes for an input pulse (ClkIn) to pass through the loop. As shown, a measure signal is used to enable the measuring function. It is preferred during measuring that the phase detector and loop filter circuits ( FIG. 5 ) should be rendered transparent such that input signals received are merely passed to the outputs of these blocks. However, if this is not easy or practical, then the blocks can be by-passed altogether, such as with the use of transmission gates 110 . While by-passing the phase detector and loop filter will cause the measured delay through the loop to be slightly smaller than normal, such small skew in the measurement is satisfactory as the delays in the phase detector and loop filter (i.e., tF=tPD+tLF) are generally negligible (see FIG. 6 ). The measure signal can be self-generated by the PDctrl 105 block, or can be provided by another logic circuit such as a microcontroller which would normally be on the integrated circuit as the DLL circuit 100 .
[0027] Referring again to FIG. 6 , when the measure signal goes high, and after detecting a first ClkIn pulse, counter 112 start counting the number of subsequent ClkIn pulses up until the time that a pulse is detected at ClkOut_DM. After such detection takes place, the circuit waits for the next ClkIn pulse, taking this “last” ClkIn pulse as the end of the measuring period. Therefore, the measure signal can be disabled. As shown, the measured delay, tML, spans between the first and last ClkIn pulses in the measuring period, which is slightly longer than the actual loop delay, tLoop, but still comprises a useful measure of the loop delay (i.e., tML˜tLoop). In any event, the measured period can be viewed as a number of cycles of the input clock, m, which in the example of FIG. 6 equals 4 (i.e., m*tCk=tML˜tLoop). This measured value of m—the approximate ratio between the clock and loop frequencies—is stored in the register 114 for use in controlling the phase detector during normal operation of the DLL 100 , as is explained next with reference to FIG. 7 .
[0028] During normal operation, the phase detector is only enabled once during each period of the measured (or otherwise provided) loop frequency, i.e., once every tML. Specifically, 1/m controller 116 is used to process the input signal, ClkIn, by frequency dividing that signal by m, i.e., to remove all but every m-th pulse in the train to produce a phase detector enable signal PDen. (The controller 116 may also change the width of the ClkIn signal or its duty cycle). Thus, because m was measured to be four in FIG. 6 , it is seen in FIG. 7 that the PDen is high every fourth input clock pulse.
[0029] In any event, because the phase detector is only enabled at the times when PDen is high, an assessment of phase between ClkIn and ClkOut_DM, and subsequent output of an UP or DN signal, is affected only during those limited times, e.g., during windows 150 . Again, these windows 150 are assessed in accordance with the loop frequency (i.e., 1/tML˜1/tLoop), and not in accordance with the clock frequency (1/tCK) as in the prior art. This keeps the loop from overreacting, such as in FIG. 4 , where several UP signals were generated, and VDLctrl continually modified, before it was even assessed whether such phase adjustment control signals were warranted. As a result, and as shown in FIG. 7 , using the disclosed technique, the timing error, tER, will converge and not oscillate. (This assumes that the gain in the loop is not too large. The loop gain can be optimized, as one skilled in the art will appreciate, and in any event can be made higher than conventional loops not using embodiments of the disclosed invention). Thus, the effect of long delay through the delay module, tDM, are overcome by in effect measuring that delay as part of the loop delay, and taking that measured delay into account when generating control signals at the phase detector.
[0030] Selective enablement of the phase detector via the PDen signal can be achieved in several different ways, as one skilled in the art will appreciate. In one simple way, shown in FIG. 9 , the UP and DN signal outputs are grounded (via N-channel transistor 132 ) during those periods when PDen is not low, corresponding to a command that tVDL not be adjusted. During such time, connection of the circuits in the phase detector to the power supply voltage, Vdd, are disconnected (via P-channel transistors 130 ) to ensure no power-to-ground shorts.
[0031] It should be understood from this disclosure that frequency with which the phase detector is activated need not exactly match the loop delay. Thus, as shown in FIG. 6 , the loop delay, tLoop, is smaller than the measured value, tML, ultimately used to adjust the frequency of phase detector. This results due to the convenience of counting input clock pulses as an estimation of loop delay. In this regard, it should be understood that the frequency of the phase detector need (1/tML) only substantially correspond to the loop frequency (1/tLoop) in a preferred embodiment. In a less-preferred, but still beneficial embodiment, the phase detector is operated at a frequency which is somewhere between the clock frequency and the loop frequency. For example, suppose in FIG. 7 that the phase detector is enabled (via PDen) every other clock pulse (instead of every fourth as shown). Even thought this would amount to some, amount of overreaction of the loop—because not all phase adjustment commands will have had a chance to percolate through the loop to have effect before new commands are entered—the effect and stability of the loop will still be improved when compared with the prior art.
[0032] The measuring step can occur in an integrated circuit in which the DLL is used upon chip reset or initialization, or can be measured periodically during operation of the integrated circuit to ensure that the measured loop frequency is still optimal.
[0033] Although the disclosed phase detector has been shown separate from the loop filter, it should be understood that use of the term “phase detector” can comprise the loop filter aspects of the circuitry as well (if any).
[0034] While a preferred embodiment of the invention has been disclosed, it should be understood the circuitry used to affect the frequency conversion of the enablement of the phase detector can be achieved in many different ways. In short, it should be understood that the inventive concepts disclosed herein are capable of many modifications. To the extent such modifications fall within the scope of the appended claims and their equivalents, they are intended to be covered by this patent.
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A method and circuitry for a Delay Locked Loop (DLL) or a phase Locked Loop (PLL) is disclosed, which improves the loop stability at high frequencies and allows maximum tracking bandwidth, regardless of process, voltage, or temperature variations. Central to the technique is to effectively operate the loop at a lower frequency close to its own intrinsic bandwidth (1/tLoop) instead of at the higher frequency of the clock signal (1/tCK). To do so, in one embodiment, the loop delay, tLoop, is measured or estimated prior to operation of the loop. The phase detector is then enabled to operate close to the loop frequency, 1/tLoop. In short, the phase detector is made not to see activity during useless delay times, which prevents the loop from overreacting and becoming unstable.
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FIELD OF THE INVENTION
The invention relates to detection and identification of microorganisms, and in particular to detection and identification of microorganisms of the Mycobacterium tuberculosis (M.tb.) complex. This work was supported in part by grant No. CCR209585-01 from the Centers for Disease Control to John Chan.
BACKGROUND OF THE INVENTION
The Mycobacteria are a genus of bacteria which are acid-fast, non-motile, gram-positive rods. The genus comprises several species which include, but are not limited to, Mycobacterium africanum, M. avium, M. bovis, M. bovis-BCG, M. chelonae, M. fortuitum, M. gordonae, M. intracellulare, M. kansasii, M. microti, M. scrofulaceum, M. paratuberculosis and M. tuberculosis. Certain of these organisms are the causative agents of disease. For the first time since 1953, cases of mycobacterial infections are increasing in the United States. Of particular concern is tuberculosis, the etiological agent of which is M. tuberculosis. M. tuberculosis and other mycobacteria which are closely related to M.tb. (M. bovis, M. africanum, M. tuberculosis BCG and M. microti) are referred to as the TB complex mycobacteria. Many of these new cases of mycobacterial infection are related to the AIDS epidemic, which provides an immune compromised population which is particularly susceptible to infection by Mycobacteria. Mycobacterial infections other than tuberculosis are also increasing as a result of recent increases in the number of immune compromised patients. For example, Mycobacterium avium, Mycobacterium kansasii and other non-tuberculosis mycobacteria are found as opportunistic pathogens in patients infected with HIV as well as in in other immune compromised patients.
In recent years there has also been an increase in the number of clinical isolates of tuberculosis which are resistant to at least one of the antibiotics normally used to treat the disease (e.g., isoniazid, rifampin or streptomycin). Multidrug-resistant tuberculosis strains have emerged in several countries, resulting in a corresponding increase in the number of fatalities in both immunocompetent and immunocompromised individuals. Because M.tb. grows very slowly (doubling time 20-24 hrs.), conventional methods for identifying this organism and determining drug susceptibility require 2-18 weeks. During that time, patients are often treated empirically with antibiotics which may be ineffective, as lack of any treatment allows the patient to remain infectious and puts the patient and patient contacts at risk. Such empirical treatment can also exacerbate the development of drug resistance.
Conventional diagnosis of mycobacterial infections is dependent on acid-fast staining and cultivation of the organism, followed by biochemical and morphological assays to confirm the presence of mycobacteria and identify the species. These procedures are time-consuming, and a typical diagnosis using conventional culture methods can take as long as six weeks. Automated culturing systems such as the BACTEC™ system (Becton Dickinson Diagnostic Instrument Systems, Sparks, Md.) can decrease the time for detection of mycobacteria to one to two weeks. Once detected, culturing these slow-growing microorganisms in the presence of antibiotics to determine their drug susceptibility requires several additional weeks. There is still a need to reduce the time required for diagnosing mycobacterial infections and determining antibiotic susceptibility even further in order to allow prompt, informed treatment of M.tb. infections.
The BACTEC TB System provides one means for determining whether or not a positive mycobacterial culture is the result of TB complex mycobacteria or mycobacteria other than tuberculosis (MOTT). This is important information for the initial diagnosis of tuberculosis, and shortens the time required for determining the species present in a positive mycobacterial culture. The BACTEC identification scheme relies on a combination of three tests, namely, morphology on smear, growth characteristics and the NAP (p-nitro-α-acetylamino-β-hydroxy-propiophenone) TB differentiation test. NAP is an intermediate compound in the synthesis of chloramphenicol which markedly inhibits the growth mycobacteria belonging to the TB complex. MOTT show little or no growth inhibition, and any slight inhibition of growth is usually temporary. The mechanism of action of NAP on TB complex mycobacteria is not known, nor is the reason for its TB complex-specificity. When cultured in the presence of NAP, TB complex organisms show sharply reduced evolution of CO 2 , whereas MOTT continue to grow with increasing CO 2 production. The BACTEC TB System measures CO 2 evolution, as a "growth index" (GI) by monitoring production of 14 C -labeled CO 2 in cultures containing 14 C -labeled palmitate. Once a positive culture is obtained, speciation by determining growth (CO 2 production) in the presence of NAP generally requires an additional 4-6 days.
Luciferase is useful as a biological reporter or signal generating molecule because it catalyzes the reaction of luciferin with adenosine triphosphate (ATP), resulting in the production of light. Sensitive light-detection systems are available to detect and measure light (luminescence) generated by this reaction. Luciferase has been used for many years in the standard assay for measuring ATP. The cDNA coding for firefly luciferase (FFluc) has been cloned, which has allowed its use as a direct reporter molecule in a variety of transformed and transfected cells. In mycobacteria, FFluc has been inserted into the genomes of mycobacteriophage and into plasmids as a reporter gene for use in antibiotic susceptibility testing as an in vivo measure of cell viability after exposure to antibiotics. W. R. Jacobs, et al. (1993) Science 260:819 and WO 93/16172. Inhibition of culture growth results in reduced or absent light production from the cloned luciferase gene. This effect has been attributed to reduced amounts of ATP (required for the luciferase reaction) in antibiotic-sensitive cells, which exhibit reduced metabolic activity in the presence of an anti-TB antibiotic.
β-galactosidase is an enzyme which cleaves lactose into glucose and galactose. Other substrates for this enzyme are also known. X-gal (5-bromo-4-chloro-3-indolyl-β-D-galactoside) and chlorophenol red-β-D-galactopyranoside are colorimetric substrates for β-galactosidase. Enzymatic cleavage of X-gal produces a reaction product which is blue in color. Enzymatic cleavage of chlorophenol red-β-D-galactopyranoside produces a reaction product which is yellow to red in color. Methyl umbelliferyl-β-D-galactopyranoside is a fluorometric substrate for β-galactosidase which produces a fluorescent signal when enzymatically cleaved. This ability to produce a signal makes β-galactosidase useful as a reporter molecule in conjunction with colorimetric or fluorometric the enzymatic substrates, and these signal generating systems have been used in a variety of biological assays. Like FFluc, the bacterial gene which encodes β-galactosidase (LacZ) has been cloned and used as a reporter gene in recombinant organisms in both inducible and constitutive expression systems.
As used herein, the term "reporter gene" refers to a gene which can be expressed to produce a gene product which directly or through further reaction generates a detectable signal. This signal can be used to detect or identify cells carrying the gene, either on a plasmid or inserted into the genome of the cell. Examples of reporter genes are the gene encoding firefly luciferase (resulting in a luminescent signal upon reaction with luciferin) and the gene encoding β-galactosidase (resulting in a colored or fluorescent signal upon reaction with appropriate enzyme substrates). A mycobacteriophage carrying a reporter gene is referred to herein as a "reporter mycobacteriophage" or "RM." Mycobacteriophage carrying a luciferase reporter gene are referred to as "luciferase reporter mycobacteriphage" or "LRM." Mycobacteriphage carrying a β-galactosidase reporter gene are referred to as "β-galactosidase reporter mycobateriphage" or "β-GRM."
The host range of mycobacteriophage varies greatly, with some capable of infecting only a single species. Certain mycobacteriophage (e.g., TM4 or phAE40) have been characterized as preferentially infecting species of the TB complex, whereas others (e.g., L5) have a very broad range of mycobacterial hosts. A reporter mycobacteriophage constructed in TM4 or phAE40 would therefore be expected to be useful for specific identification of TB complex organisms, as primarily TB complex species should be infected and produce a signal. However, in practice, these mycobacteriophage are not perfectly species-specific, infecting and producing high levels of signal in certain MOTT species as well. This results in false-positives which are unacceptable for clinical detection and identification of TB complex mycobacteria. The present invention not only meets the need for a more rapid method for detection, identification and antibiotic susceptibility testing of TB complex organisms, it solves the problem of identifying false-positives and provides more accurate identification of TB complex organisms using a reporter mycobacteriophage.
SUMMARY OF THE INVENTION
The present invention uses luciferase reporter mycobacteriophage or β-galactosidase reporter mycobacteriphage and NAP to identify TB complex organisms and distinguish them from MOTT. As the mechanism of TB complex growth inhibition by NAP is not known, it was not known prior to the present invention whether NAP inhibition of bacterial growth would affect the production of light by LRM or affect the production of a reaction product by β-GRM. That is, it was not known prior to the present invention whether or not exposure to NAP would result in reduced production of light by a luciferase reporter mycobacteriophage and, if so, whether or not reduced light production could be used to distinguish TB complex organisms from MOTT. It was also unknown whether or not exposure to NAP would result in a reduction in β-galactosidase reaction products produced by β-galactosidase reporter mycobacteriophage and, if so, whether or not this response could be used to distinguish these species of mycobacteria. It has now been discovered that use of the luciferase reporter gene or the β-galactosidase reporter gene in place of CO 2 measurements in the conventional NAP identification system allows TB Complex vs. MOTT species identification in 48 hours or less. In many cases identification can be made in as little as 1-3 hours. The successful assays performed with these two reporter genes suggest that many of the reporter genes known in the art may be substituted in the RM/NAP assays of the invention with similar results.
Further, in conjunction with antibiotic susceptibility testing, the RM/NAP identification system the invention allows more information to be obtained from a determination of antibiotic susceptibility. Antibiotic resistant MOTT and antibiotic resistant TB complex organisms infected with RM both produce a positive signal when cultured in the presence of the antibiotic. However, a positive signal (e.g., luminescence from luciferin or a colored reaction product from a colorimetric substrate for β-galactosidase) which is due to an antibiotic-resistant TB complex organism is substantially reduced upon exposure to NAP, whereas antibiotic-resistant MOTT continue to produce a signal when treated with NAP.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing the time course of the reduction in luminescence of phage phAE42-12-infected M. bovis BCG in response to NAP treatment.
FIG. 2 compares the effect of NAP on luminescence generated by an LRM-infected TB complex species to luminescence generated by an LRM-infected MOTT species.
DETAILED DESCRIPTION OF THE INVENTION
The invention provides methods for clinical identification or antimicrobial susceptibility testing of M. tuberculosis and other TB complex organisms using a reporter mycobacteriophage assay and the differential effect of NAP on the growth of mycobacteria species. The inventive methods not only allow rapid identification of TB complex organisms, they distinguish between a false-positive signal arising from MOTT infected by the reporter mycobacteriophage and a true positive signal arising from phage-infected TB complex organisms. The methods may also be adapted to determine antibiotic susceptibility, distinguishing between a positive signal arising from an antibiotic-resistant TB complex organism and a positive signal arising from antibiotic resistant MOTT.
Applicants have for the first time demonstrated that NAP treatment can be used in a reporter phage assay to distinguish between TB complex organisms and MOTT. The mechanism of TB-complex-specific growth inhibition by NAP is not well understood, although it was previously known that growth inhibition was accompanied by reduced CO 2 evolution by cultures. Of significance to the present invention, however, is that it was not previously known whether or not NAP treatment would also selectively inhibit luminescence in TB complex organisms in an LRM assay, as several mechanisms of NAP-induced growth inhibition which would not affect the intracellular level of ATP could be hypothesized (e.g., cell surface effects, inhibition of transcription or translation factors, etc.). Whether or not NAP would inhibit processes necessary for the production of colored or fluorescent reaction products in the β-GRM assay was also unknown. It has now been discovered that mycobacteria cultured in a suitable liquid media can be treated with NAP in an amount sufficient to inhibit growth of TB complex mycobacteria, and detected in an LRM assay such as the assay described by W. R. Jacobs, et al. and in WO 93/16172, supra, to distinguish TB complex from MOTT organisms by reduction in luminescence. Alternatively, NAP inhibition of growth of TB complex organisms may be detected as reduced production of colored or fluorescent reaction products in a β-GRM assay.
The following discussion employs LRM as an example. However, it is equally applicable to β-GRM as well as other RM carrying other reporter genes. In the conventional LRM assay, mycobacterial cells are infected with the LRM and begin to synthesize luciferase by expression of the cloned gene carried by the reporter mycobacteriophage. Upon addition of luciferin, infected cells emit a signal (luminescence), whereas uninfected cells do not. Identification of the species of mycobacteria should therefore be possible by selection of a RM with the desired host range. However, the RM's currently available are not perfectly specific for the TB complex organisms. Although they do not infect all MOTT, many MOTT species produce high luminescence signals due to infection with "TB complex-specific" LRM such as those derived from TM4 and phAE40 . For example, luciferase reporter mycobacteriophage phAE42-12 is a mutant of phAE40 isolated for increased luminescence signal and deposited with the American Type Culture Collection (Rockville, Md.) on Feb. 7, 1995 as Accession Number ATCC 97046. phAE40 is a mutant derived from TM4, selected for broadened range of infection of TB complex organisms. Like its parent phage, phAE42-12 efficiently infects M. flavescens, M. smegmatis, M. intracellulare and M. chelonae and gives high luminescence signals. phAE42-12 generally does not infect M. fortuitum; M. gordonae, M. kansasii and M. xenopi, but certain strains of these species have been found which are inefficiently infected. Similarly, although many strains of M. avium do not support infection or are inefficiently infected, some strains have been found which are efficiently infected. Temperature may also affect the infection capability of mycobacteriophage. For example, phAE42-12 will infect M. fortuitum and M. gordonae at temperatures greater than about 37° C.
Treatment with NAP can reduce the luminescence signal 5-10 fold or more in TB complex organisms with little or no effect on the high levels of luminescence signal from LRM-infected MOTT, regardless of whether the infection is due to lack of infection specificity or is induced by higher temperatures. This differential effect has now been used to determine whether or not a positive signal in a reporter mycobacteriophage assay for TB complex organisms is indicative of a TB complex organism or MOTT. The invention therefore increases the utility of reporter phage constructions, as perfect infection specificity for the TB complex is no longer required for a useful clinical diagnostic test. Sometimes a minor reduction in the luminescence signal is seen initially in LRM infected MOTT treated with NAP, however, this reduction is less than 5-fold and the organisms often recover. Therefore, a substantial reduction in signal (defined as a reduction in signal of about 5-fold or more) is indicative of TB complex mycobacteria.
A typical assay for distinguishing species of mycobacteria according to the invention is performed as follows. Log phase cultures of the mycobacteria to be identified are exposed to NAP under conditions appropriate for continued growth of the culture. For mycobacteria, growth conditions are typically a liquid medium conventionally used for growth of mycobacteria (e.g., Lowenstein Jensen media, 7H9 or BACTEC liquid media) and an incubation temperature of about 37° C. The culture is exposed to an amount of NAP sufficient to inhibit growth of TB complex organisms if they are present. A NAP concentration of 0.5-100 μg/ml is typically sufficient to inhibit growth of TB complex mycobacteria. The culture may be infected with the RM either simultaneously with exposure to NAP, or the culture may be incubated for a period of time in the presence of NAP prior to infection with the RM. Typically, cultures are incubated in the presence of NAP for about 1-48 hours to ensure that growth of TB complex mycobacteria, if present, is inhibited. However, as illustrated in Example 2, the period of exposure to NAP in many cases may be as short as 1-3 hours. It is only necessary that the exposure to NAP be long enough to result in a detectable reduction in luminescence or β-galactosidase reaction product in TB complex mycobacteria in the RM assay. If the culture medium contains a detergent, the cells must be pelleted, washed and resuspended in a medium which does not contain a detergent prior to mycobacteriophage infection. The RM are then added to the culture (with NAP if the cells were not previously exposed) and incubated at about 35°-50° C. for a period of time to allow phage infection. Typically, about 1-5 hours is allowed for infection, however, the time for infection can be routinely optimized and adjusted for a particular RM/NAP assay system. The luminescence of LRM-infected cells is then determined upon addition of luciferin, measuring light emission in a luminometer. If a β-GRM is used, the colorimetric or fluorometric substrate is added and incubated with the β-GRM infected cells for a period of time sufficient for the enzymatic reaction to occur (typically several hours or overnight). The amount of the reaction product is then determined qualitatively or quantitatively. Colored reaction products may be detected, for example, visually or by optical density. Fluorescence may be detected, for example, visually or by instrumentation.
The above assay for distinguishing species of mycobacteria may be included in protocols for antibiotic susceptibility testing (AST) of mycobacteria to determine whether or not an antibiotic-resistant strain is an antibiotic-resistant TB complex mycobacterium or antibiotic-resistant MOTT. This allows identification of the mycobacterium at essentially the same time as its antibiotic susceptibility is determined. For example, a clinical specimen suspected of containing a species of mycobacteria may be cultured and then tested in parallel in the NAP RM assay of the invention and in an RM assay for antibiotic susceptibility, for example the LRM assay described by Jacobs, et al., supra. After culturing, several subcultures are prepared: 1) a subculture containing 0.5-100 μ/ml NAP, 2) at least one subculture containing an antibiotic (e.g., streptomycin, isoniazid, rifampicin or ethambutol), and 3) a control subculture containing neither antibiotic or NAP. After incubation of the subcultures for a period of time to allow NAP and the antibiotics to take effect, the control, NAP and antibiotic subcultures are infected with an RM as described above. Typically, the subcultures are infected about 48 hours after subculturing so that the NAP result and the antibiotic sensitivity result are available at approximately the same time. The luminescence of LRM-infected cells or reaction product produced by β-GRM infected cells is then determined as described above, and the signal in the NAP and antibiotic subcultures is compared to the uninhibited control. If signal is substantially reduced or absent in the NAP subculture, the mycobacterium present in the clinical sample is a member of the TB complex. If the RM signal is also reduced or absent in one or more of the antibiotic subcultures, that TB complex mycobacterium is also sensitive to the antibiotic present in the subculture or subcultures in which the signal is reduced or absent. If the RM signal is comparable to the control in the NAP subculture and reduced or absent in one or more of the antibiotic subcultures, the mycobacterium is a MOTT which is sensitive to the antibiotic present in the subculture or subcultures in which the signal is reduced or absent. Antibiotic-resistant TB complex mycobacteria produce levels of signal comparable to the control in the subculture(s) containing the antibiotic(s) to which they are resistant, but signal would be reduced or absent in the NAP subculture. Antibiotic-resistant MOTT produce levels of RM signal comparable to the control in the subculture(s) containing the antibiotic(s) to which they are resistant and in the NAP subculture. Of course, a microorganism may be resistant to one concentration of an antibiotic but sensitive at higher concentrations. The level of resistance or sensitivity may be determined by adjusting the concentration of antibiotic in the subcultures in the methods of the invention.
The effect of NAP on TB complex mycobacteria can be detected in the RM assay with 1-3 hours exposure to NAP, whereas longer exposure to the antibiotic (e.g., 48 hours) may be required to detect sensitivity or resistance. For this reason, it may be useful to first determine whether or not a clinical specimen contains TB complex mycobacteria using the NAP RM assay and subsequently determine antibiotic sensitivity if TB complex mycobacteria are found to be present. In this way, a clinician will know within a few hours whether or not clinically relevant TB complex mycobacteria are present in a specimen.
The invention improves RM assays by simplifying the interpretation of assay results for identification of mycobacterial species and significantly shortening the time required to obtain these results. The conventional BACTEC NAP identification system is not begun until the culture reaches GI 50, and then requires an additional 4-6 days to complete. Results may be obtained using the inventive methods in approximately the same amount of time as in probe-based hybridization systems for identification of mycobacteria (often 3 hours or less). In addition, antibiotic susceptibility testing (AST) using the RM/NAP methods of the invention provides a time savings of about 5-8 days (starting from BACTEC cultures) as compared to conventional BACTEC AST protocols. The conventional BACTEC AST is begun when the culture reaches GI 500 and then requires an additional 5-6 days to complete. Conventional AST on solid media requires even longer time periods than conventional BACTEC AST to obtain a result. In contrast, AST performed with the RM assay of the invention begins at GI <500 (typically GI less than about 250) and can be completed in 1-2 additional days.
EXAMPLE 1
Representative TB complex organisms (M. bovis bcg and M. tuberculosis strain 201) and various mycobacteria other than tuberculosis were differentiated using LRM detection with and without NAP treatment. The growth of the test mycobacteria on Lowenstein Jensen slants was standardized by inoculation into BACTEC liquid media, subculturing when necessary to obtain log phase cultures at moderate growth index (typically GI 100-300). BACTEC culture bottles containing 5 μg/ml NAP were prepared by addition of 0.1 ml of 200 μg/ml NAP to each 4.0 ml bottle. The organism to be tested was subcultured into BACTEC culture bottles with or without NAP by addition of 0.5 ml of the liquid culture to each bottle. Subculture bottles containing NAP were incubated at 37° C. for an additional 24-48 hours, monitoring GI daily. The luciferase phage assay was then performed using phage phAE42-12, comparing the luminescence signals obtained from infections of NAP treated organisms with untreated organisms, as follows.
After the NAP treatment period, media were removed and the organisms in each culture bottle were washed. Cells were pelleted by centrifugation at 1500 xg for 15 minutes at room temperature and resuspended in room temperature 7H9 medium (Difco) containing 0.2% glycerol and 10% ADC (5% albumin/2% dextrose/145 mM sodium chloride). The cells were washed a second time as before, resuspending the cells in a final volume of 350 μgl 7H9. To initiate infection, phage phAE42-12 were added in a volume of 7.5 μl to give 4×10 9 pfu/ml and incubated at 37° C. for 3 hours. The luminescence signal was measured after 3 hours of infection by transferring 100 μl of phage-infected cells to a luminometer cuvette and adding 100 μl of 1 mM luciferin in 0.1 M sodium citrate pH 4.5. Light emission was measured immediately after addition of these reagents, integrating the signal for 15 seconds. Luminescence was measured as the ratio of luminescence signal to background luminescence in uninfected cultures. A ratio of signal to background of 2 or greater is considered positive for light production by the LRM.
To assess the effect of temperature on the assay, similar experiments were performed with phage infection at 47° C. For several MOTT the signal was higher for infections at 47° C. as compared to infections at 37° C. NAP treatment had little effect on the luminescence signal generated by these organisms, regardless of the temperature of phage infection. However, the signal from untreated TB complex organisms was greatly reduced with infection at 47° C. as compared to untreated TB complex organisms infected at 37° C.
The luminescence signal from TB complex organisms was substantially reduced by more than 1 log by pretreating with 5 μg/ml NAP for 24-48 hours. For MOTT the signal was essentially unchanged by NAP pretreatment. The results are shown in the following Table:
______________________________________ NAP Exposure LuminescenceMycobacterium NAP 5 μg/ml (hrs.) (Signal/Background______________________________________TB COMPLEXTB201 - 24 27 + 3.9 - 48 32 + 1BCG - 48 5650 + 4BCG - 48 120 + 0.9BCG - 48 100 + 1.1BCG - 48 138 + 1.2BCG - 48 169 + 1.3BCG - 48 378 + 2.4MOTTxenopi - 24 1 + 1 - 48 1.9 + 1.1kansasii - 24 1.3 + 1.7 - 48 2.4 + 2.1avium 1546 - 24 1.3 + 1.4 - 48 5.6 + 4.2flavescens - 24 13 + 12 - 48 51 + 33smegmatis >37° C. - 24 580 + 1132 - 48 135 + 403fortuitum >37° C. - 24 57 + 96 - 48 221 + 184gordonae >37° C. - 24 42 + 50 - 48 146 + 164chelonae >37° C. - 24 1.2 + 1.1 - 48 1.24 + 1.25gastri #2978 - 48 9.9 + 10gastri #2977 - 48 2.1 + 2.0gastri #2973 - 48 5.3 + 3.3fortuitum 37° C. - 48 1.1 + 1.1gordonae 37° C. - 48 1.0 + 0.9smegmatis 37° C. - 48 67 + 34chelonae 37° C. - 48 1.9 + 2.6intracellulare - 48 37(Edgar B.) + 27intracellulare - 48 13(P-54) + 16______________________________________
As expected, M. fortuitum, M. gordonae, M. avium, M. kansasii and M. xenopi showed little or no infection by the LRM. Any low levels of luminescence detected in these species were essentially unchanged by treatment with NAP. MOTT strains which showed significant levels of infection by LRM were M. flavescens, M. smegmatis, M. chelonae, M. intracellulare, and M. fortuitum and M. gordonae at higher temperatures. The luminescence produced by these organisms was also essentially unaffected by treatment with NAP. In contrast, the luminescence signals of M. tuberculosis and M. tuberculosis BCG were high in the absence of NAP treatment but were substantially reduced to near or below 2 (an essentially negative signal/background) by treatment with NAP.
EXAMPLE 2
M. bovis BCG and phage phAE42-12 were used to measure the kinetics of the NAP effect on detection of TB complex organisms using LRM, comparing treatment with 5 μg/ml and 10 μg/ml NAP. Seven day roller bottle cultures of BCG were grown in 7H9 media containing 0.2% glycerol, 10% ADC and 0.01% TWEEN-80. The cells were washed twice in the same medium but without TWEEN-80 as described in Example 1. The cells were then diluted to a density of 10 7 cells/ml for phage infection. In some samples NAP was added at the same time as the phage for 3 hours. In other samples NAP was added before or after phage to obtain treatment times varying from 0-5 hours. All luminescence assays were performed as in Example 1 at 3 hours post infection. The results are shown in FIG. 1.
Three hours of NAP treatment, obtained by simultaneous addition of NAP and phage phAE42-12, was sufficient to reduce the luminescence signal more than 10 fold. However, the time course of reduction in luminescence shown in FIG. 1 indicates that the reduction in signal would be substantial and easily detectable in as little as 1 hour (about a 5-fold reduction). This rapid effect of NAP indicates that the method of the invention provides an identification test which can identify TB complex organisms in three hours or less with a simple workflow. This is in contrast to prior art methods in which the effect of NAP on culture growth is followed by monitoring CO 2 production, requiring 4-6 days for species identification.
EXAMPLE 3
The methods of the invention were used to distinguish between a TB complex species (M. bovis BCG) and a MOTT species (M. smegmatis) in about three hours. Seven day roller bottle cultures of these species were grown in 7H9 media containing 0.2% glycerol, 10% ADC and 0.01% TWEEN-80. The cells were washed twice in the same medium but without TWEEN-80 as described in Example 1. The cells were then diluted to a density of 10 7 /ml for phage infection. NAP (5 μg/ml) was added at the same time as phage. Luminescence assays were performed as in Example 1 at 3 hours post infection. The results are shown in FIG. 2. Luminescence in M. smegmatis was essentially unchanged in the presence of NAP, however, luminescence in M. bovis BCG was reduced about 14-fold, providing a clear distinction between the TB complex species and the MOTT species.
EXAMPLE 4
The FFluc gene of phAE40 (expressed from a heat shock protein "hsp" promoter) was removed and replaced with the β-galactosidase gene (LacZ) for use as a β-GRM in the NAP assay. This phage was identified as phAE40-LACZ. Colorimetric systems such as this are useful for situations in which instrumentation, such as a luminometer, is not readily available. Seven day roller bottle cultures of M. bovis BCG and overnight log phase cultures of M. smegmatis in 7H9 with 10% ADC and 0.01% TWEEN-80 were centrifuged to pellet the cells and washed twice with 7H9 medium. Assays were set up for each species at 10 8 cells/ml, 10 7 cells/ml and 10 6 cells/mi. These samples were infected with phAE40-LACZ at 2×10 10 pfu/ml, simultaneously adding 5 μg/ml or 10 μg/ml NAP. Infection was allowed to proceed for 2 hours at 37° C. Uninfected controls and infected controls without NAP treatment were also included in the analysis.
Following infection, X-Gal was added to a final concentration of 0.02% and the samples were incubated overnight to allow color development. The intensity of the blue color produced was evaluated visually and by reading absorbance at 620 nm (A 620 ). Inhibition of color development in the BCG samples was generally not as complete as inhibition of luminescence in the LRM assay. However, it was possible to differentiate BCG from MOTT visually, particularly at lower cell concentrations (10 6 cells/ml), where an estimated 4-5-fold reduction in signal was observed after treatment with either 5 μg/ml or 10 μml NAP. As cell concentration increased, the difference in color production between the two species became less distinct. The variable effect of NAP on culture growth depending on cell density ("inoculum effect") has been previously observed in other NAP assay systems, and is not believed to be due to any feature of this particular assay. Absorbance readings were also more variable than those obtained in the LRM assay, but the signal/background ratios were generally lower for BCG treated with NAP than for M. smegmatis treated with NAP.
The above experiment was repeated, substituting chlorophenol red-β-D-galactopyranoside for X-gal as the colorimetric enzyme substrate. Similar results were obtained, however, reduction in the reaction product could be detected in several hours. This substrate may therefore provide a more sensitive detection system than X-gal. It is expected that the β-GRM assay system cab be improved by further optimization of parameters such as the time of substrate addition, and the time and dose for NAP treatment. It is also expected that other colorimetric or fluorometric substrates for β-galactosidase may be routinely used in this assay to distinguish TB complex organisms from MOTT.
β-galactosidase is much more stable in the cell than luciferase, and it was therefore unexpected that a reduction in the amount of reaction product could be detected in this system within several hours of exposure to NAP. Further, the β-galactosidase signal generating system does not require ATP for signal production as luciferase does. It was therefore uncertain whether NAP treatment would result in a reduction in β-galactosidase reaction product at all. The discovery that two reporter genes with such different enzymatic mechanisms can be used in the RM assay of the invention suggests that the effect of NAP on growth of TB complex mycobacteria may affect multiple biochemical processes specific to TB complex organisms.
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Methods for using reporter mycobacteriophage (RM) and p-nitro-α-acetylamino-β-hydroxy-propiophenone (NAP) to identify TB complex mycobacteria and distinguish these species from MOTT. RM-infected MOTT show little or no reduction in signal when treated with NAP. In contrast, TB complex mycobacteria infected with RM are distinguishable from RM-infected MOTT by a reduction in signal with NAP treatment.
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BACKGROUND OF INVENTION
1. Field of the Invention
This invention is related to a light emitting diode (LED) device; more specifically it is related to a white LED package structure and its packaging methods.
2. Background Art
As a semiconductor lighting device, LED has superior advantages over traditional lighting devices, such as incandescent bulb and fluorescent tube, with a longer life time, a more compact size, a lower applied voltage source, no mercury pollution, and a more energy saving property. Therefore it is called the first option of the green lighting sources, and has already been widely used in signal light, display, and LCD backlighting. There is also a trend for the LED to replace the incandescent and fluorescent in general illumination area.
In a traditional method for making a white LED, the phosphor containing layer is directly dispensed onto and cover the surfaces of a blue or UV LED die so that the excited light from the phosphor with various wavelengths mixed together or mixed together with the excitation light if the excitation light is blue to create a white light emission. In this method, the LED suffers a great light absorption loss when the emitted light from the phosphor propagates backwardly into the LED die or to the substrate area around the LED die because of close proximity between phosphor and the LED die. An improving method is to separate the phosphor containing layer from the LED die by using a transparent spacer, such as a silicone, to reduce the chance of the excited emission from the phosphor to hit back into the LED die or the substrate area around the die. This has been described in the U.S. Pat. No. 5,959,316 as the prior art shown in FIG. 3 . In FIG. 3 , an LED die ( 60 ) is attached onto a substrate ( 62 , and the phosphor containing layer ( 66 ) is separated from the LED die ( 60 ) by using a transparent spacer ( 64 ); outside the phosphor containing layer ( 66 ) is a protective transparent layer ( 68 ). The LED die is electrically connected to the substrate ( 62 ) by using gold wires. In this structure, the emitted light from the phosphor layer in a back forwarding direction can still hit the LED die or the substrate area around the die without any obstacle, causing light absorption.
SUMMARY OF INVENTION
The present invention is to solve the above mentioned problem by providing a white LED package and its packaging method, which effectively prevents excited emission from phosphor from going back and hitting LED die and substrate area around LED die, hence enhances white lighting efficiency.
The technical solution is to use a low refractive index silicone (the second type of silicone encapsulant) to separate the phosphor containing layer from the first type of silicone encapsulant, which is used to cover the LED dies. As the refractive index of the phosphor containing layer is larger than that of the low refractive index silicone (the second type of silicone encapsulant), the light rays emitted by phosphor with an incident angle larger than the critical angle on the interface of the second type of silicone and the phosphor containing layer will be reflected and prevented from going backward to hit the LED die and the substrate area around the LED die, so that less absorption can be ensured and the overall white light output can be improved.
The multilayered encapsulation structure with top convex shape is formed by utilizing surface tension phenomenon that is enabled by the multi-ring structure with sharp edge of the leadframe package.
The effective reflective index of the phosphor containing layer is higher than that of the layer resides directly below the phosphor containing layer to reduce the amount light going backward to hit the LED die and the substrate area around the LED die. This thus reduces light absorption loss and improves light output.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic drawing of a cross-sectional view of a white LED package structure of the invention
FIG. 2 is a schematic drawing of a cross-sectional view of an alternative white LED package structure of the invention
FIG. 3 is a schematic drawing of a cross-sectional view of a prior art
DETAILED DESCRIPTION OF THE INVENTION
This invention is related to a light emitting diode (LED) device; more specifically it is related to a white LED package structure and its packaging methods.
The LED package of the invention has a multilayered encapsulation structure that is formed by utilizing surface tension method and leadframe structure providing surface tension phenomenon.
The LED package of the invention as shown in FIG. 1 comprises of metal electrodes 1 , a heat dissipation base 2 , a PPA plastic 3 to fix the metal electrodes 1 and the heat dissipation base 2 together, an LED die 4 , a die attach material 5 , gold wires 6 , silicone encapsulation layers 7 and 7 a , a phosphor containing layer 8 , an optical lens 9 , sharp edge ring-alike structures 11 , 12 , 13 , and 14 with a tilted inner surface, and ring-alike grooves 15 , 16 , and 17 formed between sharp edge ring-alike structures.
As shown in FIG. 1 , the LED die 4 is attached onto the heat dissipation base 2 by using a die attach material 5 , such as silver paste or solder, and electrically connected to the metal electrodes 1 by using gold wires 6 . The metal electrodes 1 , the heat dissipation base 2 , and the PPA plastic 3 for fixing the electrodes 1 and the heat dissipation base 3 together can be bound together by using injection molding method. The first ring-alike object with a tilted inner surface 11 as a part of the PPA 3 is located around the reflective cup of the heat dissipation base 2 , and forms an extended cup. The second ring-alike structure with a tilted inner surface 12 as a part of the PPA 3 is located around the first ring-alike structure with a tilted inner surface 11 , and separated from each other by a gap that forms the first ring-alike groove 15 . The third ring-alike structure 13 with a tilted inner surface as a part of the PPA 3 is located around the second ring-alike structure with a tilted inner surface 12 , and separated from each other by a gap that forms the second ring-alike groove 16 . The fourth ring-alike structure 14 with a tilted inner surface as a part of the PPA 3 is located around the third ring-alike structure with a tilted inner surface 13 , and separated from each other by a gap that forms the third ring-alike groove 17 .
The silicone encapsulation layer 7 completely covers the LED die and directly resides under the silicone encapsulation layer 7 a , which directly resides under the phosphor containing layer 8 . The phosphor containing layer 8 has a higher effective refractive index than the second type of silicone 7 a in the visible wavelength range of light. The optical lens 9 resides on top of the phosphor containing layer 8 .
The reflective index of the silicone material making the silicone encapsulation layer 7 a is chosen so that it is lower than that of materials used to make the silicone encapsulation layer 7 and the effective refractive index of the phosphor containing layer 8 .
The silicone encapsulation layer 7 is formed by dispensing liquid silicone material into the reflective cup of the heat dissipation base 2 and the above-mentioned extended cup. The top surface of the silicone encapsulation layer 7 can have a little convex shape that is formed by surface tension between silicone and the top sharp edge of the first ring-alike structure 11 .
The second silicone encapsulation layer 7 a can be achieved by dispensing liquid silicone material onto the silicone encapsulation layer 7 and be formed by the surface tension at the top sharp edge of the second ring-alike structure with a tilted inner surface 12 .
The phosphor containing layer 8 can be achieved by dispensing a silicone uniformly mixed with phosphor onto the silicone encapsulation layer 7 a and be formed by the surface tension at the top sharp edge of the third ring-alike structure with a tilted inner surface 13 . The phosphor containing layer 8 has a conformal shape at the bottom surface and the top surface of a convex shape formed by surface tension phenomenon. The phosphor containing layer 8 can also be pre-made by uniformly mixing the phosphor into a material chosen from glass, PC, PMMA, and silicone; The phosphor containing layer 8 can also pre-made onto a concave surface of an optical lens 9 .
There are several ways to make the LED package of the invention shown in FIG. 1 .
The first method of making the multilayered encapsulation structure is as follows. (A) The first silicone for making the silicone encapsulation layer 7 is dispensed into the reflective cup composed by the surfaces of the metal electrodes 1 , the heat dissipation base 2 , and the PPA plastic 3 , to cover the LED die 4 ; The dispensed silicone 7 spontaneously forms a convex lens surface by the surface tension at the top sharp edge of the first ring-alike structure with a tilted inner surface 11 ; The dispensed silicone 7 is solidified by using the method of heating or UV radiating. (B) A second silicone with the reflective index lower than that of the first silicone is dispensed onto the convex surface of the first silicone encapsulation layer 7 to form the second silicone encapsulation layer 7 a . The dispensed silicone 7 a spontaneously forms a convex lens surface by the surface tension at the top sharp edge of the second ring-alike structure with a tilted inner surface 12 ; The dispensed second silicone is solidified by using the method of heating or UV radiating. (C) A silicone uniformly mixed with phosphor is dispensed onto the convex surface of the silicone encapsulation layer 7 a , and is formed into a lens shape featured with a conformal concave inner surface and a convex outer surface by the surface tension at the top sharp edge of the third ring-alike structure with a tilted inner surface 13 . The dispensed phosphor-silicone layer 8 is solidified by using the method of heating or UV radiating. (D) Using a similar procedure, a clear silicone is then dispensed onto the convex surface of the phosphor containing layer 8 to form a convex and conformal concave optical lens 9 by utilizing the surface tension feature at the top sharp edge of the fourth ring-alike structure with a tilted inner surface 14 . The dispensed silicone is then cured by using the method of heating or UV radiating.
The second method of making the multilayered encapsulation structure is as follows. (A) The first silicone for making the silicone encapsulation layer 7 is dispensed into the reflective cup composed by the surfaces of the metal electrodes 1 , the heat dissipation base 2 , and the PPA plastic 3 , to cover the LED die 4 ; The dispensed silicone 7 spontaneously forms a convex lens surface by the surface tension at the top of the first ring-alike structure with a tilted inner surface 11 ; The dispensed silicone 7 is solidified by using the method of heating or UV radiating. (B) A proper amount of the second silicone 7 a is dispensed into the concave area of the pre-made phosphor containing layer 8 . (C) The phosphor containing layer 8 is reversed and put onto the convex surface of the silicone 7 . The dispensed silicone is solidified by using the method of heating or UV radiating to seal the phosphor containing layer 8 onto the silicone encapsulation layer 7 and form the second encapsulation layer 7 a . (C) Using a similar procedure, a clear silicone is then dispensed onto the convex surface of the phosphor containing layer 8 to form a convex and conformal concave optical lens 9 by utilizing the surface tension feature at the top sharp edge of the fourth ring-alike structure with a tilted inner surface 14 . The dispensed silicone is then cured by using the method of heating or UV radiating.
The third method of making the multilayered encapsulation structure is similar to the second method except that the phosphor containing layer 8 and the optical lens 9 are pre-made units and are joined together before putting onto the silicone encapsulation layer 7 .
The fourth method of making the multilayered encapsulation structure is similar to the first method except that the optical lens 9 is a pre-made unit and is putting onto the phosphor containing layer 8 by using the same steps for applying a pre-made unit onto the package as described in the second method.
FIG. 2 shows an alternative structure of white LED package of invention. The LED package of the invention shown in FIG. 2 is similar to the LED package structure shown in FIG. 1 except that the silicone encapsulation layers 7 and 7 a in FIG. 1 are combined into one layer of the same material in FIG. 2 and the effective reflective index of the phosphor containing layer 8 is higher than the reflective index of the silicone encapsulation layer 7 .
The method of making the multilayered encapsulation structure as shown in FIG. 2 is as follows. (A) The silicone encapsulation layer 7 is dispensed into the reflective cup composed by the surfaces of the metal electrodes 1 , the heat dissipation base 2 , and the PPA plastic 3 , to cover the LED die 4 ; The dispensed silicone 7 spontaneously forms a convex lens surface by the surface tension at the top sharp edge of the first ring-alike structure with a tilted inner surface 11 ; The dispensed silicone 7 is solidified by using the method of heating or UV radiating. (B) A silicone uniformly mixed with phosphor is dispensed onto the convex surface of the silicone encapsulation layer 7 , and is formed into a lens shape featured with a conformal concave inner surface and a convex outer surface by the surface tension at the top of the second ring-alike structure with a tilted inner surface 12 . The dispensed phosphor-silicone layer 8 is solidified by using the method of heating or UV radiating. (C) Using a similar procedure, a clear silicone is then dispensed onto the convex surface of the phosphor containing layer 8 to form a convex and conformal concave optical lens 9 by utilizing the surface tension feature at the top of the third ring-alike structure with a tilted inner surface 13 . The dispensed silicone is then cured by using the method of heating or UV radiating.
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A white light emitting diode (LED) package with multilayered encapsulation structure and the packaging methods are disclosed. The white LED package structure includes metal electrodes, a heat dissipation base, a PPA plastic for fixing the electrodes and the heat dissipation base together, at least one LED die, a die attaching material, gold wires for electrically connecting the LED die to the electrodes, a first type of silicone encapsulant, a second type of silicone encapsulant, and a phosphor containing layer. The invention utilizes a low-refractive index silicone (the second type of silicone encapsulant) to separate the phosphor containing layer away from the first type of silicone, which covers the LED die, to prevent/reduce emitted light going backward and hitting the LED die.
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CROSS-REFERENCE TO RELATED APPLICATION DATA
[0001] This application is a continuation of co-pending U.S. patent application Ser. No. 13/567,434 filed on Aug. 6, 2012, which in turn is a continuation of U.S. patent application Ser. No. 12/621,230 filed on Nov. 18, 2009, now U.S. Pat. No. 8,234,995 issued on Aug. 7, 2012, which claims the benefit of priority of Provisional U.S. Patent Application Ser. No. 61/122,471, filed Dec. 15, 2008, entitled, “GOAL TO GROUND MONITOR”, and all of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to a device for monitoring the present and past ground contact of moveable sport goals. In particular the invention relates a device to monitor the ground contact of soccer goals and to provide a visual indication of ground contact status of the goal.
[0003] Soccer is one of, and perhaps the most popular sport in the world. In some instances, soccer goals are fixed, or set securely (permanently or semi-permanently) into the ground. In other instances, soccer fields can be shared (e.g., also used as lacrosse fields), and as such the goals are moveable.
[0004] Typically, the goals are staked or anchored into the ground to secure the goals in place. However, at times, due to various reasons, the goals become un-staked and loose. This can cause a hazardous condition.
[0005] There is a danger of goals tipping over. Such tipping has resulted in numerous serious injuries, often of young children, with some victims as young as 3 and 4 years of age. Indeed, it is estimated that tipping over of goals results in between 90 and 200 serious injuries annually, and that such injuries can require hospitalization. Many of these injuries are to the brain and spine.
[0006] By its nature the goal is counter weighted by the base of the goal with most of its weight to the rear of the goal. However with some degree of force the goal can tip over. The force required to overturn a goal can be quite low. There are many reported instances where a goal has been overturned by wind alone. A small child climbing on the net or crossbar may also be sufficient to reduce the stability of the goal. Because of the weight of these soccer goals, averaging between about 150-500 pounds, the results of a goal striking a person can be devastating.
[0007] Maintaining these goals anchored to the ground would seem a manageable if not straightforward task. However, due to the sheer number of goals and the multi-usage of the fields, as well as other factors including, for example, changing soil conditions due to, for example, excessive rain or drought, this has proven a much more challenging and elusive task.
[0008] Accordingly, there is a need for a monitoring system that monitors change in a resting state of a ground resting goal, such as a soccer goal. Desirably, such a monitoring system is easily installed. More desirably, such a monitoring indicates minor movement of the goal from the safe or resting position and maintains such indication until reset. More desirably still, such a system provides ready visual indication of such an upset condition.
BRIEF SUMMARY OF THE INVENTION
[0009] A goal to ground monitor or indicator device indicates a ready and/or upset condition of a ground supported goal, such as a soccer goal, that has at least one bar that lies in contact with the ground. The monitor includes a base plate, a contact arm mounted to the base plate and movable relative to the base plate and an indicator arm mounted to the base plate for cooperation with the contact arm.
[0010] The contact arm and a portion of the base plate are configured for contact with the bar. That is, the bar overlies portions of the contact arm and base plate.
[0011] The indicator arm is mounted to the base plate for cooperation with the contact arm. The indicator arm is movable relative to the contact arm between a ready position and an upset position. The indicator arm is positioned such that a portion of the contact arm cooperates with a portion of the indicator arm to temporarily maintain the indicator arm in the ready position.
[0012] A biasing element, such as a spring, biases the indicator arm to the upset position.
[0013] The contact arm, resting in the base plate, cooperates with the indicator arm against the biasing element to maintain the indicator arm in the ready position when the bar overlies the contact arm. When the bar is moved from the contact arm, the spring exerts a force to move the indicator arm from the ready position, which moves the contact arm from the base plate to disengage the indicator arm and to continue moving the indicator arm to the upset position.
[0014] In an exemplary monitor, the contact arm and the indicator arm are pivotally mounted to the base plate. The pivot axis of the contact arm and the pivot axis of the indicator arm can be non-parallel, e.g., generally normal to one another or, alternately, they can be parallel to one another.
[0015] In one embodiment, the indicator arm includes a movable, biased finger configured to cooperate with the contact arm to maintain the indicator arm in the ready position. The contact arm includes a recess in a lower surface thereof such that in the ready position, the finger resides in the recess. A set lock can be provided on the contact arm that is movable between a first position in which the indicator arm is movable to the ready position with the contact arm resting in the base plate and a second position in which the set lock prevents movement of the indicator arm from the upset position into the ready position.
[0016] Indicator flag arms can be mounted to the indicator arm. The flag arms include a ready position flag arm and an upset position flag arm. The ready position flag arm can be green and the upset position flag arm can be red to provide readily visually perceptible indication whether an upset condition has occurred. The flag arms can include flags mounted thereto.
[0017] In an alternate embodiment, the contact arm and indicator arm include interfering portions configured to cooperate with one another. In this embodiment, in the ready position, the contact arm interfering portion overlies the indicator arm interfering portion to maintain the indicator arm in the ready position. After movement to the upset position, the contact arm interfering portion prevents resetting of the indicator arm without upward pivoting of the contact arm.
[0018] The base plate can be configured with one or more openings for securing the monitor device to the ground, such as by staking A cable and lock can be provided to present movement, vandalism or theft.
[0019] In still another alternate embodiment, a ground supported goal has an indicator device for indicating a ready and/or upset condition of the goal mounted directly to it. The goal includes at least one ground bar resting on the ground. The contact arm is operably mounted to the goal and is movable relative to the ground bar resting on the ground.
[0020] The indicator arm is operably mounted to the goal for cooperation with the contact arm. The indicator arm is movable relative to the contact arm between the ready position and the upset position. The indicator arm is positioned such that a portion of the contact arm cooperates with a portion of the indicator arm to temporarily maintain the indicator arm in the ready position.
[0021] A biasing element biases the indicator arm to the upset position. As such, the contact arm cooperates with the indicator arm against the biasing element to maintain the indicator arm in the ready position when the ground bar is on the ground. When the ground bar is moved off of the ground, the biasing element exerts a force to move the indicator arm from the ready position. This moves the contact arm to disengage the indicator arm and to continue moving the indicator arm to the upset position.
[0022] In a preferred alternate embodiment, the contact arm is pivotally mounted to the ground bar and the indicator arm is mounted to the ground bar and cooperates with the contact arm to maintain the indicator arm in the ready position.
[0023] These and other features and advantages of the present invention will be apparent from the following detailed description, in conjunction with the appended claims.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0024] The benefits and advantages of the present invention will become more readily apparent to those of ordinary skill in the relevant art after reviewing the following detailed description and accompanying drawings, wherein:
[0025] FIG. 1 is a front perspective view of a goal, such as a soccer goal, having a goal to ground monitor located at the rear ground bar or shoe, embodying the principles of the present invention;
[0026] FIG. 2 is a rear perspective view of the goal and the monitor;
[0027] FIG. 3 is a partial top view of the goal to ground monitor showing the indicator arm in the ready or seated position;
[0028] FIG. 4 is a partial top view of the goal to ground monitor showing the indicator arm in the upset or unseated position;
[0029] FIG. 5 is a partial top view similar to FIG. 4 with the indicator arm pivoting from the ready position to the upset position;
[0030] FIG. 6 is a partial top view similar to FIG. 5 with the indicator arm pivoted to the upset position;
[0031] FIG. 7 is a top rear perspective view illustrating the contact arm pivoted upwardly from the base plate and the indicator arm pivoted to the upset position;
[0032] FIG. 8 is a side view of the goal to ground monitor shown with the indicator arm in the upset position for ease of illustration;
[0033] FIG. 9 is a front perspective view of an alternate embodiment of a goal to ground monitor embodying the principles of the present invention;
[0034] FIG. 10 is a front perspective view of the alternate embodiment with the contact arm pivoted upwardly from the base plate and the indicator arm pivoting from the ready position to the upset position;
[0035] FIG. 11 is a front perspective view similar to FIG. 9 , but showing the indicator arm fully pivoted to the upset position;
[0036] FIG. 12 is a front perspective showing the contact arm pivoted upwardly from the base plate and the indicator arm pivoted to the upset position;
[0037] FIG. 13 is a partial top view of another alternate embodiment of the goal to ground monitor showing the contact arm having a parallel pivot axis and with the indicator arm in the upset position; and
[0038] FIG. 14 is an elevational illustration of another alternate embodiment in which the monitor is formed as part of or mounted to the goal.
DETAILED DESCRIPTION OF THE INVENTION
[0039] While the present invention is susceptible of embodiment in various forms, there is shown in the figures and photographs and will hereinafter be described a presently preferred embodiment with the understanding that the present disclosure is to be considered an exemplification of the invention and is not intended to limit the invention to the specific embodiment illustrated.
[0040] It should be further understood that the title of this section of this specification, namely, “Detailed Description Of The Invention”, relates to a requirement of the United States Patent Office, and does not imply, nor should be inferred to limit the subject matter disclosed herein.
[0041] Referring to the figures and in particular to FIGS. 1 and 2 , there is shown an embodiment of a goal to ground monitor 10 embodying the principles of the present invention. The monitor 10 is shown at the rear ground bar or rear ground shoe 12 (collectively, rear ground bar) of a soccer goal 14 . It will be appreciated that the goal to ground monitor 10 can be located along the ground bar or ground shoe 16 (collectively, ground bar), which is the bar that rests on the ground G and extends along the side of the goal 14 , rather than along the rear of the goal. For purposes of the present disclosure, reference to ground bar or rear ground bar is to any bar that forms part of the goal 14 structure, and rests on the ground G, whether such bar is along a side or along the rear of the goal 14 .
[0042] The monitor device 10 includes a base plate 20 that rests on the ground G, under the ground bar 12 , 16 . Preferably, the monitoring device 10 is positioned under the rear ground bar 12 . If it is positioned at the ground bar 16 (that is along a side of the goal 14 ), it is preferably located under a rear-most part of the bar 16 . This may be the case in those instances where there may not be a rear bar 12 or when positioning the monitor 10 at the rear bar 12 is not ideal. In that goals will typically tip by rotating about the front corners F of the goal 14 , it is preferable to locate the monitor 10 as far from the pivot point (axis A F ) as is reasonably possible, in that the farthest point moves the greatest distance when the goal 12 is tipped.
[0043] Referring to FIGS. 3-8 , the base plate 20 has mounted to it two pivoting elements 22 , 24 . The first element, or bar contact arm 22 , is pivotally mounted to the base plate 20 and, along with the plate 20 has a recess 26 , 28 formed therein, in which the ground bar 12 rests. The bar contact arm 22 pivots about an axis A 22 that is generally parallel to the ground bar 12 . In a present device 10 , the bar contact arm 22 pivots about a hinge pin 30 (see generally FIG. 7 ) that mounts the arm 22 to the base plate 20 . The contact arm 22 can be chamfered or tapered as at 32 to preclude binding of the arm 22 and to permit the arm 22 to freely pivot out of the resting or ready position (out of the base plate 20 ).
[0044] The contact arm 22 includes a set lock 34 . The set lock 34 is positioned on an upper surface 36 of the contact arm 22 and is slidable longitudinally (as indicated by the arrow at 38 ) along the contact arm 22 . The set lock 34 is lockable (or securable) in the extended or retracted position. The set lock 34 can include a shoulder bolt 40 or like fastener to facilitate securing it in the extended position. The contact arm 22 includes a ramped notch 42 that extends into the front face 44 and to the top surface 36 of the contact arm 22 . The set lock 34 is positioned over, e.g., covers, the notch 42 when the set lock 34 is in the extended position and uncovers the notch 42 when in the retracted position. A recess 46 is formed in a lower surface 48 of the contact arm 22 .
[0045] The second or indicator arm 24 is pivotally mounted to the base plate 20 , about a pivot axis A 24 that is generally normal (or perpendicular) to the contact arm axis A 22 and the ground bar 12 , 16 . The pivot 50 (the axis of which is indicated at A 24 ) of the indicator arm 24 can be mounted to the base plate 20 slightly offset from the contact arm 22 . The indicator arm 24 includes a finger 52 that extends outwardly to engage the contact arm 22 . The finger 52 is spring 54 biased to extend outwardly. Depressing the finger 52 against the bias moves the end of the finger 52 flush with the arm surface 56 .
[0046] A biasing element 58 is positioned to bias the indicator arm 24 to the upset position. In a present embodiment, the biasing element 58 is a spring that is positioned about the indicator arm pivot 50 , carried by the base plate 20 or positioned between the arm 24 and the base plate 20 . In a present monitor, the spring 58 is a coil spring and both ends 60 , 62 of the spring 58 are positioned to urge the indicator arm 24 to the upset position.
[0047] Two flag arms 64 , 66 are mounted to the indicator arm 24 . The arms 64 , 66 can be colored and can include a visual indicator such as a red flag 68 that is oriented upward to indicate the upset position and a green flag 70 that is oriented upward to indicate a ready position. A present monitor 10 includes a red flag 68 having an octagonal shape to indicate the upset condition and a green banner-like flag 70 to indicate the ready condition. In the illustrated monitor 10 , the flag arms 64 , 66 are formed with spring or resilient base sections 72 and the arms 64 , 66 themselves are coated 74 , as with a plastic coating, which can also be colored, to enhance durability and visual perception.
[0048] The base plate 20 can include openings 76 to permit the monitor 10 to be affixed to the ground G. The monitor 10 can be affixed by use of stakes, coil-like augers, corkscrew-like augers/elements or the like (not shown). The monitor 10 can include locks or locking elements so that the monitor 10 can be locked to the goal 14 . As illustrated, one suitable lock is a cable lock 78 that is affixed to the base plate 20 and looped over the ground bar 12 , 16 to secure the plate 20 to the ground bar 12 , 16 , to prevent removal, vandalism or theft of the monitor 10 . The cable 78 can be secured to the base pate 20 by a key lock 80 .
[0049] In use, the contact arm 22 is pivoted up and the indicating arm 24 is pivoted down (to the ready position). The contact arm 22 is then pivoted down into the ready position, with the finger 52 positioned in the recess 46 in the bottom 48 of the contact arm 22 . The monitor 10 , which is now in the ready position, is positioned beneath the ground bar 12 , 16 .
[0050] It will be appreciated that setting the monitor 10 can be difficult given that it is located beneath the ground bar 12 , 16 . Accordingly, the set lock 34 permits the monitor 10 to be set or reset without the need to remove the monitor 10 from under the ground bar 12 , 16 , or even lift the ground bar 12 , 16 . In this manner, the set lock 34 can be moved to the refracted position which exposes the ramped notch 42 . As the indicator arm 24 is pivoted to the ready position, the finger 52 engages the ramped notch 42 . In that the finger 52 is biased, as the arm 24 is rotated toward the ready position, the finger 52 is urged inward as it moves along or through the notch 42 , to allow the indicator arm 24 to pivot fully. Once the indicator arm 24 passes the point at which the finger 52 is beyond the contact arm 22 , that is, once the finger 52 enters the recess 46 , the spring 54 bias forces the finger 52 outward and the finger 52 engages the contact arm 22 , setting the indicator arm 24 in the ready position. The set lock 34 can then be moved and secured into the extended position by, for example, tightening down the fastener 40 .
[0051] It will be understood that when the goal to ground monitor 10 is in place under the ground bar (whether it is the rear ground bar 12 or one of the side bars 16 ), the spring 58 force on the indicator arm 24 induces an upward force on the contact arm 22 . However, the weight of the goal 14 maintains the contact arm 22 down on the indicator arm 24 and base plate 20 . When, for example, the goal 14 lifts off of the ground G, if the goal 14 pivots forwardly, the spring force from the indicator arm 24 forces the contact arm 22 to pivot upwardly (by engagement of the finger 52 with the contact arm recess 46 edge) so that the finger 52 forces the contact arm 22 to pivot up. As the two arms 22 , 24 pivot upwardly and the finger 52 disengages from the recess 46 . The indicator arm 24 then pivots by force of the spring 58 to the upset position, indicating that some upset has occurred and that the goal requires attention.
[0052] It will be appreciated that the set lock 34 prevents the indicator arm 24 from being rotated back toward the ready position and being “reset” without purposefully moving the set lock 34 from the extended position to the retracted position. Thus, if the indicator arm 24 signals some upset position, there must be some purposeful action taken to reset the arm 24 to the ready position.
[0053] An alternate embodiment of the goal to ground monitor 110 is illustrated in FIGS. 9-12 . In this embodiment, in order to assure that a goal 14 that has moved into an upset position or condition is properly indicated and checked (by an individual), the indicator arm 124 , once moved into the upset position, cannot be rotated back into the resting position without fully resetting the monitor 110 . That is, once the indicator arm 124 has pivoted out from under the contact arm 122 , in order to reset the monitor, the contact arm 122 must be pivoted upwardly, the indicator arm 124 reset to the ready position, and the contact arm 122 brought back onto the indicator arm 124 .
[0054] Accordingly, the contact arm 122 and indicator arm 124 include interfering portions that overlap. The contact arm interfering portion 146 prevents the indicator arm 124 (interfering portion 152 ) from fully seating in the base plate 120 if not properly reset. The interfering portions 146 , 152 include curved and/or angle surfaces 148 , 154 that cooperate to permit the contact and indicating arms 122 , 124 to readily slide along and move past one another when the arms 122 , 124 move from the ready to the upset position. The interfering portions 146 , 152 , however, prevent the indicating arm 124 from merely being pivoted to the ready position, without first lifting (pivoting) the contact arm 122 .
[0055] Still another alternate embodiment of the monitor 210 is illustrated generally in FIG. 13 . In this embodiment, the indicator arm 224 pivots as in the prior embodiments (that is about an axis A 224 that is generally parallel to the ground bar). The contact arm 222 , however, also pivots about an axis A 222 that is parallel to the ground bar (more specifically, parallel to the axis A 224 about which the indicator arm 224 pivots). The axes A 222 , A 224 are parallel, but preferably are not collinear; that is, they do not share the same axes. And, the location at which the arms 222 , 224 , engage one another, as indicated generally at 226 , whether it is by a finger and recess (not shown) or cooperating angled/curved surface (not shown), is preferably spaced from (e.g., not collinear with) the indicator arm and contact arm axes A 222 , A 224 . It will be appreciated that such a configuration provides the desired moment, e.g., distance between the engagement point 226 and the rotational axis A 224 , to establish both force and distance to urge the indicator arm 224 to the upset position.
[0056] Still another embodiment 310 is illustrated in FIG. 14 in which the contact arm 322 , when the monitor 310 is in the ready position, remains in contact with the ground G and remains in contact with or closely adjacent to the ground bar 12 , 16 . In this embodiment, the contact arm 322 is biased away from the ground bar 12 , 16 by spring 358 . The indicator arm 324 is held in the ready position by engagement with the contact arm 322 when the contact arm 322 is “sandwiched” between the ground bar 12 , 16 and the ground G.
[0057] As the goal 14 lifts from the ground G, the spring 358 bias urges the contact arm 322 away from the ground bar 12 , 16 . This releases or disengages the indicator arm 324 (disengage the indicator arm 324 from the contact arm 322 ). As with the prior embodiments 10 , 110 , 210 , in this embodiment 310 , the indicator 324 arm is in the ready (green) position when the indicator arm 324 is secured by the contact arm 322 and moves (pivots) to the upset position as it is released from engagement with the contact arm 322 . The contact arm 322 and indicator arm 324 can both be mounted to the ground bar 12 , 16 by pivot arrangements 330 , 350 , respectively.
[0058] It will be appreciated that the monitor 10 , 110 , 210 , 310 is of a fail-safe design. That it, because the indicator arm 24 , 124 , 224 , 324 fails to the upset position, the monitor 10 , 110 , 210 , 310 will indicate upset even if a true upset condition may not have occurred. Moreover, the upset position can be indicated even if, for example, the spring 58 , 158 , 358 fails, by weighting the indicator arm 24 , 124 , 224 , 324 or flags 68 , 70 , or by incorporation of an additional (fail-safe) spring element in the monitor 10 , 110 , 210 , 310 (which the two ends 60 , 62 of the spring 58 , 158 , 358 can be used to effectuate).
[0059] All patents referred to herein, are hereby incorporated herein by reference, whether or not specifically done so within the text of this disclosure.
[0060] In the present disclosure, the words “a” or “an” are to be taken to include both the singular and the plural. Conversely, any reference to plural items shall, where appropriate, include the singular.
[0061] From the foregoing it will be observed that numerous modifications and variations can be effectuated without departing from the true spirit and scope of the novel concepts of the present invention. It is to be understood that no limitation with respect to the specific embodiments illustrated is intended or should be inferred. The disclosure is intended to cover all such modifications as fall within the scope of the claims.
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A device indicates a ready and/or upset condition of a ground supported goal such as a soccer goal that has at least one bar that lies in contact with the ground. An indicator arm is movable relative to the contact arm between a ready position and an upset position. A contact arm cooperates with. A biasing element biases the indicator arm to the upset position. When the bar of the goal is no longer in contact with the ground the indicator arm moves from the ready position to the upset position.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to an air cleaning and circulating apparatus of the hassock fan type which contains negative ion generators and a charged filter to treat and circulate air.
2. Description of the Prior Art
There are a multitude of devices available that are used to clean and circulate air. One such device uses a high voltage negative ion generator in combination with a positively charged collector plate, the ion generator producing a fountain of ions around the device. As there is no air behind the ions they are not evenly distributed throughout the room and being negatively charged are attracted to walls, rugs and curtains, which are positively charged and therefore cause these areas to become dirty at a rate faster than normal. In addition, the collector plate is inefficient as it does not remove a large portion of the charged particles.
The use of fans of the hassock type to circulate air is well known, such fans are very efficient in high volume air circulation due to their 360° radial air flow at high volume levels which can be in the range of 400 to 600 CFM.
Due to this high volume air movement in hassock fans, filters of the mechanical type in combination with a hassock fan, which would filter 90% of the particles from the air are impractical. The impracticality results from the restriction in discharge air flow that is necessary to provide high efficiency, which restrictions would result in a typical air flow drop from 400 CFM to 100 CFM. This air flow problem would also be apparent in other fan filter configurations due to the flow restrictions necessary to achieve a high level of filtering efficiency.
The U.S. Pat. No. 2,431,724, to Adyt shows a vertical axis fan which has an ozone unit in its base, and which provides for air circulation but does not contain filtering media.
The U.S. Pat. No. 3,747,300, to Knudson shows a portable electrostatic air cleaner with three filter elements, which are a mechanical filter, an electrostatic filter, and an activated charcoal filter, and which also suffers from the problems described above.
The U.S. Pat. No. 3,716,966, to De Seversky illustrates a vertical axis hassock type fan, which is surrounded with a wet electrostatic precipitator, and which provides a complicated structure that requires frequent maintenance, and does not provide the desired high air flow.
The U.S. Pat. No. 3,783,588, to Hudis illustrates the use of an electrostatically charged air filter for air filtration, the filter being provided with openings for air flow and which may be mounted in combination with an axial type fan. The Hudis structure is fragile, complicated and does not provide a high rate of air flow.
The structure of my invention provides for efficient air filtration at a high air flow rate and provides a well distributed stream of negative ions.
SUMMARY OF THE INVENTION
In accordance with the invention, air cleaning and circulating apparatus is provided that includes a hassock type fan, with negative ion generators in the intake air stream, adjacent to a charged filter to attract negatively charged particles in the air, and negative ion generators to provide negative ions in the discharge air stream.
The principal object of the invention is to provide an air cleaning and circulating apparatus which provides a high rate of flow of filtered air.
A further object of the invention is to provide apparatus of the character aforesaid which is simple to construct but sturdy and reliable in operation.
A further object of the invention is to provide apparatus of the character aforesaid that is economical to operate.
A further object of the invention is to provide apparatus of the character aforesaid that operates at low voltages.
A further object of the invention is to provide apparatus of the character aforesaid which provides a stream of negative ions in the discharge air stream that are effectively distributed for beneficial use.
A further object of the invention is to provide apparatus of the character aforesaid which can be used as a fan alone, or in combination as a fan and filtering apparatus.
Other objects and advantageous features of the invention will be apparent from the description and claims.
DESCRIPTION OF THE DRAWINGS
The nature and characteristic features of the invention will be more readily understood from the following description taken in connection with the accompanying drawings forming part hereof in which:
FIG. 1 is a view in perspective of the apparatus of the invention, with a portion removed to show the details of construction;
FIG. 2 is a side elevational view of the apparatus of FIG. 1, with a portion removed to show the interior construction;
FIG. 3 is a view similar to FIG. 2 with additional portions removed to show additional interior construction details;
FIG. 4 is an exploded perspective view, enlarged, showing details of the apparatus filter;
FIG. 5 is a fragmentary perspective view of the apparatus of FIG. 1 with the top removed to show details of the interior construction;
FIG. 6 is a fragmentary perspective view, enlarged, of one of the ion generators of the apparatus; and
FIG. 7 is an electrical circuit diagram illustrating the electrical circuitry associated with the apparatus of the invention.
It should, of course, be understood that the description and drawings herein are illustrative merely, and that various modifications and changes can be made in the structure disclosed without departing from the spirit of the invention.
Like numerals refer to like parts throughout the several views.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now more particularly to the drawings and FIGS. 1 to 6 thereof, the apparatus 10 of the invention is there illustrated, and includes, a base 11 of circular raised dish shape, with slots 12 therethrough, and which is provided with a plurality of feet 13, four being shown to raise it off the floor (not shown) and permit air to flow through slots 12.
The base 11 has an electric motor 18 of well known type mounted thereto by bolts 19 and has a shaft 20 extending vertically upwardly with a fan 21 mounted thereto by retainer 23, and which fan 21 has blades 22. The motor 18 is connected to wire 28 and by wires (to be described) to a speed reduction device 27 of well known type.
The base 11 has vertical ribs 30 attached thereto around it periphery above and at feet 12 by screws (not shown), four ribs being shown, which have a cone 31 attached thereto at the top by bolts 32. The cone 31 has the speed reduction device 27 and a power supply 34 secured thereto in well known manner.
The cone 31 has two negative ion generators 36 attached thereto on opposite sides adjacent the center thereof on the underside 33 of cone 31, which include ion emitter heads 35 of well known type, and which are engaged in grommets 37 mounted in the cone 31.
The negative ion generators 36 are upstream of a filter 38 which filter includes a plurality of filter packs 40, four being shown.
The filter packs 40 are of segmented configuration each with a frame 41, a foam pre-filter 42 of well known type, an electrically charged filter element 43 and a retainer 44.
The charged filters 43 as illustrated are of the electrete or pre-charged type available from Minnesota Mining and Manufacturing Co. (3M), Minneapolis, Minn.
The filter 43 can also be of the type that is naturally positively charged, with an uninduced charge so that negatively charged particles are attracted to it. If desired the filter element 43 could be of the conductive charge type made from materials such as carbonized foam, or metal screen to which a charge is applied during operation and which would provide a filter with greater particle attraction and which is washable. The charged filter 43, as illustrated, must be periodically checked and replaced by the user when it becomes dirty. The frames 41 of filter packs 40 each has a hook 45, and a snap member 46 to engage adjacent ribs 30 for retention thereto.
The ribs 30 have side panels 47 and 48 engaged therewith and retained thereto by screws 49. The base 11, ribs 30, cone 31 and side panels 47 and 48 are of molded plastic construction. The side panels 47 and 48 have ribs 49a with slots 50 therebetween to permit air to pass into the interior of apparatus 10. The panels 47 and 48 can be detached from ribs 30 to permit access to the interior of apparatus 10 by removing the screws 49, as desired.
The cone 31 on the underside 33 has an additional pair of negative ion generators 54 mounted thereto on opposite sides thereof adjacent outermost rim 55 of cone 31 but downstream of filter 38 in the discharge air stream. The generators 54 include ion emitter heads 56 of well known type, which are engaged in grommets 57 mounted in the cone 31.
The apparatus 10 also includes a top panel 60 which fits over the cone 31 and is secured thereto in well known manner.
Referring now also to FIG. 7, the circuit diagram includes wires 28 and 29 connected to a source of electrical power (not shown), wire 28 is also connected to an on-off switch 70 of well known type which has a rocker 71 to close a circuit through contacts 72 and 73, and through wire 74 provides electrical power to the power supply 34 which is connected to wire 29.
The switch 70 has a lamp 80 of well known type therein also activated by closing of contacts 72 and 73. The power supply 34 has wires 81, 82, 83 and 84 attached thereto, wires 81 and 82 extending to the upstream negative ion generators 36, and wires 83 and 84 extending to the downstream negative ion generators 54.
The speed reduction device 27 includes a multi-position switch 85, with three positions shown, respectively connected by wires 86, 87 and 88 to the motor 18 in well known manner.
The mode of operation will now be pointed out.
When it is desired to use the device as a fan only, the speed is selected by adjusting switch 85 and motor 18 will operate, turning fan 21 with air drawn in through the side slots 50 and through slots 12 in base 11. The air passes upwardly through the filter packs 40 and some filtration is achieved by foam prefilter 42 and filter 43 before the air is discharged between the top 60 and the side panels 47 and 48.
When it is desired to utilize the ionization feature, the switch 70 is activated so that electrical power from power supply 34 causes the ion generators 36 and 54 to emit negative ions. The air drawn in through the slots 12 and side slots 50 of panels 47 and 48, is ionized upstream of filter 37 by ion generators 36 and the air and negatively charged particles are passed through filter packs 40 where the negatively charged particles are attracted to the charged filter 43, retained thereon and relatively particle free air is discharged with the ion emitters 54 placing negative ions in the discharge air stream.
Tests have shown that because of the placement in the air stream of the filter 38 and the use of ionization generators 36 upstream of the pre-charged filter 43 there is much less air loss than if 100% of the air were drawn through the filter 43. This results, as air is drawn over, as well as through the filter 38, and particles are removed from the air through electrical attraction both as they pass over and through the filter. Tests have shown filtration is 40% efficient on particles down to 0.5 microns in size, and with a total air delivery of 400 CFM, the clean air delivery is approximately 160 CFM. The air is refiltered approximately 5 times an hour in an average sized room. Testing has also shown that in a 1700 cubic foot room contaminated with 0.5 micron particles, 96.8% were removed in the first 30 minutes and 99.9% after one hour. It has also been determined that because of the improved circulation of the negative ions, power supply voltages can be reduced without effecting particle removal ability. Higher voltage ion generators tend to have more problems with soiling walls and furniture, and tend to produce a "static shock" to someone touching the emitters or the air cleaner. In addition, ozone emissions are less likely with lower voltages. The tests have also shown that output voltages of less than 10 kilovolts in this configuration can effectively clean the air, with most ion generators available in the market producing upwards of 15 kilovolts.
It should also be noted that the prefilters 42 can be removed and washed as desired to remove particles retained therein, and that the positively electrically charged filter element 43 can also be easily replaced when desired.
It will thus be seen that structure has been provided with which the objects of the invention are achieved.
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Air cleaning and circulating apparatus is disclosed, wherein the apparatus is of the hassock fan type with a negative ion generator in the intake air stream to charge particles to be removed, which are then passed over and or through a charged filter which removes them, the air is ionized a second time and discharged for use.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
THE NAMES OF THE PARTIES TO A JOINT RESEARCH AGREEMENT
[0003] Not Applicable
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
[0004] Not Applicable
BACKGROUND OF THE INVENTION
[0005] 1. Field of the invention
[0006] This invention relates to improvements in a shaver for self-shaving a person's own back, legs or other area that might be difficult to reach. More particularly, the present back shaver provides an adjustable extension arm that allows a person to connect a disposable razor that can be purchased from a store and temporally secured to the adjustable extension arm to allow a person to self-shave their back legs or other area that might be difficult to reach.
[0007] 2. Description of Related Art Including Information Disclosed Under 37 CFR 1.97 and 1.98
[0008] As people get older, especially men, hair begins to grow on the back of a person. For some the hair can grow thick and may cause trouble with clothing and may be unsightly and undesirable. Removal of the hair can take a number of different methods. One method can be to have another person remove the hair on their back using a razor, wax, laser, chemicals or electrolysis. These methods require a second person to remove the hair from a back legs or other area that might be difficult to reach. This problem can also occur in pregnancy or for a person who in handicapped and wants to shave an area that may be out of their normal reach.
[0009] For a person to shave the hair on one's own back requires a mechanism that allows access to the complete back to be shaved. To shave the hair to a minimal length of hair or a “close shave” the optimal angle of the shaving blade to the skin must be maintained over the entire surface of the back. The causes particular difficulty because the shape, length and width of a back, the use of one or both arms and the contours of a back around the sides, shoulder blades, the spine and the planar/contoured sections of a back.
[0010] A number of patents and or publications have been made to address these issues. Exemplary examples of patents and or publication that try to address this/these problem(s) are identified and discussed below.
[0011] U.S. Pat. No. 5,167,069 issued on Dec. 1, 1992 to Kathleen H. Quinn discloses an invention called the Razor Reach. The razor in this patent has a linear extending straight handle with a pivoting razor at the end of the handle. The razor is pivoted in fixed increments to allow a person to set the length of the arm, adjust the angle and then reach the razor behind their back to shave the hair. While this patent allows a person to shave their own back or other area that is difficult to reach, the razor is a custom razor and does not accept standard pre-existing razors or replacement heads.
[0012] U.S. Pat. No. 6,266,888 issued on Jul. 31, 2001 for Thomas E. Zowaski discloses a Reaching Razor. This patent has an adjustable handle with pivoting elbow sections. While the razor allows a person to reach behind them to shave a back, the pivoting elbows must be frequently readjusted to accommodate the contours of a back as the user shaves the power back, the upper back and around their sides.
[0013] U.S. Pat. No. 7,856,725 issued on Dec. 28, 2010 for Brett C. Marut discloses a Razor With Articulated Handle Extension. This paten has a handle that essentially folds in-half to shorten the handle to achieve a long reach and also to make a more compact size for storage. The patent further uses an electric razor to shave back hair without using disposable razors. While this patent provides a razor that can be used to shave a back, the razor does not use replaceable razors and razor heads.
[0014] What is needed is an extendable razor that is easily extendable to set the angle of the shaving blade at the optimal angle for hair removal. The shaver should also accept disposable razor and razor heads. This disclosure provides a solution to the problem that has not been solved by others.
BRIEF SUMMARY OF THE INVENTION
[0015] It is an object of the interchangeable shaver to accept a variety of different disposable razors. Disposable razors are made by a variety of different companies and each company has their own geometry for the head and for the shaft or handle that retains the razor blades. These disposable razors can have from one to a multiple number of razors. To retain a disposable razor with a handle the interchangeable shaver has a cavity where the handle of the disposable razor slides into the holder to grip the handle and prevents the disposable razor from rotating as the shaver is drawn up, down and along the back, legs or other area of a person. While the handle retainer firmly grasps the handle the holder also allows quick release of the disposable razor. The adapter angles the disposable razor to provide an optimal shaving angle for maximum hair removal and the closest shave to reduce the frequency of repeat shaving.
[0016] It is an object of the interchangeable shaver to have an adaptor for accepting a replaceable shaving head. While some disposable razors provide a complete razor, it is often more common to replace just the head with blades. For this type of replaceable blades the interchangeable shaver has an adapter that connects the interchangeable shaver to a disposable head. The adapter is configured to accommodate different disposable heads with a single adapter.
[0017] It is another object of the interchangeable shaver for the shaft to be extendable. Making the shaft extendable allows the user to work with a short handle, a long handle or any intermediate length to have maximum versatility with a length of between six inches and 36 inches. The extendable shaft further allows a user to reduce the overall length for storage and transportation as well as extend the shaft to a desired length for use. Extension of the handle is provided with fixed detents or with friction couplings.
[0018] It is still another object of the interchangeable shaver to have a non-round shaft. The non-round shaft is used to prevent the razor head from rotating as the razor is being dragged along the back, legs or other area of the body. The shaft can be elliptical, multi-sided or have a key that prevents rotation of the telescoping sections.
[0019] Various objects, features, aspects, and advantages of the present invention will become more apparent from the following detailed description of preferred embodiments of the invention, along with the accompanying drawings in which like numerals represent like components.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
[0020] FIG. 1 shows a side view of the telescoping hand tool extended.
[0021] FIG. 2 shows a side view of the telescoping hand tool retracted.
[0022] FIG. 3 shows a top view of the telescoping hand tool.
[0023] FIG. 4 shows a side view of the shaver.
[0024] FIG. 5 shows a front view of the shaver.
[0025] FIG. 6 shows a rear top perspective view of the shaver.
[0026] FIG. 7 shows a front top perspective view of the shaver.
[0027] FIG. 8 shows top front perspective view of the insert.
[0028] FIG. 9 shows a side sectional view of the insert.
[0029] FIG. 10 shows a perspective view of the shaver and the insert for the end of the hand tool.
[0030] FIG. 11 shows a perspective view of a razor inserted into the insert and then into the hand tool.
[0031] FIG. 12 shows a perspective view of a disposable razor head on the shaver and then into the hand tool.
DETAILED DESCRIPTION OF THE INVENTION
[0032] FIG. 1 shows a side view of the telescoping hand tool 20 extended, FIG. 2 shows a side view of the telescoping hand tool 20 retracted and FIG. 3 shows a top view of the telescoping hand tool 20 . From FIG. 1 the hand tool 200 is shown at near complete extension. The sections are configured as non-circular sections to prevent the sections from spinning within each other. This ensures that when a person is placing torsional loads on a shaver the head of the razor will not rotate to an undesirable orientation. In the preferred embodiment the shaft sections are elliptical or flattened circular sections of telescoping sizes. From the largest section 21 to the smallest section 26 . While six sections hand section, 22 , 23 , 24 , 25 and top section 26 are shown, there could be more or less than six sections.
[0033] The number of sections are selected based upon the desired length of that is desired by the user. The hand section 21 is shown with a cushion 27 that also makes the hand tool 20 easier to grasp if the users' hand is wet. The top view of FIG. 3 shows the elliptical shape of the sections. The last section 26 of the arm has an elbow 31 transitions into a cross section 32 that angles the cross section 32 from the pole sections 21 - 26 . The cross section 32 has a receiver 30 . The receiver is essentially a cylindrical receiving tube 33 with an interior hole 35 . The end of the rim 34 provides a shoulder.
[0034] In FIG. 2 the sections 21 - 26 are shown shortened to allow a user to access an area of the back that is closer to the handle. The sections are tightly telescoped together to reduce movement between adjoining sections. It is also contemplated that the sections can have detents or spring loaded pins that retain sections in fixed positions. When using spring loaded pins the pins must be depressed to allow the section(s) to slide or telescope with each other. Making the shaft extendable allows the user to work with a short handle, a long handle or any intermediate length to have maximum versatility with a length of between six inches and 36 inches. The extendable shaft further allows a user to reduce the overall length for storage and transportation as well as extend the shaft to a desired length for use. Extension of the handle is provided with fixed detents or with friction couplings.
[0035] FIG. 2 further shows the receiver 30 placed at an angle 36 to allow the receiver to provide a different angle 36 for the receiver hole 34 . It is contemplated that the elbow 31 can allow the cross section to pivot on the last section 26 to alter the angle from 90 degree to straight.
[0036] FIG. 4 shows a side view of the shaver, FIG. 5 shows a front view of the shaver 50 , FIG. 6 shows a rear top perspective view of the shaver 50 and FIG. 7 shows a front top perspective view of the shaver 50 . The shaver 50 has a bottom surface 51 with a chamfer that allows the shaver 50 to be inserted into the receiver hole 35 (shown in FIG. 1 ) of the receiver 30 . A taper 52 allows the shaver 50 to be gripped within the receiver hole 35 . Both the taper 52 of the shaver 50 and a taper in the receiver hole 35 are approximately the same to provide sufficient gripping forces without the use on fasteners or bonding agents. The mid-section of the shaver 50 is a curved neck 55 . The curved neck 55 provides a preferred angle of about 40 degrees to create a more optimal angle for shaving. The curved neck 55 extends to an expansion 56 .
[0037] The expansion spreads the shaver 50 to provide a locating and gripping portion for securing a replaceable razor head (not shown). The top of the shaver 50 has a curved surface that allows a replaceable razor to move in an arc travel 57 on the shaver 50 and on the curved face 60 . A plurality of locating and stop pins 59 is located on the end of the shaver 50 to limit the arc travel of a replaceable razor head.
[0038] The shaver 50 has a split 58 that extends down to a through hole 54 near a relief 53 near the taper 52 . This split 58 allows the two sides of the shaver 50 to be flexed together to accept a disposable razor head and to return to a normal position to retain the disposable razor head. The shape and configuration of the pins and arc travel 57 allows different disposable razor heads from different manufactures to mount onto the shaver 50 thereby allowing the shaver 50 to provide a universal solution for disposable razors.
[0039] FIG. 8 shows top front perspective view of the insert 80 , FIG. 9 shows a side sectional view of the insert 80 . The insert 80 has a bottom end 81 with a relief hole 82 that provides a reduced weight to the insert 80 . From the base 81 the side is tapered 84 to allow the insert 80 to be inserted and gripped by the inside tapered diameter of the receiver 30 (shown in FIG. 1 ) without the use of a fastener or bonding. A shoulder 85 prevents the insert 80 from being inserted too far into the receiver 30 . The body of the insert 80 then expands to a plurality of spring tabs 86 .
[0040] In this preferred embodiment of the insert 80 there are six spring tabs 86 , but more or less than six spring tabs 86 are contemplated. The selection of six spring tabs 86 has provided the optimal number for grasping onto the handle of a disposable shaver 120 (as shown in FIG. 11 ). The spring tabs 86 are relieved with slots 87 that extend to a slot relied 88 hole that essentially allows each spring tab 86 to operate independently from the base of the insert 80 to the end 89 of each spring tab 86 . The inside 90 surface of the spring tab(s) 86 are curved to press against the handle of a disposable razor 120 . The inside bottom of the insert 80 has receiver pocket 91 where the end of a disposable razor 120 stops or rests.
[0041] FIG. 10 shows a perspective view of the shaver 50 and the insert 80 for the end of the hand tool 35 . From the bottom of this figure the open end 35 of the receiver 30 is shown at the end of the cross member 32 of the receiver tube 33 . The neck 55 extends to the curved face of the shaver 50 . With the insert 80 the spring tabs 86 extend from the tapered end 84 . The tapered end 52 of the shaver 50 and the tapered end 84 of the insert 80 are essentially the same and compliment the hole 35 of the receiver 30 .
[0042] The shaver 50 can be inserted 102 into the receiver hole 35 or the receiver or the insert 80 can be inserted 101 or interchanged into 100 the open end 34 of the receiver hole 35 to accept a disposable razor secured into the insert 80 or disposable shaving head secured to the shaver 50 .
[0043] FIG. 11 shows a perspective view of a disposable razor 120 inserted into the insert 80 and then into the hand tool 30 . This is a typical configuration when using a disposable razor with an attached handle 120 . A user inserts 92 the disposable razor 120 into the insert 80 , and the insert 80 into the receiver tube 33 of the receiver 30 until the end of the handle of the disposable razor 120 is gripped. The user may rotate the disposable razor 120 to obtain optimal grip of the handle of the disposable razor and the irregular shaft of the disposable razor 120 falls into the slots of the spring tabs of the insert 30 . The cross member 32 extends to the adjustable shaft of the receiver 30 to allow the user to set the desired length of the handle. After the disposable razor 120 has been sufficiently used, a user simply pulls 93 the disposable razor out of the insert 80 and can then install a replacement disposable razor 120 into the insert 80 .
[0044] FIG. 12 shows a perspective view of a disposable razor head 110 on the shaver 50 and then into the hand tool 30 . This is a typical configuration when using a disposable razor head 110 . A user inserts the shaver 50 into the receiver tube 33 of the receiver 30 and the squeezes 61 / 62 the sides of the shaver 50 as they place a disposable razor head 110 onto the shaver 50 to grip the disposable razor head 110 . The cross member 32 extends to the adjustable shaft of the receiver 30 to allow the user to set the desired length of the handle. After the disposable razor head 110 has been sufficiently used, a user simply squeezes 61 / 62 the sides of the shaver 50 to release the disposable razor head 110 . The user can then install a replacement disposable razor 110 into the insert shaver 50 .
[0045] Thus, specific embodiments of an interchangeable shaver have been disclosed. It should be apparent, however, to those skilled in the art that many more modifications besides those described are possible without departing from the inventive concepts herein. The inventive subject matter, therefore, is not to be restricted except in the spirit of the appended claims.
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Improvements in an interchangeable shaver that accepts a variety of different disposable razors. To retain a disposable razor with a handle the interchangeable shaver has a cavity where the handle of the disposable razor slides into the holder to grip the handle and prevents the disposable razor from rotating as the shaver is drawn up, down and along the back, legs or other area of a person. The adapter angles the disposable razor to provide an optimal shaving angle for maximum hair removal and the closest shave to reduce the frequency of repeat shaving. A further improvement is an adapter that connects the interchangeable shaver to a disposable head. The adapter is configured to accommodate different disposable heads with a single adapter. The shaver has an extendable handle configured to prevent the razor from rotating on the shaft.
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This is a divisional of application(s) Ser. No. 08/430,150 filed on Apr. 26, 1995, now U.S. Pat. No. 5,621,032, which is a Division of U.S. Ser. No. 08/135,125, filed on Oct. 8, 1993, now abandoned, which is a continuation of U.S. Ser. No. 07/774,587, filed on Oct. 10, 1991, now abandoned.
BACKGROUND OF THE INVENTION
The large scale industrial and commercial uses of liquid and low melting point solid bulk materials pose a multitude of practical problems. Such materials are difficult to handle; their physical properties lead to inaccurate measurements. Their physical form frequently results in a significant percentage of waste due to materials adhering to containers and handling equipment. Frequently, such materials have a limited shelf life due to decomposition. Decomposition presents a particular problem with organic peroxides which, over time, become unstable and present an explosive hazard. Low melting point solids, those solids having a melting point below 120° F., become semi-solid and usually tacky, as they approach their melting point. While this may not present a significant problem at room temperature, the ambient temperature in many plant operations may exceed 100° F. and approach the melting point of the low melting point solids. Even if the ambient temperature is well below the melting point of the low melting point solid, if the solid has been previously exposed to temperatures near the melting point, the product may have partially melted and “coalesced” into a large agglomerate.
Attempts have been made to address these problems by mixing certain liquid or low melting point solid materials with solid compounds thereby giving such materials an interim solid form so that they will remain solid over a wider temperature range. The resulting product is then added to formulations which call for the liquid or low melting point solid. However, the products that result from such attempts have significant drawbacks. Frequently, the dispersion of the liquid or low melting solid material is not uniform; this results in a wide variability in the concentration of the material within the product. Variability is a particular problem in products which use mineral fillers, such as clay, as a binder component. Where the liquid or low. melting point solid is absorbed or adsorbed onto a mineral filler like clay, there is a strong tendency toward particle agglomeration, especially if the product experiences wide temperature variation during transportation and storage. Where a mineral such as clay is mixed into a liquid, the clay tends to settle out before the product fully solidifies, resulting in a stratified product. This stratification produces an uneven concentration of the liquid or low melting point solid throughout the final product. Also, products that have a mineral filler as a binder, present a dispersion problem during the products incorporation into the end formulation, such as into a rubber formulation.
Also, such products frequently have a low “activity”, that is, the product contains a low percentage of the desired liquid or low melting point solid ingredient. A higher activity is desired by the purchasers since first, more of the desired liquid or low melting point solid is available for the money, and, second, since the product will have correspondingly less binder, there are fewer compatibility problems between the binder and the purchaser's formulation which requires the liquid or low melting point solid.
In addition, such products are frequently powdered. Powders may present a respiratory hazard for persons handling the product and may present an explosive hazard as well. Furthermore, many products “bleed”, that is, the liquid ingredient tends to disassociate from the solid component.
It would be desirable to have a liquid or low melting point solid in a solid form, to facilitate handling, measuring and storing, and which can be added directly to the processes which require the liquid or low melting point solid ingredient. It would also be desirable to have a high activity, homogenous product in a non- powdered form. Finally, a product that would fully melt into a formulation, such as a rubber formulation, during processing, eliminating the undispersed solid particles, would be very desirable.
SUMMARY OF INVENTION
The present invention relates to either a liquid compound or a low melting point solid compound, referred to herein as “active ingredients”, uniformly mixed with a binder, to provide a solid composite of high activity and longer shelf life, and also relates to the method of their preparation. The composites provide a temporary form for liquid or low melting point solid ingredients; the composites may be incorporated into a variety of industrial and/or commercial processes in the same way that the active ingredient would be used. The composites may be added to processes which tolerate the addition of the binder. Composites may be made of a variety of active ingredients, such as: organic dialkyl peroxides; modified melamine resins; cyanurates; aldehyde-amines; phenylamines; methacrylates; organo-silanes and brgano-phosphites. As used herein “composite” means a solid mixture of an active ingredient and a binder. The “activity” of a particular composite, that is, the percentage of active ingredient in the composite, will depend upon the type of active ingredient. The active ingredient is “composited” by being combined with a thermoplastic binder, which contains a wax, and a thermoplastic polymer. Depending upon the type of active ingredient in the composite, the binder may also contain a compatibilizing agent such as a fatty acid or an ethylene vinyl acetate copolymer resin, or both. Optional minor components, such as wetting agents, stabilizers, plasticizers, homogenizing agents and mineral oils may also be added.
The composite is prepared by blending the active ingredient with the binder preferably while both are in a liquid phase, then cooling the mixture and forming or shaping the composite, using conventional forming procedures.
DETAILED DESCRIPTION OF THE INVENTION
The Active Ingredient
According to the present invention, a variety of liquid and low melting point solid active ingredients are “composited” to produce composites that are easier and safer to handle, easier to measure, have an increased shelf life, and a high activity, that is, a high percentage, in some composites up to 80%, of the active ingredient. The maximum percentage of active ingredient depends on the type of active ingredient. When more than the maximum percent of the active ingredient is present in the composite (and thus, less than minimum binder is present) the composite becomes oily, frosted and/or tacky. This condition is often described as surface bloom. Where the active ingredient is present in the preferred amount, the composite has a high activity without a surface bloom. Where the active ingredient is present in an amount between the preferred amount and the maximum amount, the composite contains some surface bloom but may be satisfactory for some uses. While as little as about 1% active ingredient may be present in the composite, the economic interests dictate that the composite have a higher activity, usually at least 30%.
For organic peroxide, a high activity means the composite will have about 70% to about 80% organic peroxide. For cyanurates, modified inelamine resins, organo-silanes, organo-phosphites, and aldehyde-amine reaction products, a high activity means the composite will have about 50% to about 80% active ingredient. For phenylamine based antidegradants and methacrylates, a high activity means the composite will have about 60% to about 80% active ingredient.
Composites may be made of a variety of organic peroxides, for example, dialkyl peroxides, including dicumyl peroxide, 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, a,a′-di(t-butyl peroxy)diisopropylbenzene, 2,5-dimethyl-2,5-di(t-butylperoxy) hexyne-3 and butyl-4,4-bis(t-butylperoxy) valerate. A suitable dicumyl peroxide is sold by Hercules, Inc. under the tradename DICUP R, or by Akzo Chemicals Inc. under the tradename PERKADOX BC. A suitable 2,5-dimethyl-2,5-di(t-butylperoxy)hexane is sold by Akzo Chemicals Inc. under the tradename TRIGONOX 101, or by Atochem under the tradename LUPERSOL 101. A suitable a,a′-di(t-butyl peroxy)diisopropylbenzene is sold by Hercules, Inc. under the tradename VULCUP R, or by Akzo under the tradename PERKADOX 14S. A suitable 2,5-dimethyl-2,5-di(t-butylperoxy) hexyne-3 is sold by Atochem under the tradename LUPERSOL 130 or by Akzo under the tradename TRIGONOX 145. A suitable m-butyl4,4-bis(t-butyl-peroxy) valerate is sold by Akzo under the tradename TRIGONOX 17, or by Atochem under the tradename LUPEROX 230.
The compositization of organic peroxides according to this invention preserves the shelf life of the peroxides, and thus is particularly beneficial because peroxides are unstable and over time, present an explosive hazard. In addition, many organic peroxides are semi-solids at operating temperature and thus are difficult to handle and measure because of their tendency to stick to containers and to reagglomerate. The organic peroxide composites of the present invention overcome these problems.
A composite may be made containing a modified melamine resin, (also known as modified melamine formaldehyde resin) such as hexamethoxymethylmelamine. A suitable hexamethoxymethylmelamine is available from American Cyanamid under the Trademark “Cyrez 963” or from Monsanto Company under the Trademark “Resimene 3520”. Hexamethoxymethylmelamine is a methylene donor and is widely used particularly in the tire industry, as an adhesion promoter.
Composites may be made from cyanurates, such as triallyl cyanurate, which is a low melting point solid and triallyl isocyanurate, which is a liquid at room temperature. A suitable triallyl cyanurate is sold by Akzo under the tradename PERKALINK 300, or by American Cyanamid under the tradename TRIALLYLCYANURATE. A suitable triallyl isocyanurate is sold by Akzo under the tradename PERKALINK 301. Cyanurates are used in various industrial applications as reactive monomers for free radical polymerization. In the rubber industry cyanurates are used as co-agents, in the non-sulfur, (peroxide) curing of rubber.
Composites may be made of phenylamine based antidegradants such as: phenylenediamines, such as N-phenyl-N′-2octyl-p-phenylenediamine, which is a liquid at room temperature; alkylated diphenylamines; and the reaction products of diphenylamines, such as the reaction product of diphenylamine and acetone, commercially available as “BLE-25” from Uniroyal. The BLE-25 formulation is proprietary; it is characterized by a viscosity of 25-50 poise at 86° F., and specific gravity of 1.08 to 1.10. A suitable N-phenyl-N′-2-octyl-p-phenylenediamine is sold by UOP Inc. under the tradename UOP 688. The phenylamine based antidegradants serve as antidegradants in rubber compositions.
Composites may be made of methacrylates, such as trimethylolpropane trimethacrylate and trimethylolpropane triacrylate. A suitable trimethylolpropane trimethacrylate is sold by Sartomer Corporation under the Trademark “Sartomer Resin 350”. A suitable trimethylolpropane triacrylate is also sold by Sartomer Corporation under the Trademark “Sartomer Resin 351”. Methacrylates often serve as a co-agent in the peroxide curing of rubber.
Composites may be made of organo-silanes, such as bis(3-triethoxysilylpropyl)tetrasulfane and a liquid organo-functional silane known as “UCARSIL RC-1” and sold by Union Carbide. The formulation of “UCARSIL RC-1” is proprietary. A suitable bis(3-triethoxysilylpropyl)tetrasulfane is sold by Degussa Corporation under the tradename “SI-69”. Organo-silanes serve as adhesion promoters and coupling agents in rubber formulations.
A composite according to the present invention may also be made of organo-phosphites, such as tri (monononylphenyl) phosphite and tri (dinonylphenyl) phosphite or mixtures thereof. A suitable mixture is sold under the trademark “POLYGARD HR” by Uniroyal Chemical Company. The organo-phosphites serve as antidegradants in rubber compositions.
Composites may also be made of aldehyde-amine reaction products, such as butyraldehyde-aniline reaction products, butyraldehyde-butylamine reaction products, formaldehyde-ammonia-ethyl chloride reaction products, and heptaldehyde-aniline reaction products. A suitable butyraldehyde-butylamine reaction product is sold by R.T. Vanderbilt under the tradename “VANAX 833”. A suitable formaldehyde-ammonia-ethyl chloride reaction product is sold by Uniroyal under the tradename “TRIMENE BASE”. A suitable heptaldehyde-aniline reaction product is sold by Uniroyal under the tradename “HEPTEEN BASE”. Suitable butyraldehyde-aniline reaction products are sold by R.T. Vanderbilt under the tradenames “VANAX AT” and “Vanax 808”. The aldehyde-amine reaction products serve as accelerators in rubber formulations.
It should be understood that the active ingredients, particularly commercial grades, depending on their source, may contain substantial amounts of a wide variety of impurities. Therefore, such impurities also will be incorporated into the composite.
The Binder
As used herein, the term “binder” includes all additives, except the active ingredient, in the composite. The binder has a higher melting point/softening point than the active ingredient, and imparts the solid form to the composite. The binder contains at least one wax, and at least one thermoplastic polymer, for example, a polyolef in, preferably polyethylene, most preferably oxidized polyethylene. Depending on the type of active ingredient, the binder may also contain at least one compatibilizing agent, for example, ethylene vinyl acetate copolymer resin or a fatty acid, or mixtures thereof. A compatibilizing agent promotes the compatibility between the active ingredient and the binder, which promotes the cohesiveness of the composite. Where the active ingredient and the binder are of sufficiently different polarity so that the composite is not cohesive, a compatibilizing agent may be required. Optional minor components such as wetting agents, stabilizers, plasticizers, and mineral oils may also be added.
Any wax could be used, including, but not limited to, petroleum derived waxes such as paraffin and microcrystalline wax, and natural waxes such as beeswax and carnauba. Good results have been obtained using paraffin wax or a microcrystalline wax or mixture of both. Paraffin is preferred. However, it should be understood that paraffin may contain some microcrystalline wax. While any paraffin wax may be used, good results have been obtained using a paraffin wax having a melting point in the range of 140° to 145° F. A suitable paraffin is sold by Astor Wax Company available through M. F. Cachat, Cleveland, Ohio under the Trademark “Astax 140/145 Paraffin”. The wax helps impart the solid form to the binder.
A thermoplastic polymer, such as polyethylene, preferably oxidized polyethylene, promotes compatibility between the active ingredient and the binder components and helps to impart the necessary hardness to the composite. A suitable oxidized polyethylene having a melting point from about 170° F. to about 250° F., a viscosity from about 80 to about 160 cps at 120° C., and a hardness of from about 1 to about 5 penetration units at 25° C., is sold by Hils of Germany, and is available from M. F. Cachat, Cleveland, Ohio under the Trademark “Vestowax AO 1539”.
Depending on the active ingredient, a fatty acid may be added to the binder. The addition of fatty acids improves the compatibility of the active ingredient and the binder, and also lowers the initial melting point of the composite. Preferably, fatty acid is added where the active ingredient is a modified melamine resin, a cyanurate, or a reaction product of acetone and diphenylamine. Due to the difficulty in separating fatty acids, a fatty acid is a mixture of several different fatty acids. Preferably, a fatty acid having a stearic acid content from about 10% to about 92% stearic acid, and more preferably, a high stearic acid content fatty acid having a stearic acid content of 70% is used. The other fatty acids present in the mixture typically include palmitic acid, oleic acid and myristic acid. These fatty acids may also be used alone or in combination although they are not preferred. A suitable high stearic acid content fatty acid is sold by Witco Industries under the Trademark “HYSTRENE 7018”.
Depending on the type of active ingredient in the composite, an ethylene vinyl acetate copolymer resin may also be added. Preferably, ethylene vinyl acetate copolymer resin is added where the active ingredient is a phenylamine based antidegradant, a cyanurate, a modified melamine resin, an organo-phosphite, or the liquid organo-functional silane “RC-1”. Ethylene vinyl acetate copolymer resin acts as a homogenizer and also increases the viscosity of the heated binder-active ingredient blend, which provides a more defined shape upon forming. Good results have been obtained using an ethylene vinyl acetate copolymer resin having about 18% vinyl acetate, about 82% ethylene and a softening point of 190° F. A suitable resin is sold by DuPont DeNemours Company under the Tradename “Elvax” and also sold by Quantum Chemical under the Tradename “ULTRATHENE”.
The percentage of individual binder components will depend upon the type of active ingredient in the composite. The following binder component percentages represent the percent of total binder composition. When the active ingredient is an organic peroxide, the paraffin may be present in the binder from about 20% to about 95%, preferably about 63.3%. The polyethylene is present in the binder from about 5% to about 80%, preferably about 36.7%.
Where the active ingredient is a modified melamine resin, such as hexamethoxymethylmelamine, the paraffin may be present in the binder from about 1% to 60% of the total binder composition, preferably about 30%. The polyethylene is present in the binder from about 1% to about 40%, preferably about 20%. In addition, the binder contains either from about 1% to about 40%, of ethylene vinyl acetate copolymer resin or from about 1% to about 50%, fatty acid, or both. Preferably, the binder contains both fatty acid and ethylene vinyl acetate copolymer resin; preferably about 40% fatty acid and about 10% ethylene vinyl acetate copolymer resin.
Where the active ingredient is a cyanurate, the paraffin is present in to the binder in an amount from about 1% to about 60% of the total binder composition, preferably about 30%. The polyethylene is present in the binder from about 1% to about 40%, preferably about 15%. In addition, the binder contains either from about 1% to about 40% of ethylene vinyl acetate copolymer resin or from about 1% to about 50% fatty acid, or both. Preferably, the binder contains both fatty acid and ethylene vinyl acetate copolymer resin; preferably about 40% fatty acid and about 15% ethylene vinyl acetate copolymer resin.
Where the active ingredient is a phenylamine, such as N-phenyl-N′-2-octyl-p-phenylenediamine, the paraffin is present in the binder in an amount from about 5% to about 70% of the total binder composition, preferably about 38%. The polyethylene is present in the binder from about 1% to about 40%, preferably about 12%. Preferably from about 5% to about 70%, preferably about 50%, of ethylene vinyl acetate copolymer resin is added.
Where the active ingredient is a liquid high temperature reaction product of acetone and a diphenylamine, such as “BLE-25”, the paraffin is present in the binder in an amount from about 5% to about 50% of the total binder composition, preferably about 20%. The polyethylene is present in the binder from about 1% to about 60%, preferably about 30%. In addition, the binder contains either from about 1% to about 60% of ethylene vinyl acetate copolymer resin or from about 1% to about 50% fatty acid, or both. Preferably, the binder contains both fatty acid and ethylene vinyl acetate copolymer resin; preferably about 20% fatty acid and about 30% ethylene vinyl acetate copolymer resin.
Where the active ingredient is an organo-silane such as bis(3-triethoxysilylpropyl)tetrasulfane, the paraffin is present in the binder in an amount from about 20% to about 95% of the total binder composition, preferably about 63.3%. The polyethylene is present in the binder from about 5% to about 80%, preferably about 36.7%. Where the active ingredient is the liquid organo-functional silane “UCARSIL RC-1”, the paraffin is present in the binder in an amount from about 5% to about 70% of the total binder composition, preferably about 47.5%. The polyethylene is present in the binder from about 1% to about 50%, preferably about 27.5%. Preferably, ethylene vinyl acetate copolymer resin is also present in the binder from about 1% to about 60%, more preferably about 25%.
Where the active ingredient is a methacrylate the paraffin is present in the binder in an amount from about 20% to about 99% of the total binder composition, preferably about 63.3%. The oxidized polyethylene is present in the binder from about 1% to about 80%, preferably about 36.7%.
Where the active ingredient is an organo-phosphite, the paraffin is present in the binder in an amount from about 5% to about 50% of the total binder composition, preferably about 20%. The oxidized polyethylene is present in the binder from about 1% to about 60%, preferably about 40%. Preferably, ethylene vinyl acetate copolymer resin is also present in the binder from about 1% to about 60%, more preferably about 40%.
Where the active ingredient is an aldehyde-amine reaction product, the paraffin is present in the binder in an paamount from about 5% to about 95%, preferably about 50.6%. The oxidized polyethylene is present in the binder from about 1% to about 60%, preferably about 29.4%. Preferably, ethylene vinyl acetate copolymer is also present in the binder from about 1% to about 50%, more preferably about 20%.
Additional components such as stabilizers, plasticizers, wetting agents and mineral oils may be added, in minor amounts, to the binder. Stabilizers, such as hydroquinone, may be added to the binder in an amount from about 0.1% to about 10%, to prevent the oxidation or hydrolysis of the active ingredient in the composite. Plasticizers, such as phthalate plasticizers, preferably diisodecylphthalate or dioctylphthalate may be added to the binder in an amount from about 1% to about 20% to decrease the melting point of the composite. Wetting agents, such as amine derivatives of fatty acids, may be added in an amount from 1% to about 50% to promote compatibility of the active ingredient in the composite. Mineral oils, such as paraffinic oils and naphthenic oils, may be added to the binder to decrease the melting point of the composite. A suitable paraffinic oil is sold by Sun Oil under the Trademark “SunPar 2280”. A suitable naphthenic oil is sold by Ergon under the Tradename “Hyprene V 2000”. The mineral oil is added in an amount sufficient to adjust the melting point of the composite to the desired melting point.
The Composite
The composite of the active ingredient and the binder is prepared by combining the active ingredient with the binder so that at some point in the mixing procedure, the binder and the active ingredient are both in a liquid phase, and are then blended while both are in a liquid phase. As used herein, “liquid phase” includes high viscosity paste-like phases. This may be accomplished by mixing the liquid active ingredient (or if active ingredient is a semi-solid, heating the active ingredient beyond its melting point) with a molten binder. Alternatively, the active ingredient may be mixed with a solid binder and the temperature of the mixture raised above the melting points of the active ingredient and the binder ingredients. Then, once both the active ingredient and binder are in a liquid phase, they are thoroughly blended to provide a homogenous mixture, at a temperature which will keep both the binder and active ingredient in a liquid phase. After a thorough blending, the homogenous mixture is cooled just above the melting point of the composite. The mixture is then fed through conventional forming processes so that the finished composite may be in the form of pellets, pastilles, flakes, prills, powder or slabs, depending upon the desired form. A suitable method of forming the composites into pastilles, or half sphere shape, is by using a rotary head for forming drops onto a cooled stainless steel conveyor. This equipment is available from Sandvik Process Systems Inc.
It should be noted that as the percent of active ingredient in the composite is increased, (and the percentage of binder is correspondingly decreased) the tolerances of the binder and its components become narrower. That is, as the percentage of active ingredient increases, the percentage range of each binder component that will provide a satisfactory composite becomes narrower. Similarly, the type of the binder components needed to provide a satisfactory composite also become restricted. Where the percentage of active ingredient is very high, the preferred optional ingredients may become necessary ingredients; that is, they become necessary to maintain the form of the composite. When there is less binder in the composite, it becomes more difficult to obtain a solid composite and more difficult to form or shape the composite. These results affect not only the finished product, but also affect the operating speed of the composite forming equipment and the stability of the composite during storage and transportation. Also, decreasing the binder percentage in the composite reduces the compatibility between the active ingredient and the binder.
While the following examples of composites contain one active ingredient, more than one active ingredient may be added to a composite. It should be understood that composites having two or more active ingredients are within the scope of this invention.
The Organic Peroxide Composite
Organic peroxides, such as dialkyl peroxides may be present in the composite from about 30% to about 80%, preferably about 70%. The binder is present from about 20% to about 70%, preferably about 30%. Dialkyl peroxide composites may be prepared as follows.
EXAMPLE 1
A dicumyl peroxide (DCP) composite was prepared by measuring 136 kilograms of a recrystallized grade DCP, from Akzo Inc. which is 96-100% pure and has a melting point of about 100° F. The DCP was then placed in a vat with a hot water jacketing. The water temperature within the jacketing was controlled to yield a DCP temperature of from 150-160° F. The binder was prepared separately by melting together 36.7% of the total binder weight, or 21.4 kilograms of oxidized polyethylene (VESTOWAX AO 1539) having a melting point of 225° F. and 63.3%, or 36.9 kilograms of ASTAX 140/145 paraffin. The polyethylene and paraffin were thoroughly blended together in a heated blend tank at 195° F. Then the DCP was added to the liquid binder. The DCP-binder mixture was then thoroughly blended. (The addition of the DCP to the binder decreased the temperature of the mixture roughly to 170° F.) When a homogenous mixture was achieved, it was then fed in portions through a pelletizer, while the remainder was mildly agitated in the tank. The pelletizer, a Sandvik process system, dispensed the DCP-binder mixture in droplets onto a cold stainless steel conveyer belt. As a result, composite pellets in a “half-sphere” shape were produced.
EXAMPLE 1A
A dicumyl peroxide (DCP) composite was also prepared by first preparing the binder. The binder was prepared by melting together 36.7% of the total binder weight, or 21.4 kilograms, of oxidized polyethylene (VESTOWAX AO 1539) having a melting point of 225° F. and 63.3%, or 36.9 kilograms of ASTAX 140/145 paraffin. The polyethylene and paraffin were thoroughly blended together in a heated blend tank at 195° F. Then 136 kilograms of a recrystallized grade DCP, from Akzo Chemical Inc. which is 96-100% pure and has a melting point of about 100° F., was added to molten binder. The DCP-binder mixture was then thoroughly blended. (The addition of the DCP to the binder decreases the temperature of the mixture roughly to 170° F.) When a homogenous mixture was achieved, it was then fed in portions through a pelletizer, while the remainder was mildly agitated in the tank. The pelletizer, a Sandvik process system, dispensed the DCP-binder mixture in droplets onto a cold stainless steel conveyer belt. As a result, composite pellets in a “half-sphere” shape were produced.
EXAMPLE 2
An a,a′di(t-butylperoxy)diisopropylbenzene-composite was prepared by first preparing the binder which was made by placing 36.7% of the total binder weight, or 5.5 grams of oxidized polyethylene (VESTOWAX AO 1539) having a melting point of 225° F. and 63.3%, or 9.5 grams of ASTAX 140/145 paraffin in an aluminum dish. The dish was then heated on a hot plate to melt the binder components. When temperature reached 250° F. and the binder components were completely melted, the binder was thoroughly stirred. The binder was then cooled to just above 225° F. and then 70% or 35 grams of a,a′di(t-butylperoxy)diisopropylbenzene was added. The a,a′di(t-butylperoxy)diisopropylbenzene-binder mixture was maintained at between 150-200° F. and thoroughly blended. When a homogenous mixture was achieved, production methods for forming the composite were simulated by dispensing droplets from a stirring rod onto a chilled metal surface, such as aluminum. As a result, composite pellets in a “half-sphere” shape were produced.
EXAMPLE 3
A 2,5-dimethyl-2,5-di(t-butylperoxy)hexane (DBPH) composite was prepared as in Example 2. The binder was prepared by mixing together 36.7% of the total binder weight or 9.2 grams oxidized polyethylene, (VESTOWAX AO 1539) and 63.3% or 15.8 grams of ASTAX 140/145 paraffin having a 140-145° F. melting point. An equal weight, 25 grams, of DBPH, (LUPERSOL 101) was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Modified Melamine Resin Composite
The modified melamine resin, such as hexamethoxymethylmelamine, may be present in the composite in an amount of from about 1% to about 80%, preferably about 30% to about 70%, most preferably about 50%. The binder is present from g about 20% to about 99%, preferably about 70% to about 30%, most preferably about 50%. A hexamethoxymethylmelamine composite was prepared as follows.
EXAMPLE 4
The composite was prepared as in Example 2. The binder was prepared by mixing together 20% of the total binder weight or 5 grams, oxidized polyethylene (VESTOWAX AO 1539), 30% or 7.5 grams, of ASTAX 140/145 paraffin having a 140-145° F. melting point, 40% or 10 grams stearic acid (HYSTRENE 7018) and 10% or 2.5 grams EVA copolymer (ELVAX). An equal weight, 25 grams of hexamethoxymethylmelamine, (CYREZ 963) was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Cyanurate Composite
The cyanurate may be present in the composite in an amount from about 1% to about 80%, preferably 30% to about 70%, most preferably about 50%. The binder is present from about 20% to about 99%, preferably about 70% to about 30%, most preferably about 50%. A triallyl cyanurate (TAC) composite was prepared as follows.
EXAMPLE 5
The composite was prepared as in Example 2. The binder was prepared by mixing together 15% of the total binder weight or 3.75 grams of an ethylene vinyl acetate copolymer resin, (ELVAX), 15% or 3.75 grams oxidized polyethylene, (VESTOWAX AO 1539), 40% or 10 grams high stearic acid content fatty acid (HYSTERENE 7018) and 30% or 7.5 grams ASTAX 140/145 paraffin having a 140-145° F. melting point. An equal weight, 25 grams of TAC, (PERKALINK 300) was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Phenylamine Composite
Phenylamines, particularly phenylamine based antidegradants, may be present in the composite in an amount from about 30% to about 80%, preferably about 60%. The binder is present from about 20% to about 70%, preferably about 30% to about 50%, preferably about 40%. Phenylamine composites may be prepared as follows.
EXAMPLE 6
A composite of N-phenyl-N′-2-octyl-p-phenylenediamine was prepared as in Example 2. The binder was prepared by mixing together 50% of the total binder weight or 10 grams of an ethylene vinyl acetate copolymer resin, (ELVAX) 12% or 2.4 grams oxidized polyethylene (VESTOWAX 1539) and 38% or 7.6 grams ASTAX 140/145 paraffin having a 140-145° F. melting point. Then 30 grams of N-phenyl-N′-2-octyl-p-phenylenediamine, (UOP 688) was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
EXAMPLE 7
A composite of a high temperature reaction product of acetone and diphenylamine, commercially available as “BLE-25” from Uniroyal Chemical Company, was prepared as in Example 2. The binder was prepared by mixing together 30% of the total binder weight or 7.5 grams of an ethylene vinyl acetate copolymer resin, (ELVAX) 30% or 7.5 grams oxidized polyethylene, (VESTOWAX AO 1539) 20% or 5 grams ASTAX 140/145 paraffin having a 140-145*F melting point, and 20% or 5 grams of a high stearic acid content fatty acid. An equal weight, 25 grams, of BLE-25 was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Orqano-silane Composite
The organo-silane may be present in the composite in an amount of from about 30% to about 80%, preferably about 50% where the organo-silane is bis(3-triethoxysilylpropyl)tetrasulfane and preferably about 60% where the organo-silane is UCARSIL RC-1. The binder is present from about 20% to about 70%, most preferably about 50%, where the organo-silane is bis(3triethoxysilylpropyl) tetrasulfane, and preferably about 40% where the organo-silane is UCARSIL RC-1. Organo silane composites may be prepared as follows.
EXAMPLE 8
A composite of bis(3-triethoxysilylpropyl)tetrasulfane was prepared as in Example 2. The binder was prepared by mixing together a 36.7% of the total binder weight or 9.2 grams oxidized polyethylene (VESTOWAX AO 1539) and 63.3% or 15.8 grams ASTAX 140/145 paraffin having a 140-145° F. melting point. An equal weight, 25 grams of bis(3-triethoxysilylpropyl)tetrasulfane, (DEGUSSA's Si-69) was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
EXAMPLE 9
A composite of the liquid organo-functional silane “UCARSIL RC-1” was prepared as in Example 2. The binder was first prepared by mixing together a 27.5% of the total binder weight or 5.5 grams oxidized polyethylene, (VESTOWAX AO 1539) 47.5% or 9.5 grams ASTAX 140/145 paraffin having a 140-145° F. melting point, and 25% or 5 grams of ethylene vinyl acetate copolymer resin. Then 30 grams of UCARSIL RC-1 was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Methacrylate Composite
The methacrylate is present in the composite in an amount from about 30% to about 80%, preferably about 60%. The binder is present from about 20% to about 70%, preferably about 30% to about 50%, most preferably about 40%. A composite of trimethylolpropane trimethacrylate may be made as follows.
EXAMPLE 10
The composite was prepared as in Example 2. The binder was prepared by mixing 36.7% of the total binder weight or 7.3 grams oxidized polyethylene (VESTOWAX AO 1539) and 63.3% or 12.7 grams ASTAX 140/145 paraffin. Then 30 grams of trimethylolpropane trimethacrylate, (SARTOMER RESIN 350) was;
added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
Organo-phosphite Composite
The organo-phosphite is present in the composite in an amount from about 30% to about 80%, preferably about 50%. The binder is present from about 20% to about 70%, most preferably about 50%. A composite of tri(mixed monononylphenyl and dinonylphenyl)phosphite may be made as follows.
EXAMPLE 11
A composite was prepared as in Example 2. The binder was prepared by mixing 40% of the total binder weight or 10 grams oxidized polyethylene, (VESTOWAX AO 1539) 20% or 5 grams ASTAX 140/145 paraffin, and 40% or 10 grams ethylene vinyl acetate copolymer resin (ELVAX). An equal weight, 25 grams, of “POLYGARD HR” a tri(mixed monononylphenyl and dinonylphenyl)phosphite, was added to the binder mixture while agitating the mixture. The composite was prepared as in Example 2.
The Aldehyde-Amine Reaction Product Composite
The aldehyde-amine reaction product composite is present in the composite in an amount from about 1 to 80% preferably 30% to about 70%, more preferably about 50%. The binder is present from about 30% to about 70% preferably about 50%. A composite of the reaction product or butyraldehyde and aniline may be prepared as follows.
EXAMPLE 12
A butyraldehyde-aniline composite was prepared as in Example 2. The binder was prepared by mixing together 20% of the total binder weight or 5 grams of ethylene vinyl acetate copolymer resin, (ELVAX) 29.4% or 7.3 grams oxidized polyethylene (VESTOWAX AO 1539) and 50.6% or 12.7 grams ASTAX 140/145 paraffin and mixed as in Example 2. A equal weight, 25 grams of VANAX 808, a butyraldehyde aniline reaction product was added, and the composite was prepared as in Example 2.
While Examples 2-12 were done on a laboratory scale, the same formulations can be adapted to a commercial scale with appropriate modifications similar to Examples 1 and 1A.
While the invention has been described with a certain degree of particularity, various adaptations and modifications can be made without departing from the scope of the invention as defined in the appended claims.
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A method and product which provides a solid, non-powdered homogeneous form to liquid and low melting point solid compounds which facilitates stability, storage, dispersability and handling and which may be added directly to formulations requiring the liquid compound or low melting point solid compound. The liquid or low melting point solid ingredient is combined with a binder which is comprised of at least a wax and thermoplastic polymer. During the method of forming the product, both the binder and the liquid compound (or low melting point solid compound) pass through a liquid phase during which they are mixed. The product is then formed and cooled.
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FIELD OF THE INVENTION
The present invention relates to a system for dynamically controlling the form of information displayed on a web browser, and in more detail relates to a system for dynamically controlling the form of data to be embedded into a page template.
BACKGROUND OF THE INVENTION
Known techniques can choose information that is less likely to be changed in an HTML template and embed information more likely to be changed into this template for displaying as disclosed in the Published Unexamined Patent Application Nos. 10-198596, 11-85727, 10-334086 and 11-66152.
However, such techniques have adopted a system, as illustrated in FIG. 43 , of selecting data to be embedded into the template, to designate the accessing method, to designate the layout, to designate the data format, and the like, under a CGI program. An alternative system, as shown in FIG. 44 , embeds a program (such as JavaBeans), to accesses prescribed data, displays them in a prescribed form, and incorporates them data into the template.
Such a CGI program (or JavaBean), in which database names, file names, and the like are described in a fixed manner, required the occurrence of a workload to modify the CGI program or to replace the JavaBeans with new ones when it was desired to incorporate information from another database, or of another file, into the template without altering the database or the contents of the file themselves. This makes it impossible to dynamically switch prescribed displayed data. Additionally, the designer of a web page may be required to have knowledge of programming.
Especially when staging a campaign for various products with a web browser on the Internet. A campaign planner wants to be able to alter the contents or the layout according to the targeted customers' interest or to schedule without having to edit the HTML file or to modify the server program (such as CGI).
Furthermore, displaying contents strictly for a prescribed user, makes it possible to enhance advertising by communicating effective information, such as advertisements, that are based on the needs of that particular user, as well as to increase sales in electronic commerce.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a system permitting alteration of the contents or layout to be embedded into a page template without having to edit the HTML file or modify the server program such as CGI.
Another object of the invention is to provide a system permitting dynamic alteration of the contents or layout to be embedded into a page template according to the situation at the time of accessing by a user.
Another object of the invention is to provide a versatile and low cost system permitting information on contents and layout to be embedded into a page template to be diverted to another page template.
Another object of the invention is to provide a system permitting, on the basis of the behavior of a user having used Internet, information fitting that particular user's taste and behavioral pattern to be supplied only to the user or a group including that user.
Another object of the invention is to provide a system reduced in resources required at the time of execution.
According to one aspect of the present invention, a page template which would serve as the prototype of a web page contains formatter specifying information and display attribute information. This formatter specifying information is information to specify one out of a plurality of kinds of formatters (banner, Telop, a plurality of banners arrangement, and the like). Display attribute information is information for controlling the moves of this formatter. When a page template is called by a web browser, this formatter is actuated and effects such controls as selecting, arranging, and determining the displaying sequence and time of the contents to be embedded into the template according to the display attributes, or reducing the display area (the area made available in the template for embedding the contents) to the size of the contents.
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting page information to an information terminal having a display screen and an input unit, comprising the steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring formatter specifying information and display attribute information from the page template, (c) acquiring a formatter on the basis of the formatter specifying information, and (d) processing contents to be incorporated into the page template on the basis of the display attribute, and generating page information to be displayed on the display apparatus of the information terminal.
In the claims of the specification under the present application, “formatter specifying information” is a concept covering information used for specifying a formatter, such as the path name, file name, database name, table name, and information to identify the type of formatter. “Contents” is a concept referring to parts registered correspondingly to display areas in an arrangement rule DB to be explained with reference to an embodiment to be described below, covering not only contents registered in parts whose display conditions have prescribed values but also contents specified by descriptions fixed by a path name and the like in display areas. And “processing” is a concept covering alteration of any content in size, shape, arrangement, background color, color of its own, and display method (such as being displayed while moving from right to left, or emerging in a grid form).
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, comprising to steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring formatter specifying information and display attribute information from the page template, (c) acquiring a formatter on the basis of the formatter specifying information, (d) acquiring information on a plurality of contents to be displayed on the page template, and (e) generating, if it is judged that the display attributes include one indicating rotation, page information including information on a first content among the plurality of contents and generating, after the lapse of a prescribed length of time, page information including information on a second content among the plurality of contents.
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, comprising the steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring formatter specifying information and display attribute information from the page template, (c) acquiring a formatter on the basis of the formatter specifying information, (d) acquiring information on a plurality of contents to be displayed on the page template, and (e) excluding, if it is judged that the display attributes include one indicating random, information on a first content among the plurality of contents and generating page information including information on a second content among the plurality of contents.
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, comprising the steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring formatter specifying information and display attribute information from the page template, (c) acquiring a formatter on the basis of the formatter specifying information, (d) acquiring information on any content to be displayed on the page template, (e) acquiring size information on a display area predefined to display the content from the page template, (f) comparing the size information on the display area with the size information on the acquired content, and (g) adjusting, if it is judged that the size information on the display area has a greater value than the size information on the acquired content and the display attributes include one to instruct adjusted displaying, the size of the display area to the size of the content and generating page information.
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, comprising the steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring formatter specifying information and display attribute information from the page template, (c) acquiring a formatter on the basis of the formatter specifying information, (d) searching for information on a content to be displayed on the page template, (e) judging, if it is judged that there is no content to be displayed, whether or not information on default contents is defined in the page template, and (f) generating, if any information on default contents exists, page information including the information on default contents.
According to another aspect of the invention, there is provided a display information fixing method to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, comprising the steps of:
(a) analyzing a page template specified by a display information acquisition request from the information terminal, (b) acquiring from the page template formatter specifying information and display attribute information on a formatter to control the arrangement of a plurality of contents, (c) acquiring a formatter on the basis of the formatter specifying information, (d) searching for information on a plurality of contents to be displayed on the page template, and (e) generating page information on the arrangement of the contents on the basis of information indicating the direction of arrangement contained in the display attributes.
According to another aspect of the invention, there is provided a display information fixing apparatus for transmitting page information to an information terminal having a display screen and an input unit, comprising:
(a) an apparatus for analyzing a page template specified by a display information acquisition request from the information terminal, (b) an apparatus for acquiring from the page template formatter specifying information and display attribute information, (c) an apparatus for acquiring a formatter on the basis of the formatter specifying information, and (d) an apparatus for processing, on the basis of the display attributes, contents to be incorporated into the page template and generating page information to be displayed on the display unit of the information terminal.
According to another aspect of the invention, there is provided a display information fixing apparatus for transmitting page information to an information terminal having a display screen and an input unit, comprising:
(a) an apparatus for analyzing a page template specified by a display information acquisition request from the information terminal, (b) an apparatus for acquiring formatter specifying information from the page template, (c) an apparatus for acquiring a formatter on the basis of the formatter specifying information, and (d) an apparatus for transmitting a formatter, together with the page template, to the information terminal to process, on the basis of the display attributes, contents to be incorporated into the page template and generating page information to be displayed on the display unit of the information terminal.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting page information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, and (d) a program code for instructing processing of contents to be incorporated into the page template on the basis of the display attributes and generation of page information to be displayed on the display apparatus of the information terminal.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, (d) a program code for instructing acquisition of information on a plurality of contents to be displayed on the page template, and (e) a program code for instructing, if it is judged that the display attributes include one indicating rotation, generation of page information including information on a first content among the plurality of contents and, after the lapse of a prescribed length of time, generation of page information including information on a second content among the plurality of contents.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, (d) a program code for instructing acquisition of information on a plurality of contents to be displayed on the page template, and (e) a program code for instructing exclusion, if it is judged that the display attributes include one indicating random, of information on a first content among the plurality of contents and generation of page information including information on a second content among the plurality of contents.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, (d) a program code for instructing acquisition of information on any content to be displayed on the page template, (e) a program code for instructing acquisition of size information on a display area predefined to display the content from the page template, (f) a program code for instructing comparison of the size information on the display area with the size information on the acquired content, and (g) a program code for instructing, if it is judged that the size information on the display area has a greater value than the size information on the acquired content and the display attributes include one to instruct adjusted displaying, adjustment of the size of the display area to the size of the content and for generating page information.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, (d) a program code for instructing searching for information on a content to be displayed on the page template, (e) a program code for instructing, if it is judged that there is no content to be displayed, judgment of whether or not information on default contents is defined in the page template, and (f) a program code for instructing, if any information on default contents exists, generation of page information including the information on default contents.
According to another aspect of the invention, there is provided a storage medium storing thereon a display information fixing program to be executed on a display information fixing apparatus for transmitting display information to an information terminal having a display screen and an input unit, the program comprising:
(a) a program code for instructing analysis of a page template specified by a display information acquisition request from the information terminal, (b) a program code for instructing acquisition of formatter specifying information and display attribute information on a formatter to control the arrangement of a plurality of contents from the page template, (c) a program code for instructing acquisition of a formatter on the basis of the formatter specifying information, (d) a program code for instructing searching for information on a plurality of contents to be displayed on the page template, and (e) a program code for instructing generation of page information on the arrangement of the contents on the basis of information indicating the direction of arrangement contained in the display attributes.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention and for further advantages thereof, reference is now made to the following Detailed Description taken in conjunction with the accompanying Drawings, in which:
FIG. 1 is a block diagram of one embodiment of hardware configuration of an information terminal, web server and client machine according to the present invention;
FIGS. 2A and 2B are a block diagram of processing elements in a preferred embodiment of the invention;
FIG. 3 is a conceptual diagram illustrating the state transitions of parts in the preferred embodiment of the invention;
FIG. 4 shows message flows in a contents registration procedure in the preferred embodiment of the invention;
FIG. 5 shows message flows in a page template registration procedure in the preferred embodiment of the invention;
FIG. 6 shows message flows in a formatter object registration procedure in the preferred embodiment of the invention;
FIG. 7 is a conceptual diagram for describing a page template in the preferred embodiment of the invention;
FIGS. 8A and 8B show message flows in a part creation procedure in the preferred embodiment of the invention;
FIG. 9 shows message flows in a part creation procedure in the preferred embodiment of the invention;
FIG. 10 is a conceptual diagram illustrating the page designer's screen configuration in the preferred embodiment of the invention;
FIG. 11 shows message flows in a parts arrangement procedure in the preferred embodiment of the invention;
FIG. 12 shows message flows in a parts arrangement procedure in the preferred embodiment of the invention;
FIG. 13 shows message flows in a procedure of adding parts to a display area in the preferred embodiment of the invention;
FIG. 14 is a conceptual diagram of a part selection panel in the preferred embodiment of the invention;
FIG. 15 shows message flows in a schedule definition procedure for arranged parts in the preferred embodiment of the invention;
FIG. 16 shows message flows in a publishing decision procedure for contents to be embedded into a display area in the preferred embodiment of the invention;
FIGS. 17A and 17B show message flows in a generating procedure for contents to be embedded into a display area in the preferred embodiment of the invention;
FIG. 18 shows message flows in a generating procedure for contents to be embedded into a display area in the preferred embodiment of the invention;
FIG. 19 is a diagram illustrating one example of a code to define a display area in the preferred embodiment of the invention;
FIG. 20 is a conceptual diagram of an arrangement rule DB in the preferred embodiment of the invention;
FIG. 21 is a conceptual diagram of a component DB in the preferred embodiment of the invention;
FIG. 22 shows message flows in a procedure of shaping contents by a formatter in the preferred embodiment of the invention;
FIG. 23 is a conceptual diagram of a formatter in the preferred embodiment of the invention;
FIG. 24 is a diagram illustrating one example of parameters to be set in a display area;
FIG. 25 is a diagram for describing arrangement of parts in a display area;
FIG. 26 is a flowchart of a formatter process where a standard banner form is designated in the preferred embodiment of the invention;
FIG. 27 is a flowchart of a formatter process where a standard banner form is designated in the preferred embodiment of the invention;
FIG. 28 is a diagram illustrating one example of parameters to be set in a display area;
FIG. 29 is a diagram for describing arrangement of parts in a display area;
FIG. 30 is a diagram for describing arrangement of parts in a display area;
FIG. 31 is a flowchart of a formatter process where a banner flow form is designated in the preferred embodiment of the invention;
FIG. 32 is a flowchart of a formatter process where a banner flow form is designated in the preferred embodiment of the invention;
FIG. 33 is a conceptual diagram for describing creation of an array of parts in the preferred embodiment of the invention;
FIG. 34 is a conceptual diagram for describing creation of an array of parts in the preferred embodiment of the invention;
FIG. 35 is a conceptual diagram for describing creation of an array of parts in the preferred embodiment of the invention;
FIG. 36 shows message flows in an event monitor registration procedure in the preferred embodiment of the invention;
FIG. 37 shows message flows in a campaign definition procedure in the preferred embodiment of the invention;
FIG. 38 is a conceptual diagram of an arrangement rule DB in the preferred embodiment of the invention;
FIG. 39 shows message flows in an event subscription procedure in the preferred embodiment of the invention;
FIG. 40 is a conceptual diagram showing information managed by a user management DB in the preferred embodiment of the invention;
FIG. 41 is a conceptual diagram showing items managed by a subscription DB in the preferred embodiment of the invention;
FIGS. 42A and 42B show message flows in an event monitoring and notification procedure in the preferred embodiment of the invention;
FIG. 43 is a prior art for embedding contents into a page template; and
FIG. 44 is a prior art for embedding contents into a page template.
DETAILED DESCRIPTION OF THE INVENTION
A. Hardware configuration
FIG. 1 shows a schematic view of hardware configuration for realizing an information terminal 110 , a web server 120 and a client machine 130 (See FIGS. 2A and 2B , collectively FIG. 2 ) according to the present invention. The information terminal 110 , the web server 120 and the client machine 130 include a central processing unit (CPU) 1 and a memory 4 . To the CPU 1 and the memory 4 are connected hard disk units 13 and 31 as auxiliary memory units via a bus 2 and the like. Floppy disk units (or medium drive units 26 , 28 , 29 and 30 such as MOs 28 or CD-ROMs 26 and 29 ) 20 are connected to the bus 2 via a floppy disk controller (or various controllers including an IDE controller 25 and an SCSI controller 27 ) 19 .
Into the floppy disk unit (or medium drive units 26 , 28 , 29 and 30 such as MOs and CD-ROMs) 20 are inserted floppy disks(or media such as MOs or CD-ROMs), and these storage media such as floppy disks or the hard disk unit 13 , the ROM 14 or the like can record, working in concert with an operating system, computer program codes for giving commands to the CPU and the like and implementing the invention, and they are executed by being loaded into the memory 4 . These computer program codes can be compressed or divided into a plurality to be recorded into a plurality of media.
The information terminal 110 , the web server 120 and the client machine 130 can further be put together into a system provide with user interface hardware, and this user interface hardware would include, for instance, a pointing device (mouse, joystick, track ball or the like) 7 for inputting screen position information, a keyboard 6 for supporting key inputting, and displays 11 and 12 for presenting image data to the user. A loudspeaker 23 receives audio signals from an audio controller 21 via an amplifier 22 , and outputs them aurally.
These information terminal 110 , web server 120 and client machine 130 can communicate with other computers or the like via a serial port 15 and a modem or a communication adapter 18 , such as a token ring.
The present invention can be implemented with a conventional personal computer (PC), a workstation, or a computer incorporated into a household electrical appliance such as a television receiver or a facsimile machine, or a combination thereof. However, these constituent elements are cited merely as examples, but all these constituent elements are not indispensable for implementation of the invention. Particularly, since the invention is intended for dynamic alteration of contents to be embedded into a page template, such constituent elements as the audio controller 21 , the amplifier 22 and the loudspeaker 23 are dispensable in some modes of carrying out the invention.
The operating system on the side of the information terminal 110 , the web server 120 and the client machine 130 is not limited to any specific operating system environment, but realization is possible with what supports GUI multi-window environment as a standard function, such as Windows NT (a trademark of Microsoft), Windows 9x (a trademark of Microsoft), Windows 3.x (a trademark of Microsoft), OS/2 (a trademark of IBM), MacOS (a trademark of Apple), or Linux (a trademark of Linus Torvlds) or X-WINDOW system (a trademark of MIT) on AIX (a trademark of IBM), one for a character base environment such as PC-DOS (a trademark of IBM) or MS-DOS (a trademark of Microsoft), a real time OS such as OS/Open (a trademark of IBM) or VxWorks (a trademark of Wind River Systems, Inc.) or an OS incorporated into a network computer such as Java OS.
B. System configuration
FIG. 2 is a functional block diagram illustrating the system configuration of a system including a web page generating system in a preferred embodiment of the present invention.
In the preferred embodiment of the invention, in an information terminal 11 is installed a web browser 111 . The web browser 111 designates URL, and transmits an HTTP request to a prescribed web server 120 . It also receives a response transmitted from the web server 120 , and displays it on a display screen.
On the other hand, the web server machine 120 in the preferred embodiment of the invention is provided with a formatter 121 , a display area contents creator 123 , a schedule engine 125 , a web server program 127 , an e-mail sender 151 , an event monitor 153 , a subscription receiver 155 and a subscriber DB manager 157 .
The formatter 121 formats contents into a prescribed form on the basis of attribute information in which various resources are set in a display area to be described below (including the display position, height, width, style and format).
The display area contents creator 123 searches an arrangement rule DB for candidates of contents to be embedded into a page template, and pinpoints contents to be displayed out of the candidates according to such conditions as schedule and customer cell. It also hands over to the formatter 121 the contents to be displayed and information set in the display area, receives formatted contents, embeds them into the page template, and returns them to the web server 127 .
The schedule engine 125 judges whether or not the time of accessing by the user satisfies the conditions of schedule definition. The schedule definition can also set conditions combining such items as the day of the week and the time range in addition to the period.
The subscription receiver 155 provides the user with a list of published event parts registered with an arrangement rule DB manager 143 to be described below, and registers into a subscriber DB 157 the ID, condition formula and notification form of the parts selected by the user, together with user information extracted from a user management DB 159 .
The event monitor 153 periodically monitors the contents of this subscriber DB 157 to check external or internal resources to be monitored (the external web server 115 in the illustrated example). If the checked resource meets a prescribed condition, accesses the subscriber DB 157 with that condition as the key, references the notification form, and executes processing matching the notification form.
The e-mail sender 151 takes out e-mail parts from the arrangement rule DB 143 in response to an instruction from the event monitor 153 , generates an e-mail by embedding prescribed information, and transmits it. The user management DE 159 manages customer information.
The client machine 130 is provided with a template parser 131 , a resources manager 133 , a resources DB manager 135 , a page designer 137 , a component DB manager 141 , and an arrangement rule DB manager 143 .
The template parser 131 analyzes the page template, detects a display area contained in the page template, and extracts its attributes (including the display position, height, width, style and format).
The resources manager 133 provides the operator with a GUI for registering/altering/deleting JavaBeans. In the preferred embodiment of the invention, objects such as the page template, banner, Telop and button, and the customer cell (where the contents to be displayed vary with the user, a user group for whom different information is to be displayed is called a customer cell) are also registered into the resources DB as JavaBeans. Each Bean has a Java object code and attributes, and the Java object code is caused to be executed and a list of attributes held by the Bean to be taken out by making an inquiry with a common interface. In the case of a banner Bean for instance, it has such attributes as the type of Bean, part name, image file to be displayed, URL of link destination, and explanatory statement. In the preferred embodiment of the invention, the page template is also registered as a JavaBean in order to enhance versatility.
The resources DB manager 135 manages the resources DB. The resources DB manages parts before attribute information is set. In the preferred embodiment of the invention, for a part managed by the resources DB, only its type (as to the page template, Telop, banner and so forth) and bibliographical items are registered, but no substantive attributes such as what kind of image is to be displayed are registered. This configuration contributes to increasing the speed of retrieval among other advantages.
The component DB manager 141 manages the component DB. The component DB manages attribute information on parts. Where the part is a banner Bean for instance, it manages such items of information as the part name, image file to be displayed, URL of link destination, and explanatory statement.
The arrangement rule DB manager 143 manages the arrangement rule DB. The arrangement rule DB stores information to associate display areas with parts, schedule information, and information for determining the possibility of publishing. The operator can also obtain a list of parts stored in this DB by using the page template name and the display area name as the keys.
The page designer 137 provides the operator with a GUI which makes possible for a part to undergo arrangement registration, schedule setting, and registration/alteration of publishing decision or the like.
FIG. 3 is a conceptual diagram illustrating the state transitions of parts in the preferred embodiment of the invention. In the figure, registered parts 203 (class) consist of information (metadata) registered under the management of the resources manager 133 , and permit alteration and deletion. These registered parts 203 are stored into the resources DB 135 . At this stage, for any such part, only its type (as to the page template, Telop, banner and so forth) and bibliographical items are registered, but no substantive attributes such as what kind of image is to be displayed are registered.
Set parts 205 (instance) associate registered parts 203 with set information (banner, Telop, list and so forth) according to the property of each part, and permit alteration and deletion. These set parts 205 are stored into the arrangement rule DB 143 . In this state, the set parts 205 have, if the part is a banner Bean for instance, such attributes as the type of Bean, part name, image file to be displayed, URL of link destination, and explanatory statement. The attributes are stored into the component DB. In the preferred embodiment of the invention, in setting the properties of a part, the operator can reference and select contents registered in the resources DB.
Arranged parts 207 are associated with the set parts 205 with respect to display areas, and permit deletion. The set parts 205 are stored into the arrangement rule DB 143 .
Publishable parts 209 are arranged parts having undergone schedule setting, and permit alteration and deletion. These publishable parts 209 are stored into the arrangement rule DB 143 . Published parts 211 are publishable parts having been published. They can be returned to publishable parts 209 by unpublishing operation. These publishable parts 209 are stored into the arrangement rule DB 143 . Expired parts 213 are either publishable parts 209 or published parts 211 whose schedule has expired.
Incidentally, while in the preferred embodiment of the invention information to associate a display area with parts is stored in the arrangement rule DB with a view to reducing the time required to retrieve parts arranged in a prescribed display area, the invention can as well be implemented by assigning such information to individual parts. Further, out of the parts arranged in the prescribed display area, the schedule is also held incidental to individual arranged data in the arrangement rule DB to reduce the time taken to determine what satisfies the schedule condition, the invention can also be implemented by assigning this information to individual parts. Similarly, information on whether or not a given part is published is managed by the arrangement rule DB, it may as well be managed by the component DE as attributes of part.
Whereas each functional block shown in FIG. 2 has been described so far, these functional blocks are logical functional block, and it is not meant that each of them is realized by an integrated set of hardware or software, but they can be combined or realized by a common set of hardware or software. Especially, while the web server 120 and the client machine 130 are mounted on different machines in this embodiment, the functions described with reference to the client machine 130 can as well be assigned to the web server 120 . Further, all the functional blocks shown in this FIG. 2 are not indispensable constituent elements for the invention.
C. Procedures of operation
C-1. Registration of contents
FIG. 4 shows message flows in the contents registration procedure in the preferred embodiment of the invention. As shown in FIG. 4 , the contents creator 501 opens a resources manager main panel 503 provided by the resources manager 133 , designates created contents (in the preferred embodiment of the invention the location of the contents—URL—is designated), and registers the contents (message 5001 ).
The resources manager main panel 503 , in response to this, generates metadata 507 on the memory (messages 5002 and 5003 ). If the generation has been completed normally, the URL of the contents is registered into the metadata 507 (message 5004 ). The resources manager main panel 503 then opens a resources metadata definition panel 505 (messages 5005 , 5006 and 5007 ).
The contents creator 501 enters bibliographical items (including the creator, the date of creation and a description of contents) into this resources metadata definition panel 505 . Further in the preferred embodiment of the invention, such items as the date and hour of registration are automatically set, and the type of contents can be selected from a pulldown menu. When the contents creator 501 presses an OK button on the resources metadata definition panel 505 , metadata (including information on the link to the contents) are written into the resources DB 509 , and the inherent ID of the contents is generated and set, associated with the metadata, in the resources DB 509 (messages 5010 , 5011 , 5012 , 5013 , 5014 and 5015 ).
C-2. Registration of page template
FIG. 5 shows message flows in the page template registration procedure in the preferred embodiment of the invention. As shown in FIG. 5 , the contents creator 501 opens a resources manager main panel 503 provided by the resources manager 133 , designates a page template (in the preferred embodiment of the invention the location of the contents—URL—is designated), and registers the page template (message 5101 ).
The resources manager main panel 503 , in response to this, generates metadata 507 on the memory (messages 5102 and 5103 ). If the generation has been completed normally, the URL of the contents is registered into the metadata 507 (message 5104 ).
Next, the resources manager main panel 503 hands over the URL to the template parser 511 , and requests analysis of a display area (message 5105 ). The template parser 511 accesses the page template 250 as shown in FIG. 7 , and analyzes the display area contained in the page template 250 . In the preferred embodiment of the invention, it searches for SERVLET tags 261 and 263 contained in the HTML and, by detecting a character string ‘code=“icdacrt” ’, recognizes it as a servlet defining the display area.
If a display area is recognized, such items of information on each display area contained in a page template as the position in the sequence of display areas contained in that page template, display area name, display position, display style, width and height are recognized (message 5106 ).
Then the resources manager main panel 503 opens the resources metadata definition panel 505 (messages 5005 , 5006 and 5007 ). The contents creator 501 enters bibliographical items (including the creator, the date of creation and a description of template) into this resources metadata definition panel 505 . Further in the preferred embodiment of the invention, such items as the date and hour of registration are automatically set.
When the contents creator 501 presses the OK button on the resources metadata definition panel 505 , the resources metadata definition panel 505 writes metadata (including information on the link to the contents) and display area information recognized by the template parser 131 (such items of information as the display area number, display area name, display position, display style, width and height) into the resources DH 509 (messages 5112 , 5113 , 5114 and 5115 ).
C-3. Registration of formatter
FIG. 6 shows message flows in the formatter object registration procedure in the preferred embodiment of the invention. As shown in FIG. 6 , the contents creator 501 opens a resources manager main panel 503 provided by the resources manager 133 , designates a formatter object (in the preferred embodiment of the invention the location of the contents—URL—is designated), and registers the formatter (message 5151 ).
The resources manager main panel 503 , in response to this, generates metadata 507 on the memory (messages 5152 and 5153 ). Then the resources manager main panel 503 opens the resources metadata definition panel 505 (messages 5154 to 5156 ). The contents creator 501 enters into this resources metadata definition panel 505 the format style (designates outputting of banners in a matrix form and so forth), output type (such as HTML, FAX or PostScript), adaptable part types (banner, Telop and so forth), formatter location (the location of the program to be actually executed) and other bibliographical items (messages 5157 to 5164 ). In the preferred embodiment of the invention, such items as the date and hour of registration are automatically set.
When the contents creator 501 presses the OK button on the resources metadata definition panel 505 , the resources metadata definition panel 505 writes metadata (including information on the link to the format execution program) into the resources DE 509 (messages 5168 to 5172 ).
C-4. Setting of attributes of part (creation of part)
FIGS. 8A and 8B (Collectively FIG. 8 ) and FIG. 9 show message flows in the part creation procedure in the preferred embodiment of the invention. As shown in FIG. 8 , the web page creator 521 opens from the page designer main screen a list of set parts screen 523 (message 5201 ), and as it selects part creation (message 5202 ), a part type selection screen 525 is opened. The screen configuration of a page designer 137 in the preferred embodiment of the invention is illustrated in FIG. 10 .
As the web page creator 521 selects a part type in the parts type selection screen 525 , metadata on registered parts fitting that part type are acquired from the resources DB 135 (messages 5203 and 5204 ). Further, a distinct part ID and part name are assigned to each part type (messages 5205 , 5206 , 5207 , 5208 and 5209 ).
Confirmation of a part type by the web page creator 521 (message 5210 ) results in generation of a new part 531 (messages 5211 and 5212 ), metadata and the creator name of the registered part are set (messages 5213 to 5216 ), and a part attribute definition panel 533 is opened (messages 5217 to 5219 ).
The web page creator 521 sets on this part attribute definition panel 533 prescribed properties (a list of unregistered Telop messages, URL of link destination and so on), part name and explanatory statement (messages 5221 to 5227 ).
The web page creator 521 can as well open a contents selection panel 537 from this part attribute definition panel 533 and access images, texts and the like registered in the resources DB 527 (messages 5228 to 5234 ). If it is a banner part, for instance, a list of images to be displayed and URL of link destination among others can be obtained or, if it is a Telop part, a list of messages to be outputted can be obtained.
When the web page creator 521 selects prescribed contents from a list of contents, contents information stored in the resources DB 135 is registered as part properties (messages 5235 to 5241 ). Then, as the web page creator 521 makes final confirmation on the part attribute definition panel 533 , part information, parts ID and alteration history information are registered into the component DB 535 (messages 5242 to 5249 ).
C-5. Arrangement of parts
FIGS. 11A and 11B (Collectively FIG. 11 ) and FIG. 12 show message flows in the parts arrangement procedure in the preferred embodiment of the invention. As shown in FIG. 11 , the web page creator 531 first accesses a part selection panel 543 via a part arrangement panel 533 (messages 5301 and 5302 ), and acquires a display area in which to arrange parts registered in the resources DB 537 (messages 5303 and 5304 ). Then it acquires attribute information (including the display position, height, width, style and format) on the display area (messages 5305 and 5306 ).
In the preferred embodiment of the invention, items of attribute information on a display area include what is known as a display area style. This display area style is an item of attribute information to designate the form of displaying a part (by using HTML) selected (according to the conditions of cell and schedule). Available display styles include, for instance, bannerFlow and itemizedList.
With each display style, the type of display-shapable parts is associated in advance by a resources manager. For instance, Banner part (image file with a link) is associated with the bannrFlow style, and LisIitem part (1 line text with a link), with itemizedList. In the preferred embodiment of the invention, this association is designated when a formatter to generate HTML according to each display style is registered with a resources manager.
A list of parts that can be pasted in a display area shows the type of parts displayable in the display area, selected out of set parts on the basis of information associating a display area style with displayable part types (messages 5303 to 5331 ).
Then, as the web page creator 531 selects a desired part out of this list, the part is associated with a display area, and the association is stored into the arrangement rule DB 553 .
C-6. Addition of parts to display area
FIG. 13 shows message flows in the procedure of adding parts to a display area in the preferred embodiment of the invention. In the preferred embodiment of the invention, there is a separate GUI panel for selecting and associating display areas and parts as illustrated in FIG. 14 . When a display area 621 is selected from this display area list 630 on this panel and a “parts arrangement” button 643 is pressed, messages 5301 to 5331 in the sequential FIGS. 11 and 12 are processed. FIG. 13 shows subsequent message flows.
When the web page creator 541 selects a prescribed part out of the parts list displayed on the part selection panel 543 (message 5401 ), an arranged object 545 is newly generated on the memory. Then, a part ID and a display area ID are set on this generated arranged object 545 (messages 5404 to 5409 ), and written into the arrangement rule DB (messages 5410 to 5414 ).
C- 7 . Schedule definition
FIG. 15 shows message flows in the procedure of schedule definition of arranged parts in the preferred embodiment of the invention. As illustrated in FIG. 15 , the web page creator 551 first designates a set of a display area and parts in the parts arrangement panel 553 , opens a schedule definition panel 555 (messages 5501 and 5502 ), and accesses an arranged part to undergo schedule registration (revision) by the web page creator 551 (messages 5503 and 5504 ).
If that arranged part is not published, a schedule currently set for the part is acquired to newly set or alter a schedule (message 5505 ). If no schedule is set, a schedule registration screen with no data thereon will be outputted or, if a schedule is already set, there will emerge a schedule revision screen. In the preferred embodiment of the invention, no schedule alteration can be done unless no part is published (in an unpublished state). This is intended to prevent a part display schedule from being changed when general users are watching it.
C-8. Publishing decision
FIG. 16 shows message flows in the procedure of publishing decision on contents to be embedded into a display area in the preferred embodiment of the invention. As illustrated in FIG. 16 , as the web page creator 571 designates a display area and parts on a part arrangement panel 573 and designates publishing, a publish flag is set on an arranged object 575 (messages 5701 to 5703 ), and the contents of the arranged object are written into the arrangement rule DB. Cancellation of publishing (unpublishing) can be designated in a similar procedure.
C-9. Generation of contents for display area
FIGS. 17A and 17B (Collectively FIG. 17 ) and FIG. 18 show message flows in the procedure of generating contents to be embedded into a display area in the preferred embodiment of the invention. As illustrated in FIG. 17 , as a user 561 transmits an HTTP request from the web browser 111 to the web server 127 , the web server 127 acquires a page template matching that HTTP request.
The web browser 127 detects a servlet tag contained in the page template, hands over a code ( FIG. 19 ) contained in the servlet tag to the display area contents creator 123 (message 5601 ), and stands by until the result is received.
Then the display area contents creator 123 acquires a display area (messages 5602 and 5603 ), and acquires metadata of a template containing that display area from the resources DB 567 (messages 5604 and 5605 ). In the preferred embodiment of the invention, display areas are managed by a display area name 701 , and the resources DB 567 and the arrangement rule DB 565 can be accessed with this display area name 701 as the key.
With these display area name 701 and page template ID 725 (acquired by message 5605 ) as the keys, the arrangement rule DB of this display area is accessed, and arranged objects are acquired (messages 5606 and 5607 ). Incidentally, while arranged objects are acquired with the display area name 701 and the page template ID 725 as the keys in the preferred embodiment of the invention, they can as well be accessed with only the display area name as the key by providing a display area name that can uniquely specify every page template.
In the example of FIG. 20 , arranged objects 0001 and 0002 are acquired. Schedule information pieces 727 and 728 are taken out of these acquired arranged objects (messages 5608 and 5609 ), and a schedule engine 571 is inquired of about their validity (messages 5610 and 5611 ). It is further checked whether or not their parts are published (messages 5612 and 5613 ). In the example of FIG. 20 , both the arranged objects 0001 and 0002 are published. Incidentally, supposing that the current date and hour are 19:00 on Jul. 26, 1999, in the example of FIG. 20 , the arranged object 0001 does not meet the schedule condition while the arranged object 0002 does meet the schedule condition.
If it is judged that the scheduled is a valid one and a published part, a component DB 575 is accessed, and such items of information matching that part as the display image file, URL of link destination and explanatory statement are acquired (messages 5714 and 5715 ).
FIG. 21 is a conceptual diagram of the component DB in the preferred embodiment of the invention. In the preferred embodiment of the invention, a banner 750 , list item 760 , Telop 770 and so forth are registered as objects, instead of a simple table, to match a plurality of types of objects. Contents information items such as items of information to specify the display image of a banner (the bus name, directory name and file name) are set as properties of a banner object 750 . The system can acquire contents information and make available to itself image information and the like by making an inquiry with the part name or the part ID as the key.
Referring back to FIG. 17 , a display area contents creator 563 acquires display attributes 703 ( FIG. 19 ) (message 5616 ) and, using a formatter 577 , shapes the contents to adapt them to the display area (messages 5617 to 5631 ).
FIG. 22 shows message flows in the procedure of shaping the contents by the formatter in the preferred embodiment of the invention. As shown in FIG. 22 , the display area contents creator 563 takes out of formatter metadata 578 a format style registered as a category, compares it with the style of the display area, and judges whether or not those contents can be displayed (messages 5651 to 5653 ). It further takes out the type of output registered as a subcategory of metadata, and checks if the output form is HTML (messages 5654 to 5656 ).
While the formatter to be used is thus specified according to the type of part or output means such as the banner (standard), (a plurality of) banners, Telop and list item in the preferred embodiment of the invention, it is also acceptable to adopt a method by which the formatter is specified by using an ID which uniquely identifies a specific formatter or a method to specify a formatter by calculating a prescribed assessment value.
Then, information indicating the location of an actual format program (Identifier) is acquired from metadata 578 (messages 5657 and 5658 ), and a format program is loaded on the basis of that information (message 5659 ). This loaded format program is defined as the formatter to be used for this processing (messages 5660 and 5661 ).
FIG. 23 is a conceptual diagram of a formatter 780 in the preferred embodiment of the invention. As illustrated, it has a parameter defining section (setStyleParm), width defining section (setWith), height defining section (setHight), overfull processing defining section (setoverfull), underfull processing defining section (setUnderfull) and format processing defining section (render).
The parameter defining section is a portion wherein a parameter received for each formatter is defined. The width defining section and the height defining section are portions where the size of a display area is acquired. The overfull processing defining section is a portion to acquire the type of processing to be performed when the size of any part to be displayed in a display area is greater than the display area, while the underfull processing defining section is a portion to acquire the type of processing to be performed when the size of any part to be displayed in a display area is smaller than the display area. The format processing definition section (render) is information to specify the location of the actual format program.
This formatter is such that, where for instance the definition in the display area is in a standard banner form (banner is set as the style) as shown in FIG. 24 , the four banners to be displayed are replaced every two seconds in the display area as shown in FIG. 25 if, in an overfull case, the rotation is to take place at two second intervals (rotation=2 is set in partsOverful).
Further, as “shrink” is set in partsUnderful, when the size of any part to be displayed in a display area is smaller than the display area, the display area is displayed in a size shrunken to the size of the banner. Moreover, since an image is set on “default,” the image defined here is displayed if there is no banner to be displayed.
FIGS. 26 and 27 are flowcharts showing the formatter process where a standard banner form is designated in the preferred embodiment of the invention. First, the formatter acquires the number of parts (step 401 ), and checks that number of parts. In one aspect of the present invention, whereas the number of parts registered corresponding to a display area in the arrangement rule DB 720 and whose display conditions 727 to 729 have prescribed values matches the number of parts, in one aspect of the invention the contents to be displayed in a specific display area are stated in a bus name and the like in a fixed manner, and the number of such statements, or the number of contents as the result of acquisition thereby accomplished, corresponds to the number of parts.
In order to judge that the number of parts is smaller than one (the number of parts=0) (step 403 ), first the control command of partsUnderful is checked. If “none” is designated as the control command of partsUnderful (step 407 ), an HTML containing a blank area of a designated size is generated, and it is handed over to the display area contents creator 123 (step 407 ).
If “shrink” is designated as the control command of partsUnderful or there is no particular designation (in the preferred embodiment of the invention, partsUnderful=shrink is default), it is further judged whether or not a default display image is designated (step 409 ). If a default display image is designated, an HTML including bus information designated for default is generated, and handed over to the display contents creator 123 (step 411 ). If no default display image is designated, the absence of output information is notified back to the display contents creator 123 (step 413 ).
On the other hand, if the number of parts is judged to be l (step 421 ), an HTML to display the contents of the part in an area of a designated size is generated, and handed over to the display area contents creator 423 (step 423 ).
If the number of parts is judged to be more than one (step 421 ), it is further checked whether or not partsOverfull contains a command instructing rotation (step 425 ). If PartsOverfull contains designation of random, or if there is no particular designation (in the preferred embodiment of the invention, random is default), one part is selected out of a plurality of parts at random (step 427 ), an HTML to display the contents of parts within an area of a designated size is generated, and handed over to the display area contents creator 423 (step 423 ).
If it is judged that partsOverfull contains a command to instruct rotation, parts are selected in succession (step 429 ), an HTML to display the contents of the parts in an area of a designated size is generated, and handed over to the display area contents creator 423 (step 431 ). Then, after standing by for a prescribed length of time included in the rotation command, step 429 and step 431 are repeated (step 433 ). Incidentally, while a command to generate a time out is transmitted, in the preferred embodiment of the invention, from the web server 120 side between step 431 and step 433 to instruct the browser 111 to perform replotting, it is also acceptable to transmit a formatter logic to the browser 111 side as JavaScript or the like and to let a replotting event be generated on the browser 111 side.
On the other hand, in a form wherein a plurality of banners are displayed side by side (bannerFlow is set as the style) as shown in FIG. 28 , if, in an overfull case, the rotation is to take place at two second intervals (random is set in partsOverful) the four banners to be displayed, as shown in FIG. 29 , are placed in sequence from the top left of the display area and, when the width of the display area is overstepped, shift to a stage below to be displayed. Incidentally, in this example, the direction in which the banners are placed is horizontal and the background color is set to be gray. If the direction is set to be vertical, the banners can as well be placed in a vertical direction as illustrated in FIG. 30 .
FIGS. 31 and 32 are flowcharts showing a formatter process in which a banner flow form is designated in the preferred embodiment of the invention. First the formatter acquires the number of parts (step 441 ), and checks that number of parts. If the number of parts is judged to be smaller than one (the number of parts=0) (step 443 ), it is further judged whether or not a default display image is designated (step 481 ). If a default display image is designated, an HTML including path information designated for default is generated, and handed over to the display contents creator 123 (step 483 ). If no default display image is designated, the absence of output information is notified back to the display contents creator 123 (step 485 ).
If there is any part to be displayed, an array of parts to display (the contents of) every part is created (step 445 ). This array of parts constitutes data to designate which part is to be arranged on which line in which row. FIG. 33 is a conceptual diagram for describing the creation of an array of parts at step 445 in the preferred embodiment of the invention.
The formatter first confirms that the direction of arrangement is horizontal and that the width of the display area is not smaller than the width of the parts. Then it acquires parts in succession, and allocates those parts to a position (n, m) (both are 0 in initial value). It checks whether or not the total of the widths of the parts surpasses the width of the display area and, if it does not, allocates the parts to that position, and raises m to m+1. If the total of the widths of the parts surpasses the width of the display area, with n being raised to n+1 and m reduced to 0, those parts are allocated to that position, and m is raised to m+1. This procedure is repeated for all the parts, and the maximum values of n and m are acquired. The size of the array of parts will be the part width×m and the part height×n. Further, by comparing the part height×n with the display area height every time n is incremented by one, the appropriate number of parts to be accommodated by the display area can also be acquired. The array of parts in the vertical direction can be created in a similar procedure.
Then it judges whether or not the height of the display area is in sufficient (in the case of arranging in the horizontal direction) or the width of the display area is in sufficient (in the case of arranging in the vertical direction) as a result of (or in the process of) arraying the parts (step 447 ). If it is judged that the display area is not too small, it is further judged whether or not there is a surplus height of the display area (in the case of arranging in the horizontal direction) or there is a surplus width of the display area (in the case of arranging in the vertical direction) (step 449 ). If it is judged that the size of the array of parts is appropriate for the display area, an HTML to display that array of parts is generated, and handed over to the display contents creator 123 (step 451 ).
If it is judged that the display area is too large, the control command of partsUnderful is checked. If “none” is designated as the control command of partsUnderful (step 455 ), an HTML to display the array of parts in a display area of the designated size is generated, and handed over to the display area contents creator 123 (step 407 ). If “shrink” is designated as the control command of partsUnderful, or if there is no particular designation (in the preferred embodiment of the invention, partsUnderful shrink is default), an HTML to reduce the designated size of the display area and display the array of parts is generated, and handed over to the display area contents creator 123 (step 457 ).
On the other hand, if it is judged at step 447 that the display area is too small, the control command of partsoverful is checked. It is checked whether or not a command instructing rotation is contained as the control command of partsoverful (step 461 ).
If it is judged that partsOverfull contains a command instructing rotation, the parts are selected in succession to re-create an array of parts (step 463 ). FIG. 34 is a conceptual diagram for describing the creation of an array of parts at step 463 in the preferred embodiment of the invention. As illustrated, parts in the appropriate number of parts acquired at step 445 are selected in succession, and an array of parts is created by the method described with reference to FIG. 33 . After the lapse of a designated length of time, parts in the appropriate number of parts are selected in succession from the next part onward to re-create an array of parts.
Then, an HTML to display the contents of the array of parts in a display area of the designated size is generated, and handed over to the display area contents creator 423 (step 465 ) and, after standing by for a prescribed length of time included in the rotation command, step 429 and step 431 are repeated (step 467 ).
If partsoverfull contains no designation of rotation at step 461 , it is further checked whether or not the control command of partsOverful contains “expand” (step 471 ).
If “expand” is contained in partsoverfull, an HTML to expand the designated size of the display area and display the array of parts is generated, and handed over to the display area contents creator 123 (step 473 ), if “random” is designated by partsoverfull or if there is no particular designation (in the preferred embodiment of the invention, random is default), parts in a number to be appropriately arranged in the display area are selected out of a plurality of parts at random to create an array of parts (step 475 ).
FIG. 35 is a conceptual diagram for describing the creation of an array of parts at step 475 in the preferred embodiment of the invention. As illustrated, parts in the appropriate number of parts acquired at step 445 are selected at random, and an array of parts is created by the method described with reference to FIG. 33 . Then, an HTML to display the contents of the array of parts in a display area of the designated size is generated, and handed over to the display area contents creator 423 (step 477 ).
D. Example of application to campaign using Internet
An aspect to alter the information to be displayed for a prescribed user in accordance with the circumstances of external resources and an aspect of notification in combination with e-mail will be described below.
D-1. Registration of event monitor, condition determining cell parts and event cell parts
FIG. 36 shows message flows in a procedure to register an event monitor in the preferred embodiment of the invention. As shown in FIG. 36 , a registrant 571 , using a resources manager 573 as in the case of FIG. 4 , can register into a resources DB 575 event monitor parts in the JavaBean form (messages 5701 and 5702 ). In an event monitor JavaBean in the preferred embodiment of the invention, there are such items as monitoring object, monitoring frequency, notification form, and path information for event cell parts.
Also, in a procedure similar to the foregoing, condition determining cell parts and event cell parts are also registered. Condition determining cell parts include the conditions of an event target (for instance, out of user information to be contained in the user management DB, conditions for categorizing a user such as a prescribed age bracket, prescribed occupation, prescribed income level and a prescribed official position and their explanatory statements are contained as the items). Event cell parts are cell parts for registering persons for whom an event is to be actually held, and hold as their items information to specify condition determining cell parts (parts ID), filtering conditions and e-mail part ID. E-mail parts include such items as “from”, “to”, contents and explanatory statement.
D-2. Definition of campaign
FIG. 37 shows message flows in a campaign defining procedure in the preferred embodiment of the invention. As shown in FIG. 37 , a campaign registrant 581 , using a prescribed screen of a page designer 585 as in the case of FIG. 8 to FIG. 12 , accesses the resources DB 575 , and acquires a list of registered event monitors (messages 5801 to 5803 ).
A campaign definer 581 selects registration of a new event monitor (message 5804 ), and registers properties from the registration screen (message 5805 ). For instance, as monitoring objects, there are set an explanatory statement allowing intuitive perception of a monitoring object (such as the stock of an information company listed in the first section of the Tokyo Stock Exchange) and information which can identify the location where that information can be acquired (URL, information to specify a particular type of data in an HTML tag). As monitoring frequencies, such items as the default value, upper limit and lower limit are set. Notification forms which are set include the presence or absence of an e-mail notification. As path information for an event cell part, the path name, directory name and file name of the published event cell part are set. It is also practicable to set a part ID.
Then, as elements of campaign rules, schedule information and information on publication or non-publication are entered (message 5807 ). Incidentally, in this aspect of generating an event depending on the situation of other resources, it is desirable that an arrangement rule DB 720 manage such information as shown in FIG. 38 . As this table shows, information including a part type 731 , event flag 733 , cell part ID 735 is added to the arrangement rule DE 720 . The part type 731 is information to distinguish the type of the part, such as a banner part, Telop part, event cell part, condition determining cell part or event monitor part. Further, the event flag 733 is a flag to determine, where subscription to be described below takes place, whether an event is validated or not, and as the cell part ID 735 is set, in the case of an event monitor part, a condition determining cell part to be used by a user having performed subscription to be described below judges whether or not prescribed conditions are met, and in other cases, an event cell part registered for persons for whom the event is actually intended is registered.
Then, a page designer 583 designates an arrangement object for an event monitor 589 to instruct starting of the event monitor for the event (message 5808 ). This causes the event monitor 589 to start monitoring the event.
D-3. Subscription to event
FIG. 39 shows message flows in an event subscribing procedure in the preferred embodiment of the invention. As shown in FIG. 39 , a user 591 desiring to subscribe to an event accesses a web page (message 5901 ). An execution run time (a component including the display area contents creator 123 and the schedule engine 125 in FIG. 2 ) accesses a user management DB 594 , and acquires a user ID with Cookie contained in the HTTP request as the key (message 5902 ).
FIG. 40 is a conceptual diagram showing items of information managed by a user management DB 740 in the preferred embodiment of the invention. As shown in the table, the user management DB 740 manages a user ID 741 , Cookie 743 , e-mail address 745 and user profile information 747 . The user profile information 747 includes information on that user including his or her age, occupation, place of work, home address and office address. In the preferred embodiment of the invention, a user registers these items of information on condition that he or she receive prescribed service on Internet. The user ID is automatically generated by the system. The system can acquire information contained in that record with the Cookie 743 and user ID as the keys.
If the execution run time 593 recognizes the uses as a registered member, it displays a list of published event monitor parts for the user (messages 5904 to 5906 ). Incidentally, if the execution run time 593 does not recognize the user as a registered member, a user registration panel can as well be outputted. Further, the preferred embodiment of the invention supposes subscription service for a membership, and it is also possible to provide subscription service for general public instead of a specific membership.
When the user has selected an event monitor, an event setting screen is displayed (messages 5907 and 5908 ). Then the user sets parameters for a condition formula and a notifying method (message 5909 ). For instance, the user can set such a condition that a notification by e-mail is desired when the stock price of Company A has risen above =Y120.00.
Then these set information and user management DB information are stored into a subscription DB 597 (messages 5910 to 5913 ). FIG. 41 is a conceptual diagram showing items managed by the subscription DB 597 in the preferred embodiment of the invention. As shown in the table, a subscription DB 750 manages a subscription ID 751 , user ID 753 , part ID 755 , condition formula 757 , notification form 758 , and campaign flag 759 . Then, if the event monitor designated by the user is not started, it is started (message 5914 ).
D-4. Monitoring and notification of event
FIGS. 42A and 42B (Collectively FIG. 42 ) shows message flows in an event monitoring and notifying procedure in the preferred embodiment of the invention. As shown in FIG. 42 , a started event monitor 653 monitors a monitoring object 651 containing data varying periodically or non-periodically in a period based on set monitoring frequency information (message 6501 ). In the preferred embodiment of the invention, the event monitor 653 has information items including a monitoring object, event generating condition, monitoring frequency, subscription ID and event flag, and monitors objects whose event flag is on. Incidentally, in the preferred embodiment of the invention, there further is a monitor part to monitor the event monitor, turning off the event flag 733 ( FIG. 38 ) whose schedule has ended and notifying the event monitor 651 of that action.
Then, if the event monitor 651 finds that the event generating condition has been met, it accesses a subscription DB 655 and returns a user ID and part ID matching the subscription ID (messages 6502 and 6503 ). Then, the event monitor 653 accesses an arrangement rule DB 657 with the part ID as the key, and acquires a condition determining cell part ID 735 ( FIG. 38 ). It further accesses the component DB, takes out a determining condition for condition determining cell parts, compares it with the user profile of the user management DB, and judges whether or not it is an object of the campaign (messages 6504 and 6505 ).
If the user is judged to be a target of the campaign, an event cell part matching the condition determining cell part is taken out, and the user ID or Cookie of that user is registered into that event cell part (message 6506 ). It is also possible to register only those users having designated a web in the notifying form.
Then, if the notification form 758 taken out of the subscription DB designates e-mail, the event monitor 653 hands over the ID of the e-mail part registered in the event cell part and the user ID to the execution run time 659 (message 6507 ).
The execution run time 659 accesses the e-mail part, acquires an e-mail sender (From) (messages 6508 to 6511 ), and requests an e-mail sender 663 to send the e-mail together with the user ID (message 6512 ).
The e-mail sender 663 accesses a user management DB 665 , acquires an e-mail address from the user ID, generates an e-mail on the bases “from” and contents information held as a property by the e-mail part, and transmits the e-mail (message 6515 ).
And, if this user has transmitted an HTTP request asking for a prescribed page template, the processing described with reference to FIGS. 17 and 18 is executed. Then, an arrangement object used for this processing judges the event flag 733 and cell part ID 735 shown in FIG. 38 , together with the schedules 727 and 728 and publish flag 729 as display conditions. In such a case, a cell part in which this user is registered is designated in the cell part ID 735 by message 6506 of FIG. 42 , and the event flag is also set to be on, so that an HTML to display prescribed parts (banner) in the display area is acquired.
Thus, since shaping of a banner part has been taken up in describing the preferred embodiment of the invention, its formatter performs shaping (to fit the size of contents) of a display area, outputting of a default image, control of the background color, selection of the contents to be displayed, and control of the displaying sequence, display position, display time and display method of contents, but in the case of a formatter shaping a Telop part, it can also control the scrolling speed, font name, font size and character color.
As hitherto described, according to the present invention, it is possible to alter contents and their layout to be embedded into a page template without obliging the manager of display information to edit any HTML file or modify server programs such as CGI. It is also made possible to dynamically alter contents and their layout to be embedded into a page template according to the circumstances of accessing by a user. It is further made possible to provide information seeming to fit each user's preference only to that particular user or a group including that user and to enhance the effect of advertisement or the like.
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A page template, which serves as the prototype of a web page, contains formatter specifying information and display attribute information. The formatter specifying information is information for specifying one formatter out of a plurality of types (banner, Telop, a plurality of banner arrangements or the like). Display attribute information is information for controlling the moves of the formatter. When a page template is called by a web browser, the formatter is actuated, and selects, arranges, or controls the display sequence, display time or the like of, contents to be embedded into the template in accordance with display attributes, or effects such controls as the reduction of a display area (an area in the template available for embedding contents) to the size of contents.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to the stabilization of pyrolysis gasoline (“pygas”), and more particularly to the first stage hydrogenation of pygas.
[0003] 2. Description of the Prior Art
[0004] Crude oil fractions such as a straight run naphtha from a crude oil still are conventionally steam cracked in an olefins unit to produce light olefins and aromatics, valuable chemicals in their own right. Pygas is a valuable by-product of such steam cracking because it is generally high octane and within the general gasoline boiling range of from about 100 to about 435° F., and can be used as a finished gasoline blending stream after undergoing certain processing before blending.
[0005] Because pygas is derived from steam cracking complex hydrocarbon streams such as naphthas, it can carry with it a large amount of widely varying catalyst poisons that interfere with the aforesaid pre-blending processing of pygas. The amount and severity of pygas poisons is unusually severe as compared to other gasoline producing streams, e.g., gasolines from catalytic cracking units. This makes pygas pre-blending processing quite detrimental to catalyst life during such processing.
[0006] Also unlike other gasoline streams used for finished gasoline blending, pygas, before first stage hydrotreating contains substantial amounts of gum precursors, and has poor oxidation stability.
[0007] Accordingly, pygas is challenging to stabilize and otherwise process before gasoline blending is undertaken.
[0008] The first stage of pygas processing before blending is often hydrotreating over a Group VIII metal catalyst (iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium, and platinum) to selectively hydrogenate gum precursors such as diolefins, acetylenics, styrenics, dicyclopentadiene, and the like while not hydrogenating significant amounts of mono-olefins, aromatics, and other gasoline octane enhancers. Competitive adsorption causes diolefins and acetylenics to be hydrogenated preferentially over mono-olefins and aromatics thus removing gum tendencies while maintaining octane value. Paraffins are left unchanged or mildly isomerized which can help gasoline value.
[0009] Sometimes several stages of selective hydrogenation are carried out.
[0010] Second stage hydrotreating is often done on a BTX (benzene, toluene, and xylenes) fraction of pygas for removal of sulfur and other impurities.
[0011] The poison severity usually found in pygas can severely reduce first stage hydrogenation catalyst activity and catalyst life. For example, while sulfur, carbonyls, basic nitrogen, and gums/coking tend to be temporary catalyst poisons, arsenic, mercury, lead, and phosphorous tend to be more permanent poisons. Other permanent poisons include trace silicon oxide and corrosion metal oxide dusts which tend to plug catalyst pores. Also polysiloxanes thermally decompose and permanently poison palladium or nickel catalysts.
[0012] Guard beds can be employed upstream of a first stage hydrotreater to remove such poisons, but this is an expensive approach, and it is not always physically possible or otherwise practical to install guard beds and regeneration capability.
[0013] Thus, it is-very desirable to have a pygas first stage hydrogenation catalyst that remains robust as to both selective hydrogenation activity and catalyst life when exposed to the pygas poison severity without resorting to a guard bed or other processing to remove or neutralize poisons before such first stage hydrotreating.
[0014] Group I B metals (gold, silver, and copper) have heretofore been used as a catalyst for the selective hydrogenation of unsaturates, see U.S. Pat. No. 5,068,477 to Berrbi. Berrbi's patent does not suggest directly or indirectly the use of promoters to make a pygas first stage hydrogenation Group VIII metal catalyst more robust to poisons carried in the pygas.
[0015] Group I B metals have also been suggested to be used with Group VIII metal on a support of silicon dioxide to remove alkynes, dienes and mono-olefins from olefin streams for polymerization over a metallocene catalyst or from pyrolysis gases produced in plastic recycling plants, see U.S. Pat. No. 6,204,218 to Flick et al. This patent also does not relate to the rendering of pygas hydrotreating catalyst more robust by the use of promoters.
[0016] European Patent No. EP O 738 549 A1 to Zisman et al. discloses a method for the selective hydrogenation of acetylene in the gas phase using a catalyst containing alkali metal, chemically bound fluorine, and a support. Zisman et al. disclose that when the atomic ratio of fluorine to alkali metal is in the range of 1.3:1 to 4:1 the catalyst is more resistant to deactivation to sulfur impurities. Zisman et al. optionally include silver in their catalyst but not as a promoter against sulfur poisons since Zisman et al. achieve their desired protection against sulfur deactivation when silver is not present in their catalyst.
[0017] U.S. Pat. No. 4,404,124 to Johnson et al. also discloses a method for the selective hydrogenation of acetylene in the gas phase using a catalyst containing palladium, silver, and alumina. Johnson et al. disclose that a high loading of the catalyst “is expected” to make the catalyst less sensitive to arsenic in the gaseous feed.
[0018] Thus, Zisman et al. and Johnson et al. 1) teach the use of silver as an active catalytic part of a catalyst for the selective hydrogenation of gaseous acetylene; 2) lead away from the use of silver as a promoter for sulfur poisons; and 3) only speculate as to the effect of silver high loading in respect of arsenic in the context of an acetylene selective hydrogenation catalyst. Further, neither of these patents suggest directly or indirectly the use of promoters to make a hydrogenation catalyst for normally liquid pygas more robust in the presence of the wide variety of poisons (which include sulfur poisons) normally found in a pygas feed.
DETAILED DESCRIPTION OF THE INVENTION
[0019] In accordance with this invention, conventional first stage pygas hydrotreating Group VIII metal catalyst is rendered more robust to the severity of poisons carried by pygas by employing said Group VIII metal on an alumina based support and adding to said catalyst at least one promoter selected from metals of Group I B (silver, gold, copper), zinc, Group VI B (chromium, molybdenum, tungsten), manganese, rhenium and/or oxides thereof. Presently preferred promoters are silver, gold, copper, and manganese in their reduced (elemental) state with the remainder of the materials being in an oxidized state. More preferred promoters include silver, gold, zinc, chromium, molybdenum, manganese, and copper. Of these preferred promoters, zinc, chromium, and molybdenum will be in the oxide form, and the others in the reduced state.
[0020] The promoter or combination of promoters is employed in an amount effective preferentially to trap at least one poison in said pygas and thereby separate same from said pygas before said poison reaches an active Group VIII metal site thereby leaving said Group VIII metal site active and available for said selective hydrogenation. Accordingly, the amount of promoter or promoters used can vary widely based on the amount, nature, and variety of poisons carried in the particular pygas being treated, but will generally be from about 0.01 to about 40, preferably from about 0.3 to about 15.0, weight percent based on the total weight of the catalyst.
[0021] The alumina based support of this invention is at least one of the group comprising alumina, deactivated alumina, amorphous silica-alumina, and crystalline silica aluminate. Silica by itself is not useful, contrary to Flick et al. cited hereinabove. Preferably all supports employed in this invention have slight or no acidity as measured by the conventional ammonia adsorption test, see Journal of Catalysis, Volume 2, pages 211-222, 1963. Still more preferably the support(s) has a Hammett function, H o in the range of −3.0 to 5.0 where H o =−log[a H *f B /f HB ]. a H is defined as proton activity of the support and f B , f HB are activity coefficients of the basic and acid forms of the support. The catalyst for the promoter can be employed on the surface of the support, in the interior pores of the support, or a combination of both.
[0022] Although some of the metals set forth above as promoters have been used as catalysts heretofore, they are not employed in a manner to serve as catalysts in this invention. Rather they are employed to serve as a promoter to maintain the Group VIII metal active to serve as the catalyst in the process of this invention. For example, when palladium is used in a catalyst according to this invention, it provides the active catalyst sites for the desired selective hydrogenation diolefins and acetylenics in the pygas. If silver was used as the promoter on a palladium catalyst, the silver would be many orders lower in activity as a catalyst than palladium or nickel and would serve primarily as a poison trap rather than as a catalyst. Similarly, if hydrogen sulfide (H 2 S) is a prevalent poison in a particular pygas, zinc is an especially efficient H 2 S getter (adsorbent) and could, pursuant to the inventive concept of this invention, be employed as a promoter along with silver, or in lieu of silver, on, for example, a palladium/alumina catalyst used in the first stage hydrotreating of that particular pygas. Also, silver or gold promoted palladium is particularly selective for the hydrogenation of acetylinics to their corresponding olefin.
[0023] The catalyst of this invention can be made in any conventional manner well known in the art. One such preparation method is the well known “incipient wetness” process wherein, for example, a salt of the catalyst metal in an aqueous solution is applied on an alumina support form such as an extrudate. The catalyst metal impregnated wet extrudate is dried, leaving catalytically active metal on the extrudate. The dried catalyst is then calcined. The active metals in the catalyst need to be reduced to their metallic state and in the case of nickel be partially sulfided in order to get the catalyst into the desired state for use in the pygas hydrotreating/stabilizing operation. The support impregnation process can be repeated as desired to add additional catalyst metals or promoters to the support. The same process steps are used to add one or more promoters of this invention to the same support. For more information for the preparation of catalysts, see Catalyst Manufacture Chemical Industries, Volume 14, published by Marcel Dekker (1983).
[0024] The feed material for this invention is any liquid phase pygas stream, whether full range or a fraction thereof, formed from any hydrocarbon steam cracking process. Such pygas feeds can have a wide variety of poisons and in varying amounts. Generally, they will have from about 30 ppb to about 500 ppm cumulative of a variety of catalyst poisons such as mercury, arsenic, lead, alkalai metal, phosphorus, silicon, iron oxide containing rouge dust (stainless steel corrosion products such as chromium oxide, nickel oxide and the like), sulfur, coke, halides (metal, particularly alkali and alkaline earth metal, chlorides, bromides and fluorides), siloxanes, sulfur containing compounds, nitrogen containing compounds, silica, carbonyls, and mixtures of two or more thereof. Mercury, arsenic, alkali metals, phosphorus, lead, iron oxide, sulfur, hydrogen sulfide, ammonia, and siloxanes are often present together in the same pygas fuel.
[0025] The particular combination of catalyst metal(s) and promoter(s) will vary widely as will the amounts of each employed on a single support depending on the hydrogenation selectivity desired and the variety and amount of poisons in the pygas feed. For example, palladium tends to be more selective for gum precursor hydrogenation and loses less octane in so doing, but it is quite vulnerable to poisons. It can be promoted with gold and/or silver to be more selective for acetylene hydrogenation and at the same time with zinc oxide if H 2 S is a particularly prevalent poison. The less acidic alumina supports of this invention reduce undesirable oligomerization reactions that lead to gums and coke fouling.
[0026] Also adding to the challenge of promoting the catalyst is that some of the poisons tend to be temporary while others tend to have a permanent poisoning effect. Temporary poisons include sulfur, carbonyls, and basic nitrogen. More permanent poisons include caustic, arsenic, mercury, lead, chlorides, phosphorous, transition metals from corrosion dust (Fe, Ni, Mn, Cr). Trace amounts of silicon as siloxanes from their use upstream as emulsion breakers can permanently poison palladium and nickel hydrogenation catalysts. Siloxanes (—O—Si(R 2 )—O—Si(R 2 )—O—), can be straight-chain or cyclic, e.g., hexamethylcyclotrisiloxane and octamethyl-cyclotetrasiloxane.
[0027] Also the tolerance of various catalyst metals to different poisons varies considerably. For example, in comparing a palladium based catalyst and a sulfided nickel based catalyst, the tolerances are (1) for siloxane, 500 ppm on 0.3 weight (wt.) % palladium versus several wt. % silicon on 12-18 wt. % NiS; (2) for arsenic and mercury, 6,000 ppm on 0.3 wt. % palladium to end of life versus 10 to 100 times more tolerance for nickel; (3) for H 2 S, temporary poison for palladium but permanent for NiS; for basic nitrogen (ammonia), 1 to 100 ppm is a temporary poison to both palladium and NiS; and (4) phosphorus and sodium tend to be permanent poisons for both catalysts.
[0028] Accordingly, it is most difficult, if not impossible, to define the amount of each promoter used with a given catalyst for a particular pygas composition, but one skilled in the art and apprised of the inventive concept of this invention can readily determine which promoter or combination of promoters and in what amount for each promoter will appropriately protect against a particular set of poisons and amount of each poison in a specific pygas feed.
[0029] Accordingly, as can be seen from the foregoing, it is particularly difficult to determine how much of the cumulative amount of poisons in a given feed will be removed but in every case a significant reduction of cumulative poisons, e.g., at least about 10 wt. % and up to about 100 wt. % based on the total weight of the cumulative poisons, will be realized, and a lengthening of the active life of the catalyst will be realized.
[0030] The operating conditions of the method of this invention will, in view of the foregoing, vary widely as well, but will generally be from about 120 to about 450° F., at from about 100 to about 500 psig, and a weight hour space velocity (WHSV) feed rate of from about 1 to about 15 h −1 .
EXAMPLE
[0031] A full boiling range liquid pygas feed having about 40 wt. % C 3 -C 10 hydrocarbons (saturates, olefins, and diolefins); about 54 wt. % of a mixture of benzene, ethylbenzene, toluene, and xylenes; and about 4 wt. % styrene, with the remainder being essentially C 11 and heavier hydrocarbons and containing about 100 ppm of a mixture of arsenic, mercury, sodium, phosphorus, organo-sulfur, H 2 S, ammonia, and siloxanes is subjected to first stage hydrogenation/stabilization in a conventional liquid phase hydrotreater.
[0032] The hydrotreater carries a hydrogenation catalyst prepared by conventional incipient wetness procedures comprising an alumina support having a Hammett acidity indicator of less Ho of about −1.0. The support carries about 0.3 wt. % palladium based on the total weight of the catalyst. The catalyst also carries elemental silver, zinc oxide, and reduced manganese as a promoter package, said package being about 3.0 wt. % of the total weight of the catalyst. The silver/zinc oxide/manganese can be present in the promoter package in a range of ratios 0-100/0-100/0-100, respectively.
[0033] The pygas feed is passed through the foregoing reduced and otherwise activated catalyst at temperatures in the hydrotreater varying from about 150 to about 300° F. at a pressure of about 380 psig, at a WHSV of about 12 h −1 .
[0034] The pygas feed leaving the hydrotreater contains about 10% less of the foregoing poisons based on the total weight of the poisons, and the active catalyst life is significantly extended by at least 10% of what it would have been had no promoter package been employed.
[0035] Thus, in accordance with the inventive concept of this invention by employing a combination of a Group VIII catalyst on an alumina based support with at least one promoter as aforesaid, pygas can be selectively hydrogenated with improved tolerance to pygas poison severity.
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A method for stabilizing pyrolysis gasoline by hydrogenating same over a Group VIII metal catalyst wherein the catalyst is promoted against poisoning by at least one metal from Groups I B, VI B, VII B, and zinc. Poisons preferentially bind with the promoters and not with the active catalytic metals.
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A microfiche appendix is included. Comprised of 1 fiche with 52 frames.
BACKGROUND OF THE INVENTION
The present invention relates to a novel glass cutting device and method for operating a motor driven glass cutting head on a platform.
Pieces of glass or lites normally employed with windows and doors are generally cut from large plates of glass. Prior art glass cutting devices have been developed to handle these large sheets of glass. For example, U.S. Pat. Nos. 3,790,003 and 3,881,618 describe tiltable glass cutting tables which may be employed to this end. The U.S. Pat. No. 3,570,733 describes a glass cutting table which employs air jets to permit the glass sheet to move easily on the top of the table.
In this regard, U.S. Pat. No. 4,171,657 describes a cutting machine which employs a cutting head movable in the X and Y directions. Drive motors fixed to a frame utilize belts which move the cutting head along predetermined paths. Also, this prior art device employs a numerical control signal to direct the cutting head in its cutting mode.
U.S. Pat. Nos. 4,331,050 and 4,380,944 describe cutting devices which employ digital computers to cut a particular material along a predetermined path. Russian Patent 727,581 discloses a moving sheet transverse cutting control apparatus which also includes a program for marking off and cutting the material. U.S. Pat. No. 4,422,149 and French Patent 2,484,393 describe cutting mechanisms which move along predetermined paths and generally have feedback systems to monitor the travel of the cutting head along the surface being cut.
Despite the advances in the prior art devices, a large amount of waste occurs in cutting glass sheets since efficient cutting of a multiplicity of lites from stock sheets of glass involves a great deal of calculating and planning. Moreover, it has been found that it is difficult to keep track of the lites which have been produced and the waste pieces which are a by-product of the cutting operations of the prior art. For example, waste pieces are often reuseable to produce desired lites but are often discarded because of the difficulty in retrieving and measuring of the same for reuse. Further, waste pieces are of a variety of sizes making categorization of the same difficult. At best, lites and waste pieces have been marked by hand after cutting which is a time consuming process.
SUMMARY OF THE INVENTION
In accordance with the present invention, a novel and useful X - Y cutting device, which especially useful for cutting glass which automatically optimizes the cutting sequence, is provided.
The glass cutting device of the present invention includes a carriage including a cutting tool which is mounted on a carriage movable across a sheet of glass to be cut. A marker is supported to the carriage and is used for applying indicia to selected portions of the glass sheet. Means is also included for controllably moving the cutting head across the glass sheet to effect cutting of the glass sheet and to effect marking portions of said glass sheet. The marker may be raised and lowered in relation to the glass sheet at selected times during the cutting process. Likewise, the cutting tool may be raised and lowered from the glass sheet, especially during the time sequence required for marking the glass sheet. Thus, the glass sheet may be cut and marked sequentially.
The present invention may also be deemed to include a method of operating a motor driven glass cutting head mounted on a glass cutting platform with the aid of a computer. The method would include the steps of providing the computer with a data base for the motor driven glass cutting head. The data base might include a list of dimensions of desired cut pieces of glass or lites (cut list), a list of dimensions of pieces of glass in stock (stock list), and in certain cases a list of dimensions of desired waste pieces of glass (cut-off list). The computer would repetitively compare the dimensions of a certain lite from the cut list to the dimensions of the pieces of glass on the stock list. Preferably, the largest lite would be compared to the stock list in order of smallest to largest. Determination is then made which stock piece should be used and if any remainder pieces of glass will result from this determination. The computer also decides the orientation and the cutting start and end points for the particular pattern of the lite from the cut list. This determination would produce a remainder piece of glass having a maximum area. At this point, any remainder pieces of glass are added to the stock list and sorted from smallest to largest in order to maximize the use of the glass available to meet the demands of the cut list. The above procedure is repeated in the computer for each lite on the cut list until a sequence of cutting events are determined. The operator would position the stock pieces designated for each cutting sequence and the computer would signal the motor driven cutting head to automatically effect the cuts.
In addition, where a list of dimensions of desired waste pieces of glass has been provided to the computer, before any cuts are performed, the computer would also determine where to fit glass pieces from the cutoff list onto the portions of the stock pieces of glass which are not being used to produce lites on the cut list. As was the case with the cut list, each piece of glass on the cut-off list is also determined as to orientation and the cutting start and end points. Further, the computer signals the automatic cutting head to make such cuts.
The method of the present invention may also be defined to include the steps of marking the pieces on the cut list and the cut-off list at some point during the cutting process. It has been found, that such marking should take place immediately before cutting of the pieces of glass from both lists.
It may be apparent that a novel and useful glass cutting device and method for cutting glass has been described.
It is therefore an object of the present invention to provide a glass cutting device which utilizes a cutting head movable in the X - Y direction on a table or platform which employs a dedicated computer permanently attached to the table programmed for both optimization of cutting and motor control.
It is another object of the present invention to provide a glass cutting device and method for cutting glass which provides for automatic labeling of each desired piece of glass and each desired waste piece of glass.
It is yet another object of the present invention to provide a glass cutting device and method for cutting glass which provides for the automatic trimming of remainder pieces into waste pieces of predetermined size and pattern.
Another object of the present invention is to provide a glass cutting device and method for cutting glass which utilizes a menu driven program having a display of the same immediately above the menu response keys on a keyboard.
Yet another object of the present invention is to provide a glass cutting machine and a method for cutting glass which achieves these goals to a higher degree of accuracy than most of the prior art devices.
A further object of the present invention is to provide a glass cutting device and a method for cutting glass which is relatively simple and inexpensive to operate and perform.
The invention possesses other objects and advantages especially as concerns particular characteristics and features thereof which will become apparent as the specification continues.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a top right side perspective view of the cutting platform and cutting head of the present invention.
FIG. 2 is a top right broken perspective view of the cutting head of the present invention in conjunction with portions of the drive means.
FIG. 3 is a sectional view of the marking portion of the cutting head of the present invention.
FIG. 3A is a sectional view of the cutting portion of the cutting head.
FIG. 4 is a top rear perspective view showing the console of the present invention with a keyboard on one surface thereof and the computer and translatry schematically.
FIG. 4A is top broken perspective view showing the console and driving motors mounted therein, the cutting head and portions of the bridge, and a schematic representation of the computer, stepping motor translators and air flow control mechanism.
FIG. 5 is a schematic view showing a typical cutting procedure for a lite.
FIGS. 6A, 6B and 6C are block diagrams representing the decisional flow chart for the software associated with the present invention.
For a better understanding of the invention reference is made to the following detailed description on the preferred embodiments of the invention which should be taken in conjunction with the hereinabove described drawings.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Various aspects of the present invention will evolve from the following description of the preferred embodiments which should be referenced to the hereinabove described drawings.
The invention as a whole is represented by character 10, FIG. 1. A platform or table 12 is shown in FIG. 1 and is generally known in the prior art. Bridge 14 extends across the table and includes a cutting head 16 which moves along the bridge in the "Y" direction. The bridge 14 itself moves along the "X" direction, which will discussed hereinafter. Bridge 14 includes a stiffening rod 18 and a structural member 20 which generally extends across table 12. An end piece 22 supports wheel 24 which supports one end of bridge 14 and permits the same to move in the X direction.
Turning to FIG. 2, it may be seen that cutting head 16 includes a yoke 26 which rides along shaft 28 by the use of ball bearings 30 (shown partially in FIG. 2). Affixed to yoke 26 is a bracket 32 which is held to timing belt 34 by the use of clamping member 36. Thus, cutting head 16 moves with timing belt 34 which is usually tensioned to eliminate slack. A cutting wheel 38 connects to a shaft 40 which is mechanically linked to boss 42. A cylindrical weight 44 affixes to boss 42 via set screw 46 to exert downward force on cutting wheel 38. Consequently, cutting wheel 38 is normally in the down or cutting position. Bearing 45 supports boss 42 and bracket 47 connects the cutting wheel assembly to yoke 26. An air cylinder 48 is fed by air line 50 and forces shaft 52 upwardly. A flange 54 fixed to the upper portion of shaft 52 contacts the underside of cylindrical weight 44 and forces the same upwardly. Thus, cutting wheel 38 would be lifted from the surface of glass piece 56.
The cutting device 10 also includes means 58 for marking indicia 60 on the surface of glass piece 56 according to a known four stroke system. Turning to FIG. 3, it may be seen that marking means 58 includes an air cylinder 72 which receives air through air line 62. A shaft, FIGS. 2,3 & 4 passes through a bearing block 68 and extends downwardly. A sheath 65 holds a marking pen 66 which has a tip that is able to mark indicia 60 according to a conventional four stroke code. Sheath 65 also surroundingly engages the end of shaft 64. Air cylinders 48 and 72 may be of the type Model F-1 1/8 X2-C, manufactured by Flairline of Livonia, Mich. Thus means 57 is provided for raising and lowering cutting wheel 38 from the surface of glass piece 56, FIG. 2A. Also, means 67 is defined for raising and lowering marker 66, FIG. 2.
Bearing block 71 fastens to bracket 47 which in turn connects to structural member 70. Thus, the entire assembly of the cutting mechanism and marking means 58 affixes to yoke 26. An oil dispenser 76 may also be employed to provide oil through oil tube 82 to cutting wheel 38. Oil tube 82 is shown partially in phantom on FIG. 3 for the sake of clarity. Cutting oil dispenser 76 may be of the type Model No. 1733-3, manufactured by Oil Write Corp. of Manitowic, Wis. Since oil dispenser 76 includes a solenoid, electrical conduits 80 are also provided to cutting head 16. A strap 78 permits oil dispenser 76 to be fastened to the top portion of bracket 32. Flexible conduit 74, known in the art, provides an enclosure for air lines 50 and 62 as well as electrical conduits 80. Flexible conduit 74 assumes a C-shape, FIG. 1, and unfurls as cutting head 16 moves across table 12 in the Y direction. Thus, it may be apparent that flexible conduit 74 and the utility conduits therein originate with console 86.
Turning to FIGS. 4 and 4A, it may be seen that console 86 includes a computer 88 having keyboard 90 visible to the operator of device 10. Computer 88 may be of the type Model Quark/100, Single Board, manufactured by Megatell Computer Corp., Weston, Ontario, Canada. Focussing on FIG. 4, it is illustrated that console 86 also houses Y direction motor means 92. A partition 94 holds stepping motor 96 to console 86. Pulley and belt mechanism 98 transfer the rotational motor imparted by motor 96 to shaft 100 held by bearing 102. A cog wheel 104 engages timing belt 34 which in turn moves cutting head 96 in the Y direction. Bearing 106 holds the other end of shaft 100 in position. Support 108 is likewise fixed to console 86, as is the case for partition 94. Shaft 28 affixes to bar 110 which in turn extends across table 12. Bar 110 includes a multiplicity of supports 112, FIG. 1, at periodic points across table 12. The end of bar 110 also affixes to console 86 and to support 108. U-shaped channel 114 and leg 116 connected to support 108 provide an anchor for stiffening rod 18. Channel 114 is fixed to console 86 in this regard.
Turning to the lower portion of console 86 on FIG. 4, it may be observed that extra action motor means 118 is also housed therein. Motor means 118 includes a stepping motor 120 which is coupled to cog wheel 122 via coupling 124. Pulleys 126 and 128, in combination with cog wheel 122 serve as contact points for timing belt 130. It should be added, that timing belt 130 is of the same type as timing belt 34 hereinbefore described. End portions 132 and 134 of timing belt 130 are firmly held to the ends of support track 136. Trolley 138 having wheels 140 is affixed to console 86 by any known means. Track 136 is affixed to table 12 at end portions 132 and 134 of timing belt 130. Stepping motors 96 and 120 may be of the type Model M112 FJ326, manufactured by the Superior Electric Co. of Bristol, Conn. As shown on FIG. 4 schematically, computer 88 feeds the appropriate signals to stepping motor translator 142. Translator 142 may be of the type Model No. TBM105-1218, manufactured by the Superior Electric Co. of Bristol, Conn. In addition, translator 142 feeds the appropriate signals to air flow control 144 of the type Model No. RFC1/8, manufactured by Flairline of Lavonia, Mich. As previously described, air lines 50 and 62 would feed air to air cylinders 48 and 72 to control the vertical position of cutting wheel 38 and marking means 58, respectively. The stepping motor translator 42 would be located with computer 88 in console 86.
Computer 88 is programmed to control the movement of cutting head 16 in relation to stock pieces of glass, such as glass piece 56 which are placed on table 12. Computer 88 optimizes the cutting of glass from stock pieces to greatly reduced waste in cutting. In addition, waste pieces may be trimmed down to desired sizes. All cut pieces of glass are identified and marked automatically by device 10. FIGS. 6A, 6B and 6C describe decisional flow charts associated with the software for operating computer 88. The object code of the software used with device 10 is enclosed herewith as an appendix to this application.
In general, the operator of device 10 imputs three lists of sizes of glass pieces as follows:
The sizes of glass desired (cut list);
The sizes of pieces of glass that are stocked (stock list);
and, the sizes of glass desired as waste pieces (cut-off list).
Using these three lists as a basis, the computer 88 displays to the operator on keyboard 90 and display 146 a menu of choices of lists. Keyboard 90 and display 146 may be of the type Model No. KB1012, manufactured by American Automatic Machines Corp. of Richmond, Calif. The operator chooses from the menu which list to alter. After selected deletions and/or additions to any of the particular lists, the operator signals computer 88 to "go" and the program appended hereto sorts the cut list and cut-off list such that pieces of glass having the largest areas are placed as the first elements of the lists. Also, preferably, the stock list is sorted such that pieces with the smallest areas thereupon are placed as the first elements of that list.
The program selectively sequences through the three lists. Starting with the smallest stock piece of glass and the largest desired cut piece of glass, i.e. lite, the dimensions are compared to determine if the desired piece can be cut from the stock piece. If the desired lite cannot fit, the next larger stock piece is compared. If the desired piece does fit on a stock piece of glass, the most optimum method of orientation in cutting the pattern is determined by calculating the areas of the pieces left after cutting. In the present invention, the optimum orientation and pattern would be based on that pattern and orientation that leaves the largest single area left over after a cutting operation. FIG. 5 shows four possibilities for cutting a lite 148 from a stock piece of glass 56, identified by reference characters 150, 152, 154 and 156. As shown in FIG. 5, possibility 152 would constitute the optimum cutting orientation since remainder piece A1 is larger than any remainder piece A1 in cutting sequences 150, 154 or 156.
The program next calculates the coordinates of the start and stop points of the cuts. Also, in this calculation, the sizes and coordinates of the pieces generated by the cuts are determined. Thus, a "pieces generated" list is carried by the program in addition to the initial lists which were fed into the computer.
The sequencing through the cut list and subsequent calculating of cuts takes into account the "pieces generated" list. Elements of that list are continually sorted such that the smallest sizes appear first thereupon. This greatly eliminates waste and cutting of the glass. Also, the repetitive comparison of pieces of glass on the cut list is also compared to the pieces generated list. The smallest generated piece will always be tried first by the program.
In effect, the sorting and sequencing may be further described as follows. The program attempts to fit the entire list of cut sizes onto the smallest size of stock that will hold them. If there are more pieces than will fit onto even the largest stock size, then the program trys to fit all the pieces from the cut list that will fit thereupon, skipping ones that won't fit, but trying every stock piece of glass.
When the cutting operation is determined by the program, a stock size to be initially loaded onto the table is shown by display 146. The computer is then started to control the cutting of the stock piece according to the determined sequence. Cutting wheel 38 actually cuts only a portion of glass piece 56, and such action may be better described as scoring. The computer also controls means 47 and 67 for raising and lowering the cutting wheel 38 and marking tip 66. Basically, when marking tip 66 is down on the surface of glass piece 56, the cutting wheel 38 is up and off the surface of glass piece 56, and vice versa. Oil dispensing means 76 releases oil when cutting wheel is in the down position only. Marking of the lites and desired waste pieces takes place, in the preferred embodiment, before any cuts are made on a blank stock piece of glass. The subject program determines the marking of each of these pieces of glass.
The cutting process described also results in the production of waste pieces of the particular sizes inputted to the computer ab initio. Thus, scrap pieces are trimmed down to uniform sizes to reduce the problems of storing a large number of sizes of waste pieces. The waste pieces may be inputted into the stock list after the cutting of each stock piece, if desired.
Stepping motors 96 and 120 are controlled by the program which calculates an internal list of starting and ending points for each cut. A linear interpolation is performed to calculate all the intermediate steps between the starting and ending points of a cut. For each intermediate point between the starting and ending point of a cut, an output signal is generated, sent to the translator 142, and from there sent to the motor to move the same.
To maximize the speed of the cuts in accordance with the power of stepping motors 96 and 120, the timing of the signals to the stepping motors is controlled such that the motors accelerate and decelerate between starting and ending points. This change in velocity is accomplished by varying the frequency with which the signals are sent to the stepping motors 96 and 120. To vary the frequency of the signal output, a series of timing delays are calculated, based on the distance from where the cutter is at the moment, to where the cutter is to go to complete the cut. The program continually monitors this "distance-to-go" distance and increases the delay (decelerates) or decreases the delay (accelerates), when the "distance-to-go" distance is less or more than the stopping distance for the cutter respectively.
As heretofore described, each cut piece and waste piece is labeled by marking means 58. This is accomplished when the program sequences through the cut list and extracts the four digit code which was inputted by the operator for each lite. From the coordinates and the code, the program generates the signals to move the cutting head 16 of device, and marking tip 66 to imprint as an indicia 60 such a four digit code. Of course, marking means 58 has been lowered to the surface of stock piece 56 while cutting wheel 38 has been raised therefrom by the use of means 67 and 57 hereinabove described.
The device 10 may be employed to cut out-of-square pieces of glass. When this occurs, one extra cut is programmed and accomplished to facilitate breaking out the desired piece of glass after the cut. Limitations such as cutting lites to a point or within one inch of the edge of the stock piece of glass have been programmed as limitations on the orientation of the particular cut and the cutting start and end points. Since the stepping motors 96 and 126 are extremely accurate in moving between steps, a very high degree of accuracy can be achieved in cutting glass with device 10.
While in the foregoing embodiments of the present invention have been set forth in considerable detail for the purpose of making a complete disclosure of the invention, it may be apparent to those of skill in the art that numerous changes may be made in such details without departing from the spirit and principles of the invention.
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A glass cutting device which is especially useful for cutting sheet glass having a motor driven glass cutting head mounted on a platform. The glass cutting head may include a marker as well as a cutting wheel for performing the functions of marking and cutting glass from a stock piece of glass. The motor driven cutting head may be controlled by a computer providing optimizing instructions to reduce waste in the cutting operation.
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There are no related patent applications.
This application was not subject to federal research and development funding.
FIELD OF THE INVENTION
The invention generally relates to a rigid holder for attaching a handgun holster onto a belt, shoulder harness or a waistband of a pair of trousers. More particularly, the holder includes several adjustment points for either changing an angle between the holder and a support belt or for changing the angle at which the holster hangs relative to the holder.
BACKGROUND OF THE INVENTION
There are several types of holster holding devices. For example, U.S. Pat. No. 5,544,794 to Nichols discloses a holster with a hanger device. The hanger device is arranged with bolts such that the height of the holster may be easily adjusted by loosening bolts and moving the holster body up or down relative to the hanger device. After a desired position has been reached, the bolts are tightened to hold the holster at the desired height.
U.S. Pat. No. 5,551,611 to Gilmore discloses a variable position handgun holster with a belt plate and a back plate. The handgun holster may be adjusted longitudinally and radially with respect to the belt plate. The back plate may be adjusted transversally to the belt plate.
U.S. Pat. No. 6,588,639 to Beletsky et al. discloses a molded holster belt loop assembly with a shelf. The belt loop assembly includes a tapered belt loop opening and a platform upon which the belt rests.
None of these prior art references teach a device that is simple to adjust, easy to maintain and cost effective to produce while providing a user with an ability to readily position a holster at a desired angle.
SUMMARY OF THE INVENTION
The invention includes a holder for securing a handgun holster or other such holster onto an article of clothing worn by a user. The holder may be formed of a substantially rigid material such as thermoplastic resin, thermoset plastics, ceramics, composites or any other combination thereof. Typically, the holder is produced through a molding process. The holder may be fastened to a belt, shoulder harness, waistband of a user's pants or other such article of clothing.
A holster attaches to the holder and may be adjustably rotated or twisted to change an angle at which the holster is held relative to the attached article of clothing. That is to say, an angle between the holster and holder may be adjusted or, alternatively, an angle between the holder and the belt may be adjusted.
In a first embodiment, the holder comprises a belt plate including two belt loops for passing a belt therethrough such that the belt is generally perpendicular to the belt plate. Belt angle adjustment means are provided in each belt loop for changing an angle between the belt and the holder. The holder also includes a holster angle adjustment means for varying an angle between the holder and the holster. The holster angle adjustment means includes a pair of formed arcuate slots and a mustache-shaped slot formed by the intersection of two arcuate slots, whose radii have center located above the mustache-shaped slot. Each slot receives a fastener, such as a bolt or screw, that passes therethrough and into the holster for securing it to the holder. These fasteners may be loosened or removed, depending on the size of the screw head relative to the indent formed in the plate wall, and the holster may be twisted to assume a desired angle between the holder and holster. The fasteners are then tightened or replaced to maintain the desired angle.
In a second embodiment, the holder includes a “clip-on” plate or paddle having a biased portion with an extension for securing the holder to a user's belt or waistband. The clip-on plate includes a U-shaped slot for accommodating a waistband, belt, purse strap or the like to secure the plate thereto. As in the first embodiment, arcuate slots and a mustache-shaped slot, receive fastening means for securing the holster to the holder in an adjustable fashion. Thus, in both the first and second embodiments, the holster may be twisted or rotated radially with respect to the holder to allow a user to adjust the angle at which the holster hangs from the wearer. The wearer may adjust the holster such that the handgrip end of the handgun is positioned to hang from the wearer at a desired angle.
In a third embodiment, three belt loops are included in the belt plate for changing an angle between the holder and the belt. Two of the three belt loops are positioned on a side of the holder in a vertical relationship with one above the other. The angle at which the holder hangs relative to the belt may be changed by removing the belt from one of the two vertically related belt loops and passing the belt through the other one.
More specifically, the present invention is directed to a holster holder for securing a holster to a wearer in a desired attitude, the holster holder including a plate, a first arcuate slot defined through the plate with a first fastening means extending therethrough, a second arcuate slot defined through the plate, opposite to the first arcuate slot, with a second fastening means extending therethrough, a third slot defined through the plate below the first and second slots, the third slot having a mustache shape and including a third fastening means extending therethrough, wherein the three fastening means are capable of engaging three points of attachment defined on a holster, and wherein the relative angle of the holster to the plate is adjustable by coordinated adjustment of the three fastening means within each of the three slots. Preferably the fastening means are screws or other commonly employed fasteners.
In one embodiment the holster holder further includes at least two further slots defined through the plate for receiving and securing the plate to a wearer's belt. Preferably, each of the at least two belt receiving slots includes adjustment means for adjusting the height and the angle at which the belt passes through the slot. In another embodiment the plate has at least three belt receiving slots defined therethrough, wherein two of the belt receiving slots are formed in a vertical manner such that one is above the other, thereby providing alternative paths for the belt through the plate, thereby providing for adjustment of the relative angle between the holster holder and the belt. For this embodiment it is also preferred that each of the belt receiving slots includes adjustment means for adjusting the height and the angle at which the belt passes through the slot.
In an alternative embodiment the plate of the holster holder includes a U-shaped slot for attachment of the plate to a portion of the wearer's clothing in a clip-on manner.
Also within the scope of the present invention is a holster holder for securing a holster to a wearer in a desired attitude, which includes a plate, a means for attaching a holster to the plate, at least two slots defined through the plate for receiving and securing a wearer's belt to the plate and adjustment means extending through each slot for adjusting the relative height and angle of the plate with respect to the belt. As above, in another embodiment the plate includes at least three belt receiving slots defined therethrough where two of the belt receiving slots are formed in a vertical manner such that one is above the other, thereby providing alternative paths for the belt through the plate, thereby providing for adjustment of the relative angle between the holster holder and the belt. In a preferred embodiment the means for attaching a holster to the plate is the arrangement of slots for adjustably receiving fasteners described above.
Thus, it is an object of the invention to provide a new and improved holder device for suspending a handgun holster from the waist, hip, leg, shoulder or other such body part of a wearer.
It is another object of the invention to provide a new and improved means for affixing a holster onto a body of a wearer. The means includes a plate with a plurality of adjusting points for allowing the holster to be positioned at a desired angle. In other words, the angle at which the free end of the handgun is orientated relative to the wearer's body may be readily changed.
Additional objects and advantages of the invention will be set forth in part in the description that follows, and in part will be obvious from the description, or may be learned from practicing the invention. The objects and advantages of the invention will be obtained by means of instrumentalities in combinations particularly pointed out in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective front view of a first embodiment of a holster holder having an adjustable position belt plate and taken from a side nearest the holster. A raised area includes arcuate slots and a mustache shaped slot for adjusting an angle between the belt plate and the holster. Belt adjusting means for adjusting the angle between the belt and the holder are shown. The belt adjusting means may raise or lower the height of the holster relative to the belt.
FIG. 2 is a perspective back view of a first embodiment of a holster holder including an adjustable position belt plate and shown from a side that is worn in contact with the wearer.
FIGS. 3 a through 3 c are perspective views of the adjustable position belt plate depicting alternative positioning of the belt plate with respect to a belt.
FIGS. 4 a and 4 b are perspective views of the adjustable position belt plate showing alternative positioning of the holster with respect to the belt plate.
FIGS. 5 a through 5 c are perspective views of the holster holder of the second embodiment and showing alternative positioning of the holster with respect to the “clip-on” plate.
FIG. 6 is a perspective view of a third embodiment of a holster holder having an adjustable position belt plate and taken from a side opposite the holster.
FIGS. 7 a and 7 b are perspective views of the holster holder of FIG. 6 and showing alternative positioning of the adjustable position belt plate with respect to the belt.
DETAILED DESCRIPTION OF THE INVENTION
FIGS. 1 through 4 illustrate a holster holder that comprises a belt plate 1 according to a first embodiment of the invention for suspending a holster 31 from a belt 33 worn by a user. Referring now to FIGS. 1 and 2 that show perspective views of opposite sides of the belt plate 1 , the belt plate 1 is formed from substantially rigid material and is generally rectangular in shape with rounded lower corners. The raised area shown in FIG. 1 is important for creating a clearance between the holster and the body of the wearer but not critical for practicing the invention.
The belt plate 1 includes two belt loops 5 for receiving a belt, not shown in FIGS. 1 and 2 . Each belt loop 5 includes a belt adjusting means comprising a combination screw 3 and nut 4 assembly that may be readily loosened and tightened to raise and lower the holster, as well as for changing the angle between the belt 33 and the belt plate 1 . While the figures illustrate the belt adjusting means as comprising roundhead or button head screws and nuts, it should be noted that various other bolt, screw and nut assemblies might be used to practice the invention. Similarly, while the figures illustrate the engagable screw head facing the wearer's clothing, alternatively, it may face outwardly for adjustment of the holster holder while being worn.
The belt plate 1 also includes a holster angle adjustment means comprising a pair of formed arcuate slots 6 , 7 and a mustache-shaped slot 8 . Arcuate slots 6 and 7 are mirror images of one another running in a substantially vertical fashion and formed near a top of the belt plate as shown. Mustache-shaped slot 8 is formed near the bottom of the plate 1 and in a substantially horizontal manner. Each slot receives a fastener 9 , such as a bolt or screw, that passes therethrough for securing the holster 31 to the belt plate 1 . These fasteners 9 may be loosened and the holster may be twisted to assume a desired angle between the belt plate 1 and the holster 31 as depicted in the later views.
As can be seen from a review of FIGS. 2 , 4 a, 4 b, 5 b, and 5 c, preferably the plate about slots 6 , 7 and 8 is formed to provide clearly defined beds for the heads of the fasteners. This curvature or indent of the plate wall is referenced at 6 ′, 7 ′ and 8 ′ in FIG. 2 and at 6 ″, 7 ″, and 8 ″ in FIGS. 5 b and 5 c. FIG. 2 illustrates an embodiment in which indents are formed about the outer edges of the slots only, while FIGS. 5 b and 5 c illustrate the preferred embodiment of fastener positioning indents surrounding the slots. Thus, incremental angles can be achieved by movement of the plate such that the fasteners are seated in positions, which are predefined by the indents. Upon tightening of the holster to the plate by tightening of the fasteners the holster position is fixed. Slippage of the tightened fasteners within the arcuate slots is precluded by the predefined indents. Depending on the relative size of the fastener head, each fastener must be loosened or removed prior to adjustment to another position.
Turning now to FIGS. 3 a through 3 c that depict use of the belt adjusting means for varying the height of the holster 31 relative to the belt 33 or changing the angle therebetween. In FIG. 3 a, holster 31 is depicted in phantom with broken lines. In this figure, the nuts 4 are positioned in the belt slots 5 below the belt 33 . This configuration forces the holster 31 upwards causing it to “ride” high on the belt 33 . In FIG. 3 b, the nuts 4 are positioned above the belt 33 to force the holster 31 to “ride” low on the belt 33 . In FIG. 3 c, the nuts 4 are positioned with one being above the belt 33 and the other below the belt 33 to change the angle at which the belt plate 1 is secured relative to the belt 33 . Thus, the angle of twist at which the holster is held may be readily varied as shown in FIG. 3 c.
FIGS. 4 a and 4 b illustrate rear side views of the belt plate 1 and having the belt 33 shown in phantom for ease in understanding the invention. The belt plate 1 is adjustable between the positions seen in these figures. With the fasteners 9 loosened, the holster 31 may be adjusted to assume a desired angle Z as shown in FIG. 4 b. Angle Z illustrates the adjustment of the holster with respect to the belt plate about a longitudinal axis parallel to the belt plate. That is to say, the holster fasteners 9 in the arcuate slots 6 , 7 and in mustache-shaped slot 8 may be loosened and rotated within the slots to twist the holster relative to the belt plate 1 . It will be appreciated that the previously mentioned adjustments allow the user to position the holster in an infinite number of radial angles with respect to the belt plate. Moreover, it will be readily recognized by a skilled artisan that the adjustments shown in FIGS. 3 and 4 may be undertaken simultaneously to raise or lower the holster while twisting it to a desired angle.
FIGS. 5 a through 5 c depict the second embodiment of the invention. In this embodiment, a clip-on plate or paddle 11 includes a U-shaped slot 12 for securing a holster to a waistband, purse strap, belt or other such article of clothing. The clip-on plate 11 includes the arcuate slots 6 , 7 and the mustache-shaped slot 8 as shown. The slots form adjustment points for adjusting the holster to a desired angle of twist relative to the clip-on plate. The holster 31 may be twisted or rotated relative to the clip-on plate 11 to assume an angle Y as shown in FIG. 5 c or angle Z shown in FIG. 4 b.
FIGS. 6 and 7 depict a third embodiment of the invention. A belt plate 21 includes a pair of vertically arranged belt slots 5 a, 5 b. Fastening holes 23 are formed in the belt plate 21 for passing fasteners 9 therethrough and into the holster 31 to secure it to the belt plate 21 . As seen in FIGS. 7 a and 7 b, the angle at which the belt plate 21 is relative to the belt 33 may be varied by passing the belt 33 through either belt slot 5 a or 5 b. This embodiment may also benefit from the height and angle adjustment means disclosed with respect to the embodiment of FIGS. 3 and 4 , discussed above.
Thus, the present invention encompasses various combinations of various embodiments. In one aspect the present invention is directed to the adjustable attachment means defined by two arcuate slots and one mustache-shaped slot which receive fasteners for attaching a holster holding plate to a holster, as has been discussed above with respect to FIGS. 1-5 . This inventive means for adjustably attaching a holster to a holster holder may be employed on any type of holster holder. Thus, the clip-on plate or paddle disclosed in FIGS. 5 a - 5 c, which is itself well known in the art, may advantageously include this inventive adjustable attachment means. Similarly, the inventive holster holder having three, and therefore alternative, belt receiving slots, which is shown in FIGS. 6 and 7 with a conventional means for holster attachment, may also advantageously include the present inventive adjustable attachment means. And, while the inventive holster holder having two belt receiving slots with height and angle adjustment means shown in FIGS. 1-4 is shown with the present preferred adjustable attachment means, it may also be employed with a conventional attachment means such as shown in FIGS. 6 and 7 .
While the invention has been described with respect to preferred embodiments, it is apparent to those skilled in the art that changes, modifications and additions may be made to the herein described embodiments without departing from the scope of the invention. Accordingly, it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative and not in limiting sense or use.
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An improved holster holding device for fastening a holster onto a wearer includes a belt angle adjustment for changing an angle between a belt and a belt plate. Holster adjustment means for changing an angle between a belt plate or clip-on plate and a holster are included. The holster adjustment includes arcuate slots for accepting fastening devices that fasten the holster to the belt or clip-on plate.
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PRIOR APPLICATION
This application is a U.S. national phase application based on International Application No. PCT/SE2005/000350, filed 9 Mar. 2005, claiming priority from Swedish Patent Application No. 0400940-3, filed 7 Apr. 2004.
THE PRIOR ART
In association with either one of the bleaching and the delignification of cellulose pulp in bleaching lines, the pulp passes between different treatment steps in which the pulp is subjected to bleaching or the delignifying effect of various treatment chemicals. The treatment typically alternates between alkaline and acidic treatment steps in which typical sequences may be of ECF type (elemental chlorine-free, Cl, in which chlorine dioxide may be used) such as O-D-E-D-E-D, O-D-PO or sequences of TCF-type (totally chlorine-free) such as O-Z-E-P. Other bleaching steps, such as Pa steps and H steps may be used.
The treatment steps may take place either at medium consistency (8-16%) or at high consistency (≧20-30%), but it is vitally important to wash out after each treatment step degradation products and lignin precipitated during the treatment step and to reduce to a minimum the remaining fraction of fluid, since the latter will otherwise lead to an increased requirement for pH-adjusting chemicals for the subsequent treatment steps and transfer of precipitated lignin and other degradation products, which subsequent step generally takes place at a completely different pH.
Simple vacuum filters with dewatering drums that are partially (typically 20%-40% of the drum) immersed in the pulp suspension that is to be dewatered were used in certain older types of washing step after a bleaching step or a delignification step. In these vacuum filters, a bed of pulp forms spontaneously against the outer surface of the drum under the influence of a negative pressure in the interior of the drum, and the pulp bed is drawn up from the pulp suspension by the rotation of the drum and is scraped off with a scraper on the side of the drum that is moving downwards. A consistency higher than 8-14% is generally never achieved for the pulp bed that has been dewatered, due to the limited degree of dewatering that is achieved, and the dewatered pulp that is scraped of can be readily formed to a slurry with a low consistency again in a subsequent collecting trough. The technique used here is a lower degree of dewatering followed by slurry formation with a cleaner filtrate, and this takes place in a series of vacuum filters in order to achieve the required washing effect. For this reason, it is attempted to achieve as high a degree of dewatering as possible before the dewatered pulp is again formed to a slurry with cleaner filtrate before the subsequent treatment stage.
A dominating washing machine on the market for bleaching lines is the conventional dewatering press, or thickening press, in which pulp is applied to at least one outer surface of the dewatering drum and subsequently passes a nip between the drums and acquires a consistency of 20-30% or greater after the nip. A practical upper limit lies at 35-40%, where a higher degree of dryness cannot be achieved without affecting the strength properties of the fibres negatively. A representative washing press of this type is disclosed in the U.S. Pat. No. 6,521,094.
The dewatered mat of cellulose pulp that is fed out from the washing machine's nip must first be shredded due to the high degree of dewatering, which shredding takes place in a shredder screw.
The purpose of the shredder screw has been exclusively to break up the mat of dewatered cellulose pulp and feed it onwards to equipment in which the cellulose pulp is rediluted to a consistency that makes it possible to pump it onwards to the next treatment step.
The redilution thus preferably takes place in association with adjustment of the pH, which after an alkaline wash normally involves the addition of powerful acidifiers, or the addition of acidic return water/filtrate from subsequent process steps, before the subsequent acidic treatment step. These acidic conditions have involved the dilution in general being held well separated from the previous alkaline wash as well as the associated shredder screw, since the alkaline wash can be built from simpler material than that which is normally required for washing machines that resist acidic conditions. Acidic conditions require material that can resist acids, and this is significantly more expensive that other material.
The pulp on exit from the shredder screw has a very high level of dryness, a consistency of 20-30% or greater, and this means that redilution has been carried out in all installed plants in at least one separate dilution screw arranged after the shredder screw, where the dilution fluid is added during intensive agitation from the dilution screw in order to achieve a suitable homogenous consistency that makes pumping onwards to the next treatment stage possible. The diluted pulp that is achieved after the dilution screw is fed to a stand pipe in the bottom of which a pump is arranged.
A second alternative for washing is the use of a dewatering screw, in which the cellulose pulp is first diluted and subsequently dewatered in a dewatering screw (of the Thune type or Sudor press type) to a level of dryness that considerably exceeds 20-30%. In this way, what is known as “wash-by-dilution” is achieved. A compacted and well-consolidated dewatered pulp is obtained at the exit from the dewatering screw also in this case. A redilution has been used also in this case after the dewatering screw, with the addition of dilution fluid during intensive agitation from a dilution screw.
The very high consistency of the pulp after the dewatering press or the dewatering screw has given rise to the belief that dilution to a homogenous medium consistency cannot be achieved unless dilution occurs under the influence of intensive agitation from the dilution screw. A consistency of the pulp of 20-30% or greater is experienced as dry and compacted. It can be mentioned for the sake of comparison that medium-consistency pulp is so compact that it is just about possible to walk on this pulp, when it is at the upper part of the consistency range.
The use of a dilution screw at this position, however, increases the requirement for energy, it increases investment costs, it raises the requirement for maintenance and it involves a further mechanical treatment of the pulp which has a negative influence on the strength properties of the pulp.
AIM AND PURPOSE OF THE INVENTION
The present invention is intended to remove the above-mentioned disadvantages and is based on the surprising insight that even if the pulp has been dewatered to give a very high consistency, 20-30% or more, no mechanical agitation at all is required during the dilution provided that the pulp bed has been shredded to give small granules of a suitable size, and provided that the dilution fluid is added evenly over a flow of the freely falling granulated pulp.
It has surprisingly turned out to be the case that the granulated pulp demonstrates the properties of a sponge, despite its high consistency, and that, provided the dilution fluid is added evenly to a flow of non-tightly packed granulated pulp in free-fall, a primary homogenised dilution of the pulp takes place that is fully adequate such that it can subsequently be pumped or led onwards to the following bleaching stage or treatment stage.
It is sufficient in laboratory experiments with small quantities of well-granulated pulp with a consistency around 30-35% to pour the required amount of fluid to obtain the required consistency into a container with granulated and non-compressed pulp, and the complete mixture has been homogenised to an even consistency after the addition of the fluid totally without mechanical agitation. Observation of the granulated pulp has shown that there lie cavities between the granules, and the fluid rapidly penetrates between the granules through the complete volume of the granules, after which the granules absorb the fluid as sponges.
This primarily homogenised pulp is fully adequate to be pumped with a subsequent pump, in which a secondary or complementary homogenisation takes place, and these together ensure that the same degree of homogenisation of the pulp can be achieved for the subsequent treatment stage completely without mechanical agitation from a dilution screw.
The principal aim of the invention is thus to redilute pulp from a high consistency of 20-30% or higher without the use of a dilution screw and without intensive mechanical agitation, which reduces losses in the strength of the pulp.
A second aim is to reduce operating costs and maintenance costs for the process equipment in the redilution, since no operation of dilution screw is necessary.
A further aim is to reduce the investment cost of the process equipment. A reduction of both operating costs and investment costs in the process equipment entails a reduction in the cost of manufacturing bleached pulp to an equivalent degree, and this saving is multiplied by the number of washing machines that are used in the bleaching line. No less than six washing machines are included in an O-D-E-D-E-D sequence, and thus the reduction in costs can be significant.
Approximately 50 kW is required solely for the operation of one dilution screw, and the investment cost is approximately SEK 500,000 (depending to a certain extent on requirements on materials, i.e. whether it needs to be acid-resistant or not).
The operating costs per year in an O-D-E-D-E-D bleaching line will be:
6*50 kW*SEK 0.20 (the price for an operator in Sweden)*24 hours*350 days (the number of operating days per year, excluding stoppages)=SEK 500,000 SEK per year;
and the investment cost will be:
6*SEK 500,000=SEK 3,000,000.
This investment cost at an interest rate of 5% corresponds to an annual expense of SEK 150,000.
In summary, implementation of the invention involves a total annual saving that approaches SEK 650,000-1,000,000 SEK including maintenance costs and building space (frameworks, etc.) in a bleaching line with a capacity of 1,000 tonnes per day.
Furthermore, availability of the mill increases since six machines can be removed, each of which has an MTBF (mean time between failure).
A further aim is to remove a treatment step between the washing machine and the subsequent pumping, which makes possible a more compact mill and opportunities to place the washing machines at a lower height over the ground in the mill. The washing machines are normally placed at a great height over the ground, and the pulp falls downwards after being washed in the washing machine while it passes through various conditioning steps. If one of these conditioning steps (such as the dilution screw) becomes unnecessary, the building height can be reduced, which in turn gives a saving.
DESCRIPTION OF DRAWINGS
FIG. 1 shows a typical treatment step for the pulp in a reactor with a subsequent washing press according to the prior art;
FIG. 2 shows part of the system in FIG. 1 (prior art);
FIG. 3 shows a dilution system according to the invention;
FIG. 4 shows a detail of FIG. 3 ; and
FIG. 5 shows a view seen from underneath in FIG. 4 , seen at the level of the section A-A.
FIG. 6 shows an alternative dilution system according to the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows a conventional treatment step for cellulose pulp, hereafter denoted “pulp”. The pulp is fed by the pump 1 to a mixer 2 in which necessary treatment chemicals are added. These treatment chemicals can be, for example, oxygen gas, ozone, chlorine dioxide, chlorine, peroxide, pure acid or a suitable alkali for an extraction step, or a mixture of these, and possibly other chemical or additives such as a chelating agent. The pulp is transported after the addition of the necessary chemicals by the mixer 2 to a reactor system 3 , here shown in the form of a single-vessel tower 3 of upwards flow. The reactor system can, however, be constituted by simple pipes or by one or several reactors in series, and possibly with the batchwise addition of chemicals between the towers in those cases in which the bleaching processes are compatible and do not require washing between the towers.
The treated pulp is fed after treatment in the reactor system 3 to a pulp chute/stand pipe 4 , which establishes the buffer volume and static pressure required, to a pump 5 arranged at the bottom of the pulp chute.
The pulp is fed from the pump 5 to a washing machine 7 , shown here in the form of a washing press with two drums 7 a , 7 b . The pulp is applied to the drums, here at the 12 o'clock position, and is led by convergent pulp collectors during the addition of washing fluid (not shown in the drawing) to a final dewatering nip between the drums, from where a mat of dewatered pulp is fed upwards to a shredder screw 8 .
The drums in FIG. 1 rotate in opposite directions and the pulp mat is dewatered through the outer surface of the drum while the pulp is lead approximately 270° around the circumference of the drum to the nip.
The washing press may be preferably equivalent to that revealed by the U.S. Pat. No. 6,521,094. Any other type of dewatering press or washing press, however, having a drum or drums, may be used, in which a consistency of 20-30% or higher is achieved, for example a washing press with a single dewatering drum and an opposing roller, or other types of washing press with two dewatering drums.
The pulp is fed upwards from the nip in the form of a dewatered and compressed mat 20 of cellulose pulp that has been consolidated into large pieces to a shredder screw 8 , the shredding axis of which is arranged to be essentially parallel to the axes of rotation of the drums. A small oblique mounting of a maximum of 5-10° may, for example, be present if a conical shredder screw is used, where the mat is fed to an inlet slit in the outer casing of a conical shredder screw, where the inlet slit lies parallel with the axes of the drums. The fragmented pulp is led after this shredder screw 8 out from an outlet in the casing of the shredder screw in the flow 21 to a dilution screw 30 that is driven by a motor 31 . The dilution screw exposes the pulp to continuous tumbling during the addition of dilution fluid Liq2, and the pulp is subsequently fed to a stand pipe 40 at its finally conditioned consistency. The pulp can subsequently be pumped from the stand pipe 40 to the next treatment step of similar type in the bleaching line.
FIG. 2 shows another view of a part of the same process in which the shredder screw 8 is oriented in the same direction as the dilution screw 30 . It can be seen more clearly here how the dewatered and compressed mat 20 of pulp that has been consolidated into large pieces is fed into the shredder screw 8 . The shredder screw contains a threaded screw 8 a that is driven by a motor 8 c , and that may also be equipped with a number of beaters 8 b at its outlet, which beaters further whip and break up the shredded pulp. The purpose of the shredder screw is primarily to break into smaller pieces the dewatered and compressed mat 20 of pulp that has been consolidated into large pieces, and it may sometimes be sufficient with one such shredder screw. The beaters 8 b may be arranged on the same shaft as the shredder screw and they provide an extra fragmentation effect, but they are primarily used to hold the outlet from the shredder screw free from the formation of blockages.
The fragmented flow 21 of pulp particles is fed thereafter to fall under its own weight to the subsequent dilution screw 30 .
FIG. 3 shows the dilution system according to the invention in a treatment step that is otherwise equivalent to that shown in FIG. 1 . The dewatered web of pulp, which has a consistency of 20-30% or greater, is fed in this case in to the shredder screw 8 in the same way as shown in FIGS. 1 and 2 . However, dilution occurs in the outlet from the shredder screw according to the invention in a significantly simplified manner. It is important that the web or mat 20 of pulp, which maintains a consistency of 20-30% or higher, is first fragmented by the shredder screw such that the mat 20 is granulated to a particle size that is normally distributed around a mean size that lies in the interval 5-40 mm. This is taken to denote that the fragmented pulp has a particle size that is normally distributed around a maximum size that is less than 40 mm, preferably less than 30 mm, and even more preferably less than 20 mm. It is appropriate that the normal distribution is distributed such that 90-95% of the fragmented pulp lies within ±5 mm of the maximum size, 40-30 or 20 mm, of the fragmented pulp.
The granulated pulp is then fed out from the outlet of the shredder screw in free fall into a stand pipe 22 connected to the outer casing of the shredder screw at its outlet. The dilution fluid LiqDIL is subsequently added under pressure into the stand pipe through a number of fluid jets preferably arranged around the periphery of the stand pipe and above a level LiqLEV of diluted cellulose pulp established in the stand pipe. Alternatively, some or all of the fluid jets may originate from a central pipe that is located in the flow of the fragmented pieces of pulp that are standing in free fall, and where the fluid jets are directed essentially radially outwards. A certain oblique adjustment may be established, but it is preferable that the jets are directed towards the freely falling flow with an angle of attack of 90°, or within the interval 90°±60° (=30°-155°), such that a certain minimum angle of attack is established. There may be so many fluid jets that an essentially continuous “fluid curtain” is established, or the dilution fluid may be injected into the flow of freely falling fragmented pulp through one or several slits. The important fact is that the dilution fluid is added to the flow at several points and at points at which the granulate is falling freely before it reaches the underlying surface of pulp that has been diluted to its final degree.
In the embodiment shown in FIG. 3 , the upper connection 22 of the stand pipe to the outer casing of the shredder screw has a smaller diameter than the lower part 40 ′ that lies below. The principle is that the pulp falls under the influence of gravity down through the parts 22 , 40 ′ of the stand pipe, and its lower part 40 ′ is given a larger diameter in order to be able to establish a suitable buffer volume before the pumping with the pump 41 ′ at a given level of pulp LiqLEV in the stand pipe 22 , 40 ′.
The amount of dilution fluid LiqDIL added establishes a consistency of the cellulose pulp within the range of medium consistency 8-16%, which is a consistency that allows the pulp to be sent onwards using an MC pump. The amount of dilution fluid that is required in order to establish the consistency at which the pulp is subsequently pumped is constituted to more than 75-90% of the fluid that is added at the said nozzles arranged above the level/surface that has been established in the stand pipe. A certain amount of chemicals such as acidifiers/alkali or chelating agents may be added at the bottom of the stand pipe 22 / 40 ′, but the principal dilution takes place with the dilution fluid above the pulp level established in the stand pipe.
The cellulose pulp at this medium consistency is fed by the pump 41 onwards from the lower end of the stand pipe to subsequent treatment steps for the cellulose pulp.
The dilution of the pulp from high consistency of 20-30% or greater at the upper part of the stand pipe to a medium consistency of 8-16% before the pumping from the lower part of the stand pipe takes place in this manner exclusively under the influence of the hydrodynamic effect from the addition of the dilution fluid through the said nozzles.
FIG. 3 and FIG. 4 show an embodiment of the manner in which addition of the dilution fluid can be realised. The dilution fluid is added by a pump to a distribution chamber 60 that is arranged concentrically around the stand pipe 22 . The pump pressurises the fluid to a suitable level, an excess pressure of approximately 0.1-0.8 bar. Alternatively, high-pressure nozzles can be used, which finely distribute the dilution fluid in the form of fanned plumes of fluid, oriented at a suitable angle relative to the vertical, a suitable angle being 30-90°.
A number of nozzles 62 are arranged at the bottom of the distribution chamber oriented obliquely downwards, in the direction of flow of the granulate, and inwards towards the centre of the flow. The amount of obliqueness in the mounting is appropriately 45±15° relative to the vertical. The oblique orientation downwards is favourable for achieving an ejecting influence on the granulate flow, and for avoiding the risk that the dilution fluid splashes upwards in the stand pipe.
A number of nozzles, at least four, are arranged around the stand pipe 22 / 40 ′, preferably with equal distances between them. With a stand pipe 22 having a diameter of 800-1,500 mm, it is appropriate that 10-40 nozzles are arranged around the periphery of the stand pipe. It is appropriate that the distance between adjacent nozzles be less than 50-300 mm. If high-pressure nozzles with fanned plumes of fluid are used, the nozzles may be arranged with a greater distance between neighbouring nozzles. It is important that the dilution fluid is added evenly around the complete circumference of the flow of granulate and at a sufficiently high pressure in order to penetrate to the centre of the granulate flow. The pressure setting is an engineering adaptation that is based on the nozzles being used, the diameter of the pipe and the rate of flow of fragmented pulp.
FIG. 6 shows an alternative embodiment of the invention. The difference between the embodiment shown in FIG. 3 and this embodiment is that the dewatering arrangement in this case is a dewatering screw (of Thune type or Sudor type) in which a conical screw 80 a compresses an incoming flow 20 of pulp during dewatering against a surrounding space through a screwed surrounding perforated housing, and in which filtrate 80 b is led away from this space. The driving force for the screw is normally located at its inlet, but the motor 8 c is here shown connected to the outlet of the screw.
The dewatered and compressed pulp that has been consolidated into large pieces is also in this case fed from the outlet of the screw to a simpler fragmentation arrangement in the form of a number of beaters 8 b that may be located on the same shaft as the conical screw while being located at its outlet. These beaters 8 b whip and break up the pulp that is fed out from the dewatering screw in the form of dewatered and compressed pulp that has been consolidated into large pieces. It is preferable that these beaters have their own source of power, and that they are driven at a rate of revolution that considerably exceeds the rate of revolution of the screw.
The fragmented flow 21 of pulp particles is subsequently fed by falling under its own weight to the fall 40 , in the same manner as that shown in FIG. 3 . Furthermore, a second dewatering screw 90 is arranged to receive the diluted pulp suspension at the bottom of the fall 40 . The dewatering screw 90 may be another transport arrangement or another distribution arrangement, such as, for example, a distribution screw in the inlet arrangement to a dewatering press.
The dilution otherwise functions in the same manner as in the embodiment shown in FIG. 3 , and those parts that are the same have the same reference numerals.
The invention can be modified in a number of ways within the scope of the claims. The nozzle 62 for the addition of dilution fluid may, for example, be constituted by a simple drilled hole in a thick corrugated sheet, with a minimum thickness of 8-10 mm. However, specially adapted nozzles are preferred, which preferably generate a fan-shaped plume of fluid, in order to ensure optimal penetration of the granulate flow and an even distribution over the complete circumference of the flow. Addition of dilution fluid can also take place at a sufficiently high pressure that the dilution fluid more forms a very finely divided mist in the region that the granulated pulp passes.
Addition of dilution fluid takes place in the preferred embodiment in association with an increase in the area of the stand pipe 22 to a lower part 40 ′ of the stand pipe having a larger diameter, but it is not necessary that the addition takes place in association with an increase in area.
A small amount may also be added at the outlet end of the shredder screw, with the addition flow directed down towards the stand pipe. But the dilution is to take place principally through the hydrodynamic mixing effect from the addition of the dilution fluid into the flow of granulate.
While the present invention has been described in accordance with preferred compositions and embodiments, it is to be understood that certain substitutions and alterations may be made thereto without departing from the spirit and scope of the following claims.
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The method and a device is for the dilution of dewatered cellulose pulp that maintains a consistency of 20-30% or greater. By shredding of the pulp to a finely divided dry-granulate, dilution to a homogeneous consistency in the medium consistency range can take place exclusively through hydrodynamic effects from the addition of dilution fluid. The dilution fluid is added to granulate at a position at which granulate is in free fall in a standpipe and above a level Liq LEV of diluted pulp in the standpipe. A number of nozzles are arranged around the periphery of the stand pipe, directed in towards the centre of the stand pipe, obliquely downwards in the direction of fall of the granulate. It is possible through this simplified procedure to avoid completely the conventional dilution screws, and this reduces the investment costs and operating costs, while at the same time unnecessary mechanical influence of the pulp fibres can be avoided.
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BACKGROUND OF THE INVENTION
This invention relates to a needle threader for a sewing machine adapted for threading the eye of a needle.
In the conventional needle threader, such as that disclosed in the U.S. Pat. No. 3,517,631, a thin and brittle threading hook is inserted through the needle eye and, after the thread is engaged at the hook, the hook is drawn out through the needle eye for passing the thread therethrough. With such known device, the hook may occasionally impinge on the peripheral portion of the needle eye during threading operation, often resulting in breakage of the brittle hook.
As another type of the conventional device, a pneumatic needle threader is also known as disclosed for example in the U.S. Pat. No. 3,486,472. This known device necessitates the use of pneumatic pump means and is therefore costly to manufacture.
Still another type of the prior art, such as disclosed in the U.S. Pat. No. 3,289,902, is also known wherein the thread is gripped along a predetermined straight thread path between a pair of interengaged blocks of flexible resilient material, and the needle is held with the needle eye in alignment with said thread path, said pair of blocks and the needle being moved relatively to each other for threading the eye of the needle. In this device, difficulties are encountered in aligning the needle eye with said thread path and thus reliable threading may not be assured.
There is also known in the prior art a further needle threading device comprises a plate member formed with a needle accommodating notch and a thread guide groove aligned with the eye of the needle accommodated in said notch, and a roller member of resilient and flexible material adapted for encircling the needle eye in cooperation with the plate member and for engaging with the thread inserted in said guide groove, said roller member being rotated to travel along said guide groove for transferring and passing the thread through the eye of the needle. In this device, the roller must be fabricated from highly resilient material and therefore has only poor durability.
SUMMARY OF THE INVENTION
The present invention has been made to obviate the above deficiency of the prior art and has it as an object to provide an improved needle threader which is durable and enables the thread to be passed easily and positively through the eye of the needle.
In order to fulfil such object, the needle threader of the present invention comprises a pair of resilient rollers that are rotatably mounted on a support having a needle accommodating notch and that contact at the respective peripheral edges with each other, the needle being accommodated in the notch with the eye of the needle positioned on the line passing through and tangent to the contact portion of the two resilient rollers. In the threading operation, the thread is introduced to the zone of proximity to the contact portion of the two resilient rollers through the aid of thread guide means so as to be gripped between said resilient rollers and transferred by rotation of these rollers so that the thread is passed through the eye of the needle.
According to a preferred embodiment of the present invention, one of the resilient rollers is driven by rotational operation of a knob mounted on the support, while the other roller is driven by such rotation of said one of the rollers. Thus, direct manipulation of the resilient rollers is dispensed with, thus resulting in perspiration etc. not being adhered to the rollers and the thread being positively moved towards the eye of the needle.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view of the sewing machine showing the needle threader of the present invention in the mounted state;
FIG. 2 is a left-hand side view thereof;
FIG. 3 is a section taken along line 3--3 of FIG. 1;
FIG. 4 is an enlarged plan view showing substantial parts of the needle threader;
FIG. 5 is a fragmentary plan view shown to an enlarged scale and showing substantial parts of the needle threader;
FIG. 6 is a left-hand side view corresponding to FIG. 4; and
FIG. 7 is a section taken along line 7--7 of FIG. 4.
DESCRIPTION OF THE PREFERRED EMBODIMENT
An embodiment of the present invention is explained below by referring to the accompanying drawings. A face plate 2 is hinged to the head portion of a machine frame 1 so that the inner part of the head portion may be exposed upon swinging of the face plate 2 towards its open position. A needle bar gate 3 having a substantially rectangular cross-section is mounted for swinging movement on the head portion of the frame 1, and is formed with a cutout 3a on the lower rear face thereof as shown in FIGS. 2 and 3. Projections 4 and 5 are provided to substantial the center and lower portion of the needle bar gate 3 respectively so as to project towards right as seen in FIG. 1. A jogging mechanism (not shown) as known per se is connected to the needle bar gate 3 at the lower projection 5 for causing the needle bar gate 3 to swing laterally.
A needle bar 6 is carried by the needle bar gate 3 at said projections 4 and 5 for vertical movement. A needle clamp 7 is mounted to the lower extremity of the needle bar 6. A needle 8 is removably mounted by the clamp 7 to the lower extremity of the needle bar 6 and formed with a needle eye 8a extending in the fore and aft direction. To approximately the center of the needle bar 6 is secured a needle bar clamp 6a through which the needle bar 6 may be vertically movable by a conventional crank mechanism (not shown).
A metallic plate member 9 is formed by bending so as to have a transverse section in the form of a letter L and thus has two flat portions 10 and 11 having longitudinal slots 10a and 11a, respectively. A pin 12 serving as spring retainer is secured to the lower extremity, of the left side flat portion 10, while the lower extremity of the rear flat portion 11 is formed with a needle threader attaching portion 13. The plate member 9 is mounted on the gate 3 by two stepped screws 15 by way of an attachment piece 14 having a substantially L shaped cross section, with the flat portions 10 and 11 resting on the left hand side face and rear face of the gate 3 respectively, and is vertically movable within the travel stroke as defined by engagement between the stepped screw 15 and the upper and lower ends of the slot 10a.
A metal fitting 16 is secured to the upper portion of the needle bar gate 3 so as to project towards left in FIG. 1 and a tension spring 17 is mounted between the fitting 16 and pin 12 for urging the plate member 9 upwards. Thus, under the force of spring 17, the plate member 9 is normally kept as shown by chain line in FIG. 2 to an elevated position as defined by engagement between the lower end of the slot 10a and the stepped screw 15.
Referring to the structure of a needle threader attached to the attaching portion 13 of the plate member 9, a support 18 for the needle threader consists of a metallic plate which is bent so as to have substantially the shape of a letter L when seen in side elevation, with two sides thereof providing a base portion 19 and an arm portion 20 and with one side of said base portion 19 being formed with a bent extension 21.
The support 18 is pivotally mounted to the attaching portion 13 of the plate member 9 at the foremost part of the arm portion 20 by a stepped screw 22 and by the medium of a corrugated spring washer 23. When lowered from the elevated position, the support 9 may be rotated between a retracted position as shown by the chain line in FIG. 1 in which the support 18 is spaced towards the left side of the needle 8 and a threading position as shown by the solid line in FIG. 1 in which the support 18 approaches the needle 8.
An engaging portion 24 is formed by bending the end of the arm portion 20 of the support 18 towards the front for providing retaining means for the support 18 in cooperation with the needle clamp 7, and acts for limiting the rotational extent of the support 18 through engagement with the lower edge or right hand edge of the attaching portion 13. In the threading position of the support 18 as shown by the solid line in FIG. 1, the engaging portion 24 engages the needle clamp 7 from the bottom side for setting and holding the support 18 in the threading position.
As shown in FIG. 4, the rear edge of the base portion 19 is formed with a V-shaped needle accommodating notch 25, which is brought to a position close to the needle eye 8a of the needle 8 and accommodating the needle 8 when the support 18 has been swung to the threading position. The upper surface of the base portion 19 is formed with a first recess 26 of larger diameter and a second recess 27 of smaller diameter continuous to the first recess 26.
A rotary shaft 28 is secured to the base portion 19 at the center of the first recess 26 for rotation about its own axis, and a stud 29 is also secured to the base portion 19 at the center of the second recess 27 for extending parallel to said rotary shaft 28. As shown in FIG. 7, a first resilient roller 30 of larger diameter is formed by a disk part 31 made of synthetic material or the like and secured by fitting about the shaft 28 in the first recess 26 and a ring part 32 made of rubber or similar resilient material and fitted about the disk part 31. The first roller 30 is rotatable with rotation of the rotary shaft 28. A second resilient roller 33 made in the form of a ring from rubber or similar resilient material is fitted for rotation about the stud 29 in the second recess 27 and has its outer periphery contacting the outer periphery of said first roller 30 in the vicinity of the notch 25, which is positioned on a tangent line at the contact portion 34.
As shown in FIGS. 4 and 5, the upper surface of the base portion 19 of the support 18 is formed with a thread inserting groove 35 at an opposite side of the notch 25 relative to the contact portion 34 between the pair of resilient rollers 30 and 33. The width of the thread inserting groove 35 is decreased gradually from the front edge of the base portion 19 towards the contact portion 34. A thread guide plate 36 that constitutes thread guide means in cooperation with the thread inserting groove 35 is moulded from transparent synthetic material. The thread guide plate 36 is mounted to a pin 37 secured to the base portion 19 of the support 18 and to said rotary shaft 28 so as to be vertically movable and partially overlie the thread inserting groove 35 and the resilient rollers 30 and 33. A coil spring 39 is mounted between a stop ring 38 mounted to the upper extremity of the rotary shaft 28 and the upper surface of the thread guide plate 36 so that the thread guide plate 36 is normally kept under the spring force of the coil spring 39 in pressure abutment with the upper surface of the base portion 19 and with the upper surface of the first resilient roller 30.
The lower surface of the thread guide plate 36 is formed with a thread inserting groove 40 registrable with the thread inserting groove 35 on the base portion 19.
As shown in FIGS. 5 and 6, the upper surface of the groove 40 is gradually sloped down from the front edge of the thread guide plate 36 towards the contact portion 34 between the resilient rollers 30 and 33 as far as the mid level of thickness of the rollers 30 and 33. By these thread inserting grooves 35 and 40 is defined a thread entrance through which the thread can be readily introduced to a zone close to said contact portion 34.
An operated shaft 41 is mounted on the bent extension 21 of the support 18 perpendicularly to the axis of the rotary shaft 28 so as to be rotatable about and slightly movable along its own axis. A knob portion 42 is mounted to the outer extremity of the operated shaft 41. To the inner extremity of the operated shaft 41 is secured a drive bevel gear 43 meshing with a driven bevel gear 44 secured to the lower end of the rotary shaft 28. A coil spring 45 is mounted between the drive bevel gear 43 and the bent extension 21 for positively bringing the bevel gears 43 and 44 into meshing with each other without play or backlash. By rotational operation of the knob portion 42, the first resilient roller 30 is rotated counterclockwise in FIG. 4 through the drive bevel gear 43 and driven bevel gear 44 and hence the second resilient roller 33 is rotated clockwise in FIG. 4. Thus the thread introduced into the zone close to the contact portion 34 of the rollers 30 and 33 through the thread entrance is transferred as it is gripped between said rollers 30 and 33, and is introduced through the eye 8a of the needle 8 accommodated in the notch 25.
The needle threader so far shown and described operates as follows. During normal sewing operation of the sewing machine, the plate member 9 is raised as shown by the chain line in FIG. 1, and the needle threader is kept in the raised position and housed within the face plate 2 so as not to obstruct the sewing operation.
In case of needle threading, the needle 8 is brought to a halt in the raised position by the operator. Then, the face plate 2 is swung for opening the head portion of the machine frame 1 towards left. In this state, the needle threader is pressed down manually, the plate member 9 being thus lowered against the force of the tension spring 17 and the support 18 of the needle threader is moved to a position below the needle clamp 7 mounted on the needle bar 6. Downward travel of the plate member 9 is impeded when the upper edge of the slot 10a of the plate member 9 engages with the stepped screw 15. In this state, the support 18 is turned counterclockwise in FIG. 1 by manipulation at the knob portion 42. The needle 8 is flexed slightly towards back against its own resiliency through engagement with the back surface of the base portion 19 of the support 18, and then snaps into the needle accommodating groove 25. Then the manual operation on the threader is released, the plate member 9 and the support 18 are slightly raised under the force of the tension spring 17 until the engaging portion 24 on the support 18 engages the needle clamp 7 from the bottom side, as shown by solid line in FIG. 1.
The spring washer 23 mounted around the stepped screw 22 acts to impart a force of friction to the support 18 for preventing the rotation of the support 18 against the action of tension spring 17 and maintaining the support 18 in the threading position. In this way, the resilient rollers 30 and 33 on the base portion 19 of the support 18 are maintained in the horizontal position as shown in FIGS. 4 through 7 and the eye 8a of the needle 8 accommodated in the notch 25 may approach the rear side of the contact portion 34 of the resilient rollers 30 and 33 and be placed on the tangent line passing through the contact portion 34.
Then, the thread is inserted by the operator along the thread entrance defined by the thread inserting grooves 35 and 40, the thread being readily introduced to the zone close to the contact portion 34. Upon rotational operation of the knob portion 42 in the direction of the arrow mark of FIG. 4, the first resilient roller 30 is rotated counterclockwise in FIG. 4 through bevel gears 43 and 44, and hence the second roller 33 is rotated in unison clockwise in FIG. 4. Thus the thread is transferred towards back as it is gripped between the rollers 30 and 33 and may be passed readily and positively through the eye 8a of the needle 8.
When the thread thus passed through the eye 8a of the needle 8 is then gripped at the end thereof extending towards front from the thread entrance, and is lifted towards back, the thread guide plate 36 is floated against the force of the coil spring 45, the thread being thus released from the thread entrance. After completion of the threading operation as described above, the support 18 is swung clockwise from the threading position shown by the solid line in FIG. 1, the engaging portion 24 being thus released from engagement with the needle clamp 7, and the needle 8 being disengaged from the needle accommodating notch 25. The support 18 is now raised under the force of the tension spring 17 along with the plate member 9 and returned automatically to the original raised position.
If the operator starts the sewing by mistake with the support 18 held in the threading position, the support 18 is forced to be swung clockwise in FIG. 1 through the needle clamp 7 and be retreated from the threading position towards left in FIG. 1, because downward travel of the plate member 9 against the action of the tension spring 17 is obstructed by engagement of the stepped screw 15 with the upper edge of the slot 10a. Thus there is no risk of damages done to needle threader components or to the needle to safeguard the operator's safety.
In the present embodiment, since the thread guide plate 36 is made of transparent synthetic material, thread insertion to the zone close to the contact portion 34 of the pair of resilient rollers 30 and 33 may be checked visually. Moreover, since the distal ends of the thread inserting grooves 35 and 40 are located at the mid height of the contact portion 34 of the pair of resilient rollers 30 and 33, the thread introduced to the zone close to the contact portion 34 through the inserting grooves 35 and 40 may be positively gripping by and transferred through rotation of the resilient rollers 30 and 33.
In addition, since the needle accommodating notch 25 on the support 18 is V-shaped in plan view, needles of any thickness may be positively located in the notch 25, it being understood that needles 8 of smaller thickness with smaller eyes 8a being positioned closer to the contact portion 34 between the rollers 30 and 33 than the needles of larger thickness.
The present invention is not limited to the specific embodiment described above but may comprise any modifications such as substituting the transparent material of the thread guide plate 36 by opaque or translucent material, changing the plan configuration of the needle accommodating groove 25 to a U-shaped or providing only one thread inserting groove to either the support 18 or the thread guide plate 36, providing that such modifications do not depart from the purport of the invention.
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There is disclosed a needle threader comprizing a support provided with a needle accommodating notch and a thread guide groove, and a pair of resilient rollers rotatably mounted on the support and contacting at the respective peripheral edges with each other. In the needle threader, an eye of a needle accommodated in the needle accommodating notch is located on a tangent line passing through the contact portion of the pair of resilient rollers. A thread introduced via the thread guide groove towards the proximity of the contact portion of the pair of resilient rollers is gripped by and transferred through rotation of the resilient rollers, resulting in the thread being passed through the eye of the needle.
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FIELD OF INVENTION
This invention relates to quantum effect semiconductor devices and more particularly, to semiconductor quantum oscillation (Bloch oscillation) devices, which produce electromagnetic radiation in response to an applied electric field. The frequency of the electromagnetic radiation is between the highest microwave frequencies and the lowest infrared frequencies.
BACKGROUND OF INVENTION
The basic physical principle involved in the present invention is the dynamics of electrons in a crystal subjected to a uniform electric field. Sixty year ago, F. Bloch (F. Bloch, Z. Phys. 52, 555(1928)) and C. Zenner (C. Zenner, Proc. R. Soc. 145, 523 (1934)) have shown that an electron in a crystal could be described as a wave-packet composed of Bloch functions, and in the case where both scattering and interband tunneling into higher energy bands are absent, the electron will undergo periodic motion in k space in response to the applied electric field. The frequency of the periodic motion is eFa/h, where e is the electron charge, F is the electric field, a is the crystal constant, and h is the Plank constant. The oscillatory motion of an electron in k space is accompanied by a periodic motion in real space. This oscillatory motion of electrons in a crystal subjected to a uniform electric field is generally termed Bloch oscillation (or alternately Zenner oscillation, or Zenner-Bloch oscillation or Bloch-Zenner oscillation). Bloch oscillation is caused by the Bragg reflection of ballistically accelerated electrons at the Brillouin zone boundary, which leads to the periodic motion of electrons in the first Brillouin zone. The above description of electron motion is based on the dynamics of Bloch wave packet and is generally called a quasiclassical description. Subsequent theoretical work has shown that, an electron in a crystal subjected to a uniform electric field could also be described as a wave packet composed of quasibound Wannier-Stark states. In this fully quantum-mechanical description, Bloch oscillation appears as a special case of the quantum interference of Wannier-Stark states. For a detailed theoretical analysis of Bloch oscillation, the paper titled “Warrier-Stark Quantization and Bloch Oscillator” by G. Bastard and F. Ferreira could be consulted (in Spectroscopy of Semiconductor Microstructure, NATO ASI series, Plenum, N.Y., 1989, P.333). In order to realize Bloch oscillation, electrons should complete at least one oscillation period before being excited into higher energy bands (via interband tunneling sometimes called Zenner tunneling) or before experiencing scattering. For interband tunneling, when phonon effects are neglected, its upper boundary has been established at a rigorous level based on one-electron theory approximation, which shows that an electron may execute a number of Bloch oscillations before tunneling out of a band (A. Nenciu and G. Ninciu, J. Phys. A14, 2817(1981)). Therefore, interband tunneling should not be an obstacle to the realization of Bloch oscillation. As to scattering, there are two scattering mechanisms for electron in a solid, including phonon scattering and impurity scattering. Now, it is a common belief that due to the existence of scattering, Bloch oscillation should not be observable in conventional solid for all reasonable values of electric fields (G. von Plessen and P. Tomas, Phys. Rev. 45, 9185(1992)). P. Robin and M. W. Muller (J. Phys. C: Solid State Phys. 16, 4547(1983)) studied the properties of Bloch oscillation (called coherent Zenner oscillation in their paper) and found that only quasicohorent electrons can execute Bloch oscillation. Quasicohorent electrons are classical-like electron with minimized size x, and an oscillatory position expectation.
From an application standpoint, L. Esaki and R. Tsu proposed in their U.S. Pat. (No. 3,626,328) a Bloch oscillation device that employs a superlattice structure. The starting point for their proposed device is that the condition needed for Bloch oscillation should be more easily satisfied in superlattice structures. The argument is that a mini-Brillouin zone much smaller in width than the normal Brillouin zone is formed in the superlattice direction and as a result the scattering processes might be more favorable than in conventional solids. The objective of this invention is to provide a high-frequency semiconductor superlattice bulk oscillator based on the physical principle of Bloch oscillation. Up to now, the proposed device has never being realized (L. Esaki, in Science and Technology of Mesoscopic Structures, Springer-verlag, 1992, P.3). M. W. Muller, P. Robin and D. I. Rode (Workshop on Submicron devices Physics, ed. H. L. Grubin, (New York: plenum, 1983), P. 261) proposed a concept bulk semiconductor Bloch oscillation device. In this device, time-dependent intra-band tunneling of electrons from a narrow band-gap semiconductor into a wide band-gap semiconductor is suggested as the injection scheme. P. Robin and M. W. Muller (Semicond. Sci. Technol. 1, 218 (1986)) recognized that electrons must be injected in phase to realize Bloch oscillation. They also made a qualitative analysis on the scattering of Bloch oscillation (called Zenner oscillation in their paper) and pointed out that the polar scattering in a semiconductor such as GaAs could be tuned out if the frequency of Bloch oscillation is lager than the maximum longitudinal optical phonon frequency. In addition, they further realized that the primary difficulty with the Bloch oscillations (Zenner oscillations) in bulk semiconductors is to turn them on. Though all their above viewpoints regarding to realizing Bloch oscillation are correct and are very insightful, they came to a conclusion that one could not escape the high polar scattering rate during the electron injection phase. Their concept Bloch oscillation device does not become a working device. The reason is that the time-dependent tunneling electron injection scheme proposed in their device is not practical, and in addition this electron injection scheme could not escape the polar scattering. Therefore, the key to obtain practical Bloch oscillation becomes how to find a novel electron injection scheme, which could not only escape the polar scattering but also make the injected electrons in phase. Besides, the above semiconductor Bloch oscillation devices are concentrated on electrons in the conduction band, and little is reported on how to realize Bloch oscillation using the other type carriers, i.e. holes in the valence band.
SUMMARY OF THE INVENTION
It is among the objects of the present invention to provide a semiconductor Bloch oscillation device that employs a unique carrier injection scheme to inject carriers (including conduction band electrons and valence band holes). The carrier injection scheme provided will not only overcome the high polar scattering obstacle unresolved in prior art, but also inject both coherent electrons and coherent holes. In order to implement the above objectives, the present inventor made a broad and detailed study on the conditions required to realize Bloch oscillation and the following facts pertaining to Bloch oscillation are discovered:
1). Valence electrons in the full valence band of an intrinsic semiconductor experience much less scattering in comparison with conduction-band electrons and valence band electrons (represented as holes) in doped semiconductors. The argument is that, if these valence electrons experience phonon scattering, the only possible way of being scattered is into the conduction band, as there are no available states in the full valence band. And in reality, the probability of this kind of scattering is extremely small as the band gaps of common semiconductors are usually much larger than the energy of thermal phonons.
2). Under the action of a strong electric field, band-edge valence electrons (wave vector k nearly equal zero) of an intrinsic (unintentionally doped) semiconductor could be excited into the conduction band through the interband tunneling process, so it is possible to obtain free electrons and free holes in the conduction and valence bands, respectively. Based on the discovery in 1), band-edge valence electrons in a full valence band experience little phonon scattering before the occurring of interband tunneling. Therefore, if phonon participation is being avoided for the interband tunneling process (direct interband tunneling), then the free electrons and free holes obtained will escape the influence of phonons. Considering that only the band-edge valence electrons with a wave vector of nearly zero take part in the interband tunneling process, and that a wave vector is conserved for the phonon-free interband tunneling process, it will be possible to obtain coherent free electrons and free holes by making interband tunneling occur only locally
3). Based on P. Robin and M. Mullers analysis on the scattering of Bloch oscillation (cited above), in order to tune out phonon scattering, an electric field more than 1000 KV/cm is needed to make the frequency of Bloch oscillation higher than the frequency of longitudinal optical (LO) phonons. This requirement of the electric field to tune out scattering is in agreement with the requirement to induce direct interband tunneling in semiconductors.
4). Now Molecular Beam Epitaxy (MBE), Metal-Organic Chemical Vapor Deposition (MOCVD) or other material growth methods with the capability of atomic layer control is widely used to grow various types of semiconductor multilayer structures. By controlling the thickness, composition and/or stress of each individual layer, it is possible to make direct interband tunneling occur only locally inside the multilayer structure when the whole multilayer structure is subjected to a strong electric field. The region where interband tunneling occurs can be used as the injection region for Bloch oscillation devices to obtain coherent electrons and coherent holes.
Based on the above discoveries, the present invention provides a semiconductor quantum (Bloch) oscillation device including a multilayer structure of semiconductor heterojunction material defining an interband tunneling region with a pair of carrier oscillation regions sandwiching the interband tunneling region therebetween and means for applying an operating voltage across the multilayer semiconductor structure. The operating voltage applied across the multilayer structure inducing interband tunneling of carriers in the interband tunneling region and injecting coherent carriers into the carrier oscillation regions. The device employs direct (phonon-free) interband tunneling (also called Zenner tunneling) to implement coherent electron and coherent hole injection into the pair of carrier oscillation regions, and the interband tunneling is made to occur only locally in an intrinsic or unintentionally doped semiconductor multilayer structure.
It is very difficult to build a practical oscillator using existing two-or three terminal semiconductor devices to produce electromagnetic radiation with a frequency of above 300 GHz. On the other hand, for spectral regions above mid-infrared (5-8 um), there are no solid light sources available that could directly and efficiently convert electric energy into optical energy similar to a near-infrared laser. All in all, in the spectral region from mid-infrared to the sub-millimeter region, there is a significant need for an efficient, lightweight and high-speed optical source. The frequency of Bloch oscillation covers this spectral region. Therefore, the semiconductor quantum (Bloch) oscillation device provided by the present invention will pave the way for effectively using the electromagnetic resource in this spectral region.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a diagram illustrating the structure of the semiconductor quantum oscillation device according to the invention in which direct interband tunneling is used to realize carrier injection.
FIG. 2 is a plot of the I-V characteristics for the semiconductor quantum oscillation device in FIG. 1, illustrating that there is a critical voltage Vc corresponding to the occurrence of interband tunneling.
FIG. 3 is an energy band diagram illustrating a multilayer semiconductor structure applicable to the interband tunneling region and the two carrier oscillation regions for the semiconductor quantum oscillation device shown in FIG. 1 .
FIG. 4 is an energy band diagram for the interband tunneling region and carrier oscillation structure shown in FIG. 3, illustrating a situation where a critical voltage is applied to induce interband tunneling.
FIGS. 5-7 are energy band diagrams illustrating other usable interband tunneling region and carrier oscillation region structures for the semiconductor quantum oscillation device shown in FIG. 1 .
FIG. 8 is an energy band diagram illustrating another multilayer semiconductor structure applicable to the interband tunneling region and the two carrier oscillation regions for the semiconductor quantum oscillation device shown in FIG. 1, which is a modification of the structure shown in FIG. 3 .
FIG. 9 is an energy band diagram for still another interband tunneling region and carrier oscillation region structure, in which the electron oscillation region comprises a superlattice structure.
FIG. 10 is a sectional view of an exemplary device according to the subject invention.
FIG. 11 is the I-V characteristics for the exemplary device shown in FIG. 10 .
DETAILED DESCRIPTION
FIG. 1 is a diagram illustrating the structure of the semiconductor quantum oscillation device of the present invention that comprises an interband tunneling region and two carrier oscillation regions. The entire device is designated 100 and is shown to include an interband tunneling injection region 102 ; two carrier oscillation regions, electron oscillation region 104 and hole oscillation region 106 , which sandwich interband tunneling injection region 102 ; one contact region 108 which is adjacent to electron oscillation region 104 and a corresponding metal electrode 112 formed on it; and another contact region 110 which is adjacent to hole oscillation region 106 and a corresponding metal electrode 114 formed on it. While operating the device, a positive voltage applied to metal electrodes 112 and 114 produces a strong electric filed in interband tunneling injection region 102 and carrier oscillation regions 104 and 106 . The strong electric field induces direct (phonon-free) interband tunneling in interband tunneling injection region 102 which leads to coherent electrons and coherent holes being injected into electron oscillation region 104 and hole oscillation region 106 , respectively. The injected coherent electrons and coherent holes execute Bloch oscillation in response to the strong electric field in the oscillation regions by the interaction of the coherent carriers in the oscillation regions with the crystal periodic potential and produce electromagnetic radiation. The electromagnetic wave output is perpendicular to the applied electric field, with the electric field polarization being along the direction of the applied electric field. The semiconductor quantum device of the present invention looks likes an edge-emitting semiconductor light-emitting diode (LED), though the working principles involved are quite different. Therefore, by forming a waveguide-type Fabray-Perot resonant cavity, similar to an ordinary semiconductor injection laser, or by employing other techniques to couple the radiation energy back into the device, the semiconductor quantum oscillation of the present invention can be operated as a laser.
The frequency of Bloch oscillation of carriers can be expressed as
ν=λ2 πeF/hκ (1)
where e is the electron charge, F is the electric field, h is the Plank constant, κ is the “diameter” of the Brillouin zone along the electric field direction, and λ is a numerical factor related to the detailed energy band structure of the oscillation region. For GaAs and some other compound semiconductors, the conduction band minimum is located at the center of the Brillouin zone (Γ point, κ=0), while the conduction band also has satellite valleys along the <100> and <111> crystal directions. Based on the quasiclassical description of electron motion, the frequency of the Bloch oscillation could not be calculated using the simplified formula (ν=2πeF/hκ) derived for the case in which only one energy extreme exists. Therefore, λ is introduced to account for the actual band structure effects. Though at present it is not very clear how the band structure affects the frequency of Bloch oscillations, it is expected that λ has a value of 1 to 2. For the valence band of most semiconductors, as there are no sub-extremes, λ has a value of 1. For GaAs, supposing that an electric field of 5×105 V/cm is applied along the <100> crystal direction, it can be determined that hν=27 λmeV based on equation (1). It can be seen that electromagnetic radiation from the Bloch oscillation is in the far-infrared region in this case.
Metal electrodes 112 and 114 in FIG. 1 are the terminals which access the outside world for the semiconductor quantum oscillation device of the present invention. Basically, metal electrodes 112 and 114 have two functions: one is that the voltage applied to them produces the strong electric field needed for device operation in interband tunneling injection region 102 and carrier oscillation regions 104 and 106 ; and the other is that they act as two collectors to collect the dephased electrons and the dephased holes from carrier oscillation regions 104 and 106 , respectively. A coherent carrier that executes Bloch oscillation will become dephased once it experiences a phase-breaking scattering event such as phonon-scattering. The current formed by the dephased carriers forms the external terminal current for the semiconductor quantum oscillation device 100 of the present invention. It is significant to point out that, for semiconductor quantum oscillation device 100 of the present invention, there are two requirements for metal electrodes 112 and 114 . The requirements are that electrode 112 should not inject non-coherent electrons into electron oscillation region 104 while electrode 114 should not inject non-coherent holes into hole oscillation region 106 . If the above requirements can not be met, avalanche breakdown induced by the injected non-coherent carriers from the electrodes will precede the required interband tunneling and make it impossible to achieve coherent carrier injection. Depositing metal electrodes 112 and 114 directly on the significantly undoped carrier oscillation regions 104 and 106 is not an easy way to meet the above requirements as non-coherent carrier injection could occur just like in a reverse biased Schottky diode. It is also impractical to insert a dielectric layer between the contact metal and the undoped carrier oscillation regions to prevent non-coherent carrier injection from the metal electrode. The reason is that surface states exist on the interface between the undoped semiconductor and the dielectric layer, and these surface states will act as carrier generation centers if an electric filed exists on the interface, and non-coherent carriers are injected into the carrier oscillation region. Even this method is viable by reducing the surface state density to near zero, however, the device could only operate in pulse mode. An effective means to prevent non-coherent carrier injection from the contact electrodes is to insert a semiconductor contact region between the carrier oscillation region and the contact electrode, i.e., contact region 108 is inserted between electron oscillation region 104 and metal electrode 112 and contact region 110 is inserted between hole oscillation region 106 and metal electrode 114 in FIG. 1 . Preferably, the contact between metal electrodes 112 and 114 and semiconductor contact regions 108 and 110 is an ohmic contact. An ohmic contact is not a necessity for the semiconductor quantum oscillation device of the present invention, but is believed to give best results. Opposite conductivity types are provided for semiconductor contact regions 108 and 110 i.e., contact region 112 adjacent to electron oscillation region is doped n-type and contact region 114 adjacent to hole oscillation region is doped p-type. Summarizing, the preferred overall structure of the semiconductor quantum oscillation device of the present invention resembles a reverse biased P-I-N diode, and the uniqueness is that the I region comprises an interband tunneling region and two carrier oscillation regions made of a multilayer semiconductor structure having a predetermined composition and bandgap profile. It is worthwhile to point out that if the two semiconductor contact regions are made having the same conductivity type (corresponding structures are N-I-N or P-I-P), it will be impossible to prevent non-coherent carriers from being injected into the carrier oscillation regions from the contact electrodes.
FIG. 2 is a plot illustrating the I-V characteristics of semiconductor quantum oscillation device 100 shown in FIG. 1 . There is a breakdown voltage which corresponds to the occurrence of interband tunneling, and this breakdown voltage is designated critical voltage Vc. When the applied external voltage is lower than critical voltage Vc, no current exists in the device, and this portion of the I-V plot is shown in FIG. 2 as segment 201 . When the applied external voltage is larger than the critical voltage Vc, coherent carriers injected into carrier oscillation regions 104 and 106 , through interband tunneling, execute Bloch oscillation and emit electromagnetic radiation. While executing Bloch oscillation, some of the coherent carriers lose phase coherence due to scattering and become dephased carriers. Contact regions 108 and 110 collect these dephased carriers, and the resulting current is the terminal current of device 100 and is shown as segment 202 in FIG. 2 . It is emphasized that, for semiconductor quantum oscillation device 100 , both coherent and non-coherent carriers are involved and the overall carrier system (carrier ensemble) is in a state far from thermal equilibrium. This feature is quit distinctive from all available ordinary semiconductor device where carriers as a system are either in a thermal equilibrium state with the host crystal (low field case) or in a state of thermal equilibrium but with a higher temperature than the host crystal (high-field case). As a results of the non-equilibrium nature of the carrier system for semiconductor quantum oscillation device 100 , the I-V characteristics of the device will depend on the measurement methods used. Segment 202 in FIG. 2 is drawn as a dashed line to reflect this feature of the device. Besides, the coherent electrons and coherent holes are localized in space while executing Bloch oscillations, and as a result a space charge effect arises. Another factor, which affects the I-V characteristics of semiconductor quantum oscillation device 100 , is the optical field which exists inside the device. It should be understood that the feedback effects of the space charge effect and the optical field on device operation will make the actual I-V characteristics more complex than that shown in FIG. 2 . However, the fact that there is a critical voltage corresponding to the occurrence of interband tunneling still persists. For the normal operation of semiconductor quantum oscillation device 100 , the applied voltage is higher than critical voltage Vc. An I-V characteristic obtained from an exemplary device is illustrated and explained in a later part of this application.
The active regions of semiconductor quantum oscillation device 100 of the present invention are interband tunneling injection region 102 and two carrier oscillation regions 104 and 106 . This division of the active regions of device 100 is only for the convenience of description. In fact, interband tunneling region 102 and carrier oscillation regions 104 and 106 are adjacent and can only implement their individual functions as they are combined together. How these three regions as a whole are realized for the device shown in FIG. 1 will be described below in the form of energy band diagrams. Regions 102 , 104 and 106 are generally made of an undoped or intrinsic multilayer semiconductor structure having a predetermined composition and bandgap profile. Undoping or intrinsic composition is a necessity for the device active region. Only by using an undoped or intrinsic structure, is it possible to obtain the strong electric filed required to achieve coherent carrier injection through direct interband tunneling and Bloch oscillation. It should be understood that the energy band gap illustrated in the band diagrams below is the direct bandgap at the Brillouin zone center (Γ point).
FIG. 3 is an energy band diagram illustrating a multilayer semiconductor heterojunction structure applicable for interband tunneling region 102 and carrier oscillation regions 104 and 106 of semiconductor quantum oscillation device 100 shown in FIG. 1 . In FIG. 3, a semiconductor layer 301 has a relatively larger bandgap, such as GaAlAs, and functions as hole oscillation region 106 . A semiconductor layer 305 has a relatively larger bandgap, such as GaAlAs, and functions as electron oscillation region 104 . For layer 301 and layer 305 , the minimum bandgap could be either direct or indirect. When the bandgap is direct, as in the case of GaAlAs with the Al composition less than 0.45, the band diagram is a normal one with a conduction band-edge corresponding to electron energy which is minimum at the Brillouin zone center. When the bandgap is indirect, as in the case of GaAlAs with the Al composition higher than 0.45, the conduction band-edge in the band diagram still corresponds to electron energy at the Brillouin zone center though it is now not the minimum energy for the conduction band. Also shown in FIG. 3, are two semiconductor layers 302 and 304 with a relatively small band gap, such as GaAs, and another semiconductor layer 303 with a relatively large bandgap, such as GaAlAs. With layers 301 and 303 as the barriers and layer 302 as the thin potential well, a first quantum well is formed; and with layers 303 and 305 as the barriers and layer 304 as the thin potential well, a second quantum well is formed. A quantum well is a potential well having at least one discrete energy eigenstate, i.e. the allowed energy levels do not form a continuum. This is quite different from the case of ordinary double heterojunction structures where the allowed energy is continuous. In order to form a quantum well, the well layer must be very thin and at the same time a band-edge energy difference is needed between the quantum well layer and the barrier layers. For the barrier layer 303 sandwiched by the two quantum well layers 302 and 304 , its bandgap could be either direct or indirect. However, its thickness must be thin enough to allow coupling between the two quantum wells, that is to form a coupled double quantum well. (About quantum wells, see e.g., (1) Special issue of Semiconductor Well and Superlattices; Physics and Applications of the IEEE Journal of Quantum Electronics, Vol. QE-22, September 1986; (2) E. E. Mendez and K. von Klitzing (1987), Physics and Applications of Quantum Wells and Superlattices, NATO ASI Series, Series B, Physics: 170, Plenum, N.Y.; (3) C. Weinbuch and B. Vinter, Quantum Semiconductor Structures, Academic press, 1991).
In FIG. 3, the region comprising layers 302 , 303 and 304 is where a direct interband tunneling process takes place and can be termed “an interband tunneling injection region”. Layers 301 and 305 act as the hole oscillation region and the electron oscillation region, respectively. When an external voltage is applied across the device, most of the voltage will be dropped across layers 301 and 305 and the band diagram shown in FIG. 3 will become tilted. By increasing the voltage it is possible to make the valence band-edge of quantum well 302 nearly line up with the conduction band-edge of quantum well 304 . When this occurs, there is coupling between the valence electron energy levels of the first quantum well and the conduction electron levels of the second quantum well. This kind of coupling leads to some band-edge valence electrons of quantum well layer 302 entering into the conduction band of quantum well layer 304 through resonant interband tunneling without the involvement of phonons. As layers 301 and 305 have larger band gaps than quantum well layers 302 and 304 , interband tunneling will not occur inside layers 301 and 305 for the electric field required to cause interband tunneling between quantum well layers 302 and 304 . Therefore, only locally occurring interband tunneling is realized for the structure shown in FIG. 3 . The electrons entering into the conduction band of quantum well layer 304 through interband tunneling will be further injected into electron oscillation region 305 as the strong electric field exists in the whole structure. Because all of the injected electrons originating from the valence band-edge of quantum well layer 302 have an initial wave vector of near zero and nearly identical real space positions, they are classical-like coherent electrons and meet the conditions required by Bloch oscillation. The holes left after interband tunneling in quantum well layer 302 are classical-like coherent holes and are injected into hole oscillation region 301 . These injected hole also meet the conditions required by Bloch oscillation.
FIG. 4 is an energy band diagram for the interband tunneling region and carrier oscillation regions shown in FIG. 3 illustrating the situation where a critical voltage is applied to induce interband tunneling. Based on this figure, a critical electric field Ec could be defined. The operation of the semiconductor quantum oscillation device of the present invention requires that the electric field in the interband tunneling region and the two carrier oscillation regions produced by the applied voltage is higher than the critical electric field required to induce direct interband tunneling. The applied voltage corresponding to this critical electric filed is the critical voltage defined in FIG. 2 . The critical electric field for the interband tunneling injection region and carrier oscillation region structure shown in FIG. 3 could be estimated by
F c =E g /( d w1 +d w2 +d b ) (2)
where E g is the band gap of the two quantum well layers (e.g. 302 and 304 ), d w1 is the thickness of the first quantum well layer (e.g. 302 ), d w2 is the thickness of the second quantum well layer (e.g. 304 ), and d b is the thickness of the thin barrier layer (e.g. 303 ).
Using semiconductor epitaxy techniques, GaAs/GaAlAs and GaInP/GaAs heterojunction material systems grown on a GaAs or Si substrate could be used to realized the structure having the band profile shown in FIG. 3 . In addition, other heterojunction material systems could also be used, such as material systems InGaAs/InP, InGaAs/AlInAs and InGaAsP/InP grown on an InP substrate, or GaSb/GaAlSb material system grown on GaSb, AlSb or ZnTe substrates. At present, the growth of any of the above heterojunction systems by Molecular Beam Epitaxy (MBE), Metal Organic Chemical Vapor Deposition (MOCVD) and other methods is well known for those skill in the art, see e.g., L. L. Chang and K. Ploog, eds, Molecular Beam Epitaxy and Heterojunctions, Proc. Erice 1983 Summer school, martinus Nijhoff, 1985; and relevant articles in J. Crys. Growth.
FIG. 5 is an energy band diagram illustrating another multilayer semiconductor heterojunction applicable for the interband tunneling region and two carrier oscillation regions for the semiconductor quantum oscillation device shown in FIG. 1 . The structure shown in FIG. 5 is very similar to the structure of FIG. 3, with the only difference being that a thicker single quantum well is used to replace the coupled double quantum well in FIG. 3 . When the thin barrier layer 303 in FIG. 3 is replaced by the same material that the two quantum well layers is made of, layers 302 , 303 and 304 will form a thick quantum well; and the structure shown in FIG. 5 is obtained. Under the action of a strong electric field produced by an applied voltage, for quantum well layer 502 , the valence band-edge at the region near the interface with layer 501 could be brought into line with the conduction band-edge at the region near the interface with layer 503 (in order to keep agreement with FIG. 1, the electric field direction is assumed to point to layer 501 from layer 503 , and in this case 501 and 503 form the hole and electron oscillation regions, respectively, and quantum well layer 502 forms the interband tunneling injection region). This band-edge line up between valence band and conduction band for the same quantum well layer will produce strong coupling between valence states and conduction states and leads to the occurrence of interband tunneling inside quantum well layer 502 . As the electrons which undergone direct interband tunneling are initially located at the valence band edge in k space (k=0) and at the region near the interface with the hole oscillation region in real space, they are classical-like coherent electrons and meet the conditions required by Bloch oscillation. The coherent electrons are injected into electron oscillation region 503 and execute Bloch oscillation. The holes left in quantum well layer 502 after the direct interband tunneling are also classical-like coherent carriers and meet the conditions required by Bloch oscillation. The holes are injected into hole oscillation region 501 and execute Bloch oscillation there. The structure shown in FIG. 5 could also be realized using GaAs/GaAlAs, GaInP/GaAs, InGaAs/InP, InGaAs/AlInAs, InGaAsP/InP, GaSb/GaAlSb, or other semiconductor heterojunction systems.
FIG. 6 is an energy band diagram illustrating yet another semiconductor structure usable for the interband tunneling region and two carrier oscillation regions for the semiconductor quantum oscillation device shown in FIG. 1 . The structure comprises three semiconductor layers 601 , 602 and 603 , containing two heterojunctions of Type II band alignment. For the possible heterojunction band alignments, see e.g., S. M. Sze ed., High Speed Semiconductor Devices, John Wiley & Sons, P.20, 1990. For layer 602 , the bandgap could be either direct or indirect, but it must be thin enough to form a hole quantum well. In order to keep agreement with FIG. 1, the electric field produced by the applied voltage is assumed to point in the direction from layer 603 to layer 601 . Then layer 603 acts as the electron oscillation region, and layer 601 acts as the hole oscillation region. Under the action of the electric field, the valence band edge of the quantum well layer 602 at the region near the interface with layer 601 could be brought to line up with the conduction band edge of layer 603 at the region near the interface with layer 602 . Then valence electrons of the quantum well layer will be injected into the electron oscillation region (layer 603 ) through direct interband tunneling, and the holes left will be injected into the hole oscillation region (layer 601 ). Injected electrons and holes obtained above also meet the conditions required by Bloch oscillation and will execute Bloch oscillation in the two carrier oscillation regions, respectively. The multilayer semiconductor heterojunction structure in FIG. 6 could be realized, for example, by using an AlInAs/InP heterojunction system grown on an InP substrate. The band alignment for this system is Type II with AlInAs having a higher valence edge. Therefore, AlInAs could be used for the quantum well layer 602 , and InP could be used for the two oscillation regions 601 and 603 . The band alignment between II-VI compounds ZeTe and CdSe is also a Type II. In this material system, ZnTe while having a higher valence band-edge could be used for the quantum well layer 602 , and CdSe could be used for the two carrier oscillation regions.
FIG. 7 is an energy band diagram illustrating still another multilayer semiconductor heterojunction structure usable for the interband tunneling region and two carrier oscillation regions for the semiconductor quantum oscillation device shown in FIG. 1 . The structure of FIG. 7 comprises 5 semiconductor layers, where layers 701 , 703 and 705 are made of the same semiconductor material, such as InP; layer 702 is made of another semiconductor material, such as InGaAs; and layer 704 is made of yet another semiconductor material, such as AlInAs. In this structure, the band alignment between 702 and 701 (and between 702 and 703 ) is Type I, and a first quantum well is formed with 702 as the well layer. The band alignment between 704 and 703 (and between 704 and 705 ) is Type II and a second hole quantum well is formed with 704 as the well layer. The hole well depth in the second quantum well should be shallower than that of the first quantum well. Supposing the electric field is in the direction from layer 705 to layer 701 , then 701 will act as the hole oscillation region; 705 as the electron oscillation region; and 702 , 703 and 704 together as the interband tunneling region. Under the action of a strong electric field, valence band-edge electrons of first quantum well layer 702 at the region near the interface with 701 can tunnel into layer 703 through direct interband tunneling and become conduction electrons. These electrons will be injected into the electron oscillation region 705 by further tunneling (intraband tunneling) through the thin barrier layer 704 . The holes left in the quantum well layer 702 will be injected into the hole oscillation region 701 through valence-band intraband tunneling. The injected electrons and holes also meets the conditions required by Bloch oscillation and will execute oscillation motion in the two carrier oscillation regions, respectively. In this structure, layer 703 is used to form a thin conduction band barrier to increase the probability of valence electron interband tunneling from 702 to 704 , and to this end the thickness of layer 703 should also be quite thin.
The carrier oscillation region for the multilayer semiconductor heterojunction structures shown in FIG. 3 and FIGS. 5-7 comprises only one uniform semiconductor layer. In fact, the carrier oscillation region could also be make to comprise several semiconductor layers with each layer not necessarily uniform (for example, the carrier oscillation region could be a composition gradient layer). The only requirement for the whole multilayer semiconductor heterojunction structure which comprises the interband tunneling injection region and the two carrier oscillation regions is that the structure supports direct interband tunneling which occurs first in the interband tunneling injection region. FIG. 8 is a multilayer semiconductor heterojunction structure usable for the interband tunneling injection region and the two carrier oscillation regions. In this structure, the electron oscillation region comprises two semiconductor layers 806 and 807 , and the hole oscillation region also comprises two semiconductor layers 801 and 802 . This structure also employs coupled double quantum wells as the interband tunneling injection region, similar to the structure in FIG. 3 . The two quantum well layers are 803 and 805 , and the thin electron penetrable barrier layer is 804 . For this structure, by adjusting the thickness and bandgap of layer 802 and layer 806 , the probability of direct interband tunneling could be enhanced due to the property of electron resonant tunneling. For a particular device, it is also possible that it may contain only one carrier oscillation region. This is accomplished by making the thickness of one carrier (either electron or hole) oscillation region smaller than the spatial amplitude of the respective Bloch oscillations. In an extreme example, the carrier oscillation region comprises multiple layers including a superlattice structure.
FIG. 9 is an energy band diagram illustrating another multilayer semiconductor heterostructure usable for the interband tunneling region and two carrier oscillation regions shown in FIG. 1 . In this structure the electron oscillation region comprises a superlattice structure 905 , the hole oscillation region comprises a uniform semiconductor layer 901 , and the interband tunneling injection region is a coupled double quantum well structure comprising layers 902 , 903 and 904 . The superlattice structure 905 comprises two semiconductor materials of different energy bandgap and has a period of d. In order to make direct interband tunneling take place in the interband tunneling injection region, the bandgap of the relatively small bandgap material in the superlattice structure should be not less than the bandgap of the two quantum well layers 902 and 904 . The energy band offset between the two materials comprising the superlattice and their thickness determine the subband structure of the superlattice, and are important device design parameters. As the mini-Brillouin zone associated with the superlattice is smaller than the Brillouin zone of a bulk semiconductor, higher frequency electromagnetic radiation could be obtained by employing the superlattice as a carrier oscillation region for the same electric field.
For the semiconductor quantum oscillation device, strain could also be used to tailor the energy band structure to make direct interband tunneling more readily occur in the interband tunneling injection region. The energy band diagram in FIGS. 3-9 make no distinction between heavy hole valence bands (J=3/2, mz=3/2) and light hole valence bands (J=3/2, mz=1/2) for the top of the valence band. This is appropriate for the case where no strain exists in the multilayer semiconductor heterojunction structure. In this case, the heavy hole valence band and light hole valence band are degenerate at the band-edge. Strains remove this degeneracy. For biaxial tensile strained semiconductor layers, the light hole valence band becomes the highest valence band; and for biaxial compressive strained semiconductors, the heavy hole valence band becomes the highest valence band. Based on selection rule, only the light hole valence band is coupled with the conduction band under the electric field at the Brillouin zone center. It follows that direct interband tunneling will be favored by having the light hole valence band the highest valence band. To this end, a semiconductor strained layer epitaxy technique could be used to grow strained multilayer heterojunction structures to make direct interband tunneling processes more readily occur in the interband tunneling injection region. For the interband tunneling injection region and carrier oscillation regions, it is possible to make the whole structure biaxial tensile strained by using, for example, a GaAs/AlGaAs heterojunction material system grown on a Si substrate. For the same structure, if InGaAs/InP material grown on an InP substrate is used, it will be possible to make one or both quantum well layers biaxial tensile strained by adjusting the In composition of the InGaAs a little bit smaller than the lattice-match composition with InP (0.53). Biaxial tensile strain in a semiconductor epilayer is equivalent to the superposition of a hydrostatic compressive component and an axial tensile component, and the axial tensile component is in the epitaxy grown direction, that is parallel with the applied electric filed. Therefore, even for finished devices, it is still possible to make direct interband tunneling more readily occur by applying an external axial stress along the applied electric field direction.
In addition to using a strained layer to make direct interband tunneling more readily occur, another method to enhance performance of the semiconductor quantum oscillation device is to operate it at low temperature, such as at liquid nitrogen or even liquid helium temperatures. At a low temperature, the crystal vibration becomes weak and as a result phonon density is reduced. This will not only be beneficial to direct interband tunneling but also will reduce the non-elastic scattering of coherent carriers while executing Bloch oscillation.
FIG. 10 illustrates in cross-section an example of one device that can be used as a semiconductor quantum oscillation device of the present invention. In this embodiment, the whole device structure is made of GaAs/GaAlAs heterojunction material grown on a Si substrate using MBE, or the like. By using Si as the substrate, a biaxial tensile strained state is obtained for the device structure, and this is beneficial to direct interband tunneling. How strains affect interband tunneling has been described above. In order to reduce defects for the device structure, a thick buffer layer is grown first, then the device structure is grown on the buffer layer to finish the material growth. Device processing is similar to the fabrication of a mesa type photodiode, and includes photolithography, wet chemical etching, dielectric film deposition, metal evaporation, lift-off and alloying, and other steps. In the figure, u stands for undoped in the sense that there is no intentional dopant addition during layer growth; and the super script + with n and p stand for heavily doped. The interband tunneling injection region comprises two undoped GaAs layers and an undoped thin GaAlAs layer with these three layers forming a coupled double quantum well structure. The two GaAs layers forming the quantum well layers both have a thickness of approximately 100 angstroms. The thin GaAlAs layer, which defines one edge of the two quantum well structure, has a thickness of 50 angstrom and an Al composition of 0.2. The other two undoped layers, comprise GaAlAs and define the other edge of the two quantum well structure, which form the two carrier oscillation regions. Both layers have a thickness of 2000 angstrom and an Al composition of 0.4. In FIG. 10, the n-type contact region is made of the n-type GaAlAs layer and the heavily doped n-type GaAs layer; and the corresponding contact electrode, i.e. the non-coherent electron collector, is an ohmic contact formed on the heavily doped n-type GaAs layer. The p-type contact region is made of the p-type GaAlAs layer and the heavily doped p-type GaAs layer; and the corresponding contact electrode, i.e. the non-coherent hole collector, is an ohmic contact formed on the heavily doped p-type GaAs layer. The use of the heavily doped GaAs layer in the contact region is to increase the quality of the contact electrodes. Both the n-type GaAlAs layer and the p-type GaAlAs layer have a thickness of 2000 angstroms and an Al composition of 0.4, the same as the two undoped GaAlAs layers forming the two carrier oscillation regions. The main function of the n-type and p-type GaAlAs layers is to prevent the injection of non-coherent carriers from the two contact electrodes. A strong electric field in the interband tunneling injection region and the two carrier oscillation regions is required for the operation of the semiconductor quantum oscillation device of the present invention. As the electric field is originated from space charges in the contact regions, the above function could be well realized by confining the space charge region to the two doped GaAlAs layers. For the particular exemplary device of FIG. 10, d w1 =d w2 =100, d b =50 Angstroms, and the bandgap of the GaAs quantum well layer E g =1.42 (room temperature). The critical electric field calculated using equation (2) is F c =5.68×10 5 V/cm. In order to produce an electric field of this magnitude, an areal charge density of Fc ∈∈/q=3.6×10 12 /cm 2 is required. As the two doped GaAlAs layers have a doping density of 5×10 17 /cm 2 , the resulting space charge region thickness is about 700 angstroms. Therefore, the 2000-angstrom thickness of these two layers is adequate to confine the space charge region within them.
The spatial amplitude of Bloch oscillations is given by
L=ΔE/eF (3)
where e is the electron charge, F is the electric field, and ΔE is the conduction band width of the electron oscillation region or the valence band width of the hole oscillation region in the direction of the electric field. In order to avoid scattering of Bloch oscillation by impurities in the contact region, the carrier oscillation regions should be designed having a larger thickness than the spatial amplitude calculated using (3) to confine the Bloch oscillation in the oscillation region. For GaAs and other common semiconductor materials, the bandwidth of the conduction band or the valence band along the <100> direction is normally in the range of 2-4 eV. For an electric field of 5.68×10 5 V/cm, the spatial amplitude calculated, based on equation (3), is between 400 to 800 Angstroms. It can be seen that a 2000-Angstrom oscillation region thickness in the exemplary device is adequate.
FIG. 11 is a plot of I-V characteristics obtained experimentally using a Transistor Curve Tracer (QT- 2 ) for one typical device with the structure shown in FIG. 10 . The two electrodes of the device to be tested are connected to the emitter terminal and collector terminal of the instrument, respectively, and the base terminal is not used. Measurement at liquid nitrogen temperature is also performed, and the I-V characteristics obtained are similar to FIG. 10 but with a higher peak current of about 300 A/cm 2 . It can be seen that there is a critical voltage just like the I-V curve shown in FIG. 2, and the critical voltage has a value of about 20V. Based on the total thickness of the interband tunneling injection region and the two carrier oscillation regions and the critical electric field needed to induce direct interband tunneling, an estimate for the critical voltage could be made. For a critical electric field Fc=5.68×10 5 v/cm, the voltage drop across the interband tunneling injection region and the two carrier oscillation regions (with a total thickness of 4500 angstrom) is 24.1V. Considering that a built-in potential drop, which is approximately equal to the band gap of GaAs (Eg=1.42), exists at equilibrium, the estimated critical voltage is 22.7V. It can be seen that the experimentally obtained critical voltage is in good agreement with the estimated voltage. The notable feature of the I-V curve shown in FIG. 11 is that there are two additional segments: the negative segment 3 and segment 4 . These two segments are absent in the I-V curve of FIG. 2 . While doing the measurements, it is also found that by increasing the peak value of the applied voltage (full-wave rectified sine wave), both the peak current jp and width of segment 4 increase accordingly. The above features demonstrate that the semiconductor quantum oscillation device of the present invention is different from all available semiconductor devices regarding operating principle, and that Bloch oscillation of interband tunneling injected carriers are indeed realized. As explained above, the coherent electrons and coherent holes injected into the two oscillation regions do not make a contribution to the terminal current while they execute Bloch oscillation. Therefore, both the positive-resistance segment 3 and negative-resistance segment 4 in FIG. 11 should be related to the dephased electrons and holes in the oscillation regions. Though the coherent electrons and coherent holes while executing Bloch oscillation do not contribute directly to the terminal current, they certainly influence the I-V characteristics of the device through the space-charge effect. The existence of negative-resistance segment 3 and the zero-current segment 4 in FIG. 11 and their dependence on the applied voltage is directly related to the following facts. Both the electron ensemble and hole ensemble are in a quasi-ordered state of far from thermal equilibrium and the electrons and holes while executing Bloch oscillation result in space-charge effects as they are localized in space.
The above description of the semiconductor quantum device of the present invention has explained in detail how the interband tunneling injection region and the two carrier oscillation regions could be realized using a multilayer semiconductor heterojunction structure having a predetermined band-gap and composition profile. It is needed to point out that all the structures given are by way of illustration and make no restriction on the scope of the subject invention. Those skilled in the art will appreciate that the disclosed semiconductor quantum oscillation device can be embodied using other types of band-gap profile and/or other semiconductor heterojunction material systems.
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A semiconductor quantum oscillation device, which realizes Bloch oscillation on the basis of a novel carrier injection scheme, comprises a multilayer semiconductor structure and a means for applying a voltage to said structure. The multilayer structure comprises a tunneling injection region and a pair of oscillation regions which are located on both sides of the tunneling injection region and adjacent to it. The voltage applied across the tunneling region and the pair of oscillation regions causes valence electrons to enter into the conduction band through interband tunneling in the tunneling injection region and leads to electrons and holes being injected into the pair of oscillation regions, respectively. The electrons and holes injected this way undergo quantum oscillation motion and produce far-infrared radiation. The device of the present invention will pave the way for effectively utilizing the electromagnetic spectral resource between the high-end of millimeter-wave and the low-end of far infrared.
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[0001] This application claims priority from U.S. provisional patent application 60/956,089, filed Aug. 15, 2007.
FIELD OF THE INVENTION
[0002] The present application relates generally to brush devices for grasping and manipulating tissue particularly for natural orifice surgery.
BACKGROUND OF THE INVENTION
[0003] The present assignee's U.S. patent publication no. 2007/0225734 and U.S. patent application Ser. No. 11/788,597, both of which are incorporated herein by reference, disclose various natural orifice surgery systems and methods for resolving maladies such as diverticulosis and appendicitis and for removing organs such as the gall bladder. The present application is directed to structures and methods for inverting tissue particularly in connection with natural orifice surgery to facilitate the resolution of the tissue.
SUMMARY OF THE INVENTION
[0004] An apparatus includes a tissue gripping element housed within a tubular member for advancement through a natural orifice to tissue to be inverted pursuant to resolution of a malady associated with the tissue. The tissue gripping element is advanceable out of the tubular member into the tissue to grip the tissue and is retractable into the tubular member to grip the tissue for manipulation of the tissue. The tissue gripping element includes plural discrete gripping points.
[0005] In some embodiments the gripping points can be established by ends of respective bristles oriented generally radially relative to the tubular member. In other embodiments the gripping points are established by ends of respective teeth. The teeth may be arranged on a proximal-facing transverse surface, and plural tubular member teeth can be arranged on a distal-facing transverse surface of the tubular member. The tissue gripping element is distally advanceable relative to the tubular member to space the surfaces from each other and is proximally retractable relative to the tubular member to trap tissue between the surfaces.
[0006] The tubular member may establish a vacuum lumen through which a vacuum can be drawn to attract tissue toward the tubular member. Tissue can be attracted toward an open distal end of the tubular member when a vacuum is drawn in the tubular member, and in some embodiments tissue can also be attracted toward plural vacuum openings formed in the tubular member when a vacuum is drawn in the tubular member. A cover tube may be advanced over the tubular member to block at least some of the vacuum openings.
[0007] If desired, the tissue gripping element can be rotatable relative to the tubular member. Also, a smooth rounded atraumatic surface can be provided for establishing a distal end of the tissue gripping element.
[0008] In another aspect, a method includes establishing a retracted configuration of a tissue manipulation device in which a tissue gripping element is retracted entirely within a sleeve. The tissue gripping element includes plural discrete gripping points. The method also includes providing instructions to advance the tissue manipulation device through a natural body orifice to tissue to be manipulated, providing instructions to advance the tissue gripping element out of the sleeve, and providing instructions to manipulate the tissue gripping element to grip tissue. Instructions to retract the tissue gripping element toward the sleeve can also be provided.
[0009] In another aspect, a system includes a delivery tube advanceable into a natural body orifice toward tissue to be manipulated and an elongated control rod extending from a proximal end of the tube and manipulable by a person. A tissue gripping element is coupled to the control rod and is advanceable out of a distal end of the delivery tube. The gripping element includes plural individual grippers configured to engage tissue and thereby provide a means for manipulating the tissue by manipulating the control rod.
[0010] The details of the present invention, both as to its structure and operation, can best be understood in reference to the accompanying drawings, in which like reference numerals refer to like parts, and in which:
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a perspective partially schematic view of a tissue inversion apparatus, with portions broken away;
[0012] FIG. 2 is a perspective view of the distal end of an alternate tissue inversion apparatus in the extended position;
[0013] FIG. 3 is a perspective view of the distal end of a tissue inversion apparatus in the housed position for advancing the brush toward tissue to be inverted;
[0014] FIG. 4 is a perspective view of the distal end of the tissue inversion apparatus of FIG. 3 , with the brush in the extended position in tissue to be inverted and after a vacuum has been established;
[0015] FIG. 5 is a perspective view of the distal end of the tissue inversion apparatus of FIG. 4 , with the brush retracted part way back into the sleeve to trap tissue;
[0016] FIGS. 6-8 are perspective views of the distal segments of non-limiting implementations of brush inversion apparatus;
[0017] FIGS. 9-12 are schematic diagrams of the distal portion of an alternate tissue inversion apparatus showing how tissue is clamped between opposed jagged surfaces; and
[0018] FIG. 13 is a perspective view of the distal segment of yet another non-limiting implementation of brush inversion apparatus.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0019] Referring initially to FIG. 1 , a system is shown, generally designated 10 , that includes a flexible elongated hollow sleeve-like delivery tube 12 that is advanceable into a natural body orifice such as the mouth or anus toward tissue to be manipulated. If desired, at least a distal sleeve 14 of the delivery tube 12 may be configured with plural vacuum openings 16 such as round holes, elongated slots, etc. as more fully disclosed below. The openings 16 may establish a spiral pattern as shown.
[0020] As shown in FIG. 1 , the delivery tube 12 may terminate proximally at a “wye” connector 18 , one branch of which supports a manipulable elongated control rod 20 around which a collet 22 may be tightened to prevent movement of the rod 20 relative to the “wye” 18 . The other branch of the “wye” forms a lumen that may be connected to a pressure source 24 . The pressure source 24 may be a negative pressure source (a vacuum) or a positive pressure source (such as a fluid pump or pressurized fluid source) for establishing a desired pressure within the delivery tube 12 .
[0021] As also shown in FIG. 1 , a tissue gripping element 26 is coupled to the control rod 20 and is advanceable out of an open distal end 28 of the delivery tube 12 . In the embodiment shown in FIG. 1 , the tissue gripping element 28 includes plural individual, discrete grippers 30 such as brush bristles that are configured to engage tissue and thereby provide a means for manipulating the tissue by manipulating the control rod 20 . At least some of the bristles may be oriented generally radially relative to the delivery tube 12 as shown. If desired, a cover tube 32 may be advanceable over the delivery tube to block at least some of the vacuum openings 16 .
[0022] FIG. 2 shows that in some implementations, a smooth rounded atraumatic surface 34 may be provided on the distal end of the tissue gripping element 26 to facilitate advancing the gripping element 26 into tissue atraumatically to the tissue.
[0023] FIGS. 3-5 illustrate various operational configurations of the system 10 . In FIG. 3 , the gripping element 26 is retracted within the sleeve 14 with no part of the gripping element 26 extended distally beyond the open distal end of the sleeve. In this configuration, the sleeve 14 with gripping element 26 may be advanced through the natural orifice to the tissue sought to be manipulated, such as, e.g., the appendix, gall bladder, diverticulum, etc.
[0024] Once the sleeve 14 is juxtaposed with the tissue, as shown in FIG. 4 the gripping element 26 is advanced by means of the control rod 20 out of the distal end of the sleeve 14 and into tissue 36 , typically into a void that is naturally formed by the tissue. If desired, the interior of the sleeve 14 may be evacuated by appropriately operating the source 24 of pressure shown in FIG. 1 to attract the tissue 36 toward the sleeve 14 , including toward the vacuum openings 16 and the open distal end of the sleeve. Evacuation also causes the tissue to collapse onto the grippers 30 , with the ends of a multitude of grippers establishing anchor points to the tissue. In addition to vacuum or alternatively, the gripping element 26 may be rotated to tighten the tissue onto the grippers 30 . In any case, adequate time may be allocated to permit the vacuum to collapse the tissue.
[0025] By providing multiple points of contact (e.g., multiple bristles), less damage to the tissue is effected during manipulation and furthermore, minimally traumatic disengagement of the gripping element 26 with the tissue should such become necessary is facilitated. To disengage the tissue, a positive pressure source may be actuated to pressurize the interior of the sleeve 14 and thereby urge tissue away from the sleeve and bristles.
[0026] As shown in FIG. 5 the gripping element 26 may be retracted proximally relative to the sleeve 14 to trap or wedge the tissue 36 between the grippers 30 and the interior of the sleeve 14 as shown. With the tissue thus firmly gripped, it may be manipulated as desired, e.g., the tissue may be inverted, moved, retracted, resected, etc. as appropriate for the particular procedure. Instructions may be provided on, e.g., a substrate to effect the above steps.
[0027] FIG. 6 shows that in one non-limiting implementation, a brush 40 with plural generally radially oriented and relatively rigid bristles may be engaged with a delivery tube 42 formed with plural vacuum holes 44 . The diameter “D 1 ” of the brush 40 may be 2.3 mm and the brush may be 20 mm in length. The brush 40 may slide within the tube 42 or it may be stationarily engaged with the tube 42 , in which case a cover tube such as the cover tube 32 shown in FIG. 1 that can be made of, e.g., Teflon™ can be used to enclose the brush 40 during delivery to the tissue site.
[0028] FIG. 7 shows that in another non-limiting implementation, a brush 46 with plural generally radially oriented and relatively rigid bristles may be engaged with a delivery tube 48 formed with plural elongated vacuum notches 50 that do not extend completely through the wall of the tube 48 but that terminate in respective vacuum holes 52 that do extend through the wall of the tube. The notches 50 with holes 52 may be formed in two lines on opposite sides of the tube. The diameter “D 2 ” of the brush 46 may be 2.5 mm and the brush may be 25 mm in length. The brush 46 may slide within the tube 48 or it may be stationarily engaged with the tube 48 , in which case a cover tube such as the cover tube 32 shown in FIG. 1 that can be made of, e.g., Pebax™ can be used to enclose the brush 40 during delivery to the tissue site.
[0029] FIG. 8 shows that in another non-limiting implementation, a brush 54 with plural generally radially oriented and relatively rigid bristles may be engaged with a delivery tube 56 formed with plural elongated vacuum notches 58 that do not extend completely through the wall of the tube 56 but that terminate in respective vacuum holes 60 that do extend through the wall of the tube. The notches 56 with holes 60 may be formed in two lines on opposite sides of the tube, and additional holes 62 may be formed without notches in a spiral pattern as shown. Tape may be used to cover holes that are not desired to be used to establish a vacuum. The brush can be exposed at various lengths relative to the tube. The hole pattern inhibits tissue slippage to minimize unwanted twisting of the appendix.
[0030] FIGS. 9-12 show an alternate system 100 in which a gripping element 102 is slidably engaged with a delivery tube 104 that may be formed with vacuum openings 106 in accordance with disclosure above. As shown, the gripping element 102 includes a rounded smooth atraumatic distal end 108 defining a flat disc-like proximal-facing surface formed with plural teeth 110 . Also, the distal end of the tube 104 defines a distal-facing flat disc-like surface formed with plural tube teeth 112 .
[0031] With this structure, the system 100 is advanced through a natural orifice with the gripping element 102 retracted into the tube 104 ( FIG. 9 ) such that the teeth 110 , 112 mesh, or alternatively are in substantial contact with each other. When positioned in the target tissue the gripping element 102 is advanced away from the tube 104 ( FIG. 10 ) into the tissue and then vacuum is established in the tube 104 ( FIG. 11 ) to attract tissue into the space between the teeth 110 , 112 . The gripping element 102 is then retracted proximally relative to the tube 104 ( FIG. 12 ) to trap tissue between the teeth 110 , 112 . The shaft of the gripping element 102 may further include bristles in accordance with the disclosure above in addition to the structure shown in FIGS. 9-12 .
[0032] FIG. 13 illustrates a gripping element 200 with bristles 202 and atraumatic distal tip 204 that may be slidably engaged with a sleeve 206 . The sleeve 206 may be formed with vacuum openings 208 . A cover tube 210 such as the cover tube 32 shown in FIG. 1 can be used to enclose the bristles and/or to cover the vacuum openings 208 .
[0033] While the particular BRUSH DEVICE FOR GRASPING AND MANIPULATING TISSUE are herein shown and described in detail, it is to be understood that the subject matter which is encompassed by the present invention is limited only by the claims.
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A brush-like element can be housed within a vacuum sleeve for advancement through a natural orifice to tissue, such as an appendix or gall bladder or diverticulum, to be inverted pursuant to resolution of a malady associated with the tissue. The brush is advanced out of the sleeve into the tissue and if desired rotated, and vacuum may also be drawn through the sleeve to further grip the tissue. The brush is then retracted into the sleeve to clamp or trap the tissue for inversion or other manipulation.
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GOVERNMENT RIGHTS
The Government has rights in this invention pursuant to Air Force Contract No. F33615-91-C-5618.
BACKGROUND OF THE INVENTION
The present invention relates to reinforcement of structural members. More particularly, it relates to a vacuum bag process to externally reinforce concrete structural members with advanced composites and to a prefabricated vacuum bag used for that purpose.
Concrete structural members are widely used in the construction of bridges and buildings. For example, many of the concrete bridges connected with the interstate highway system are close to 40 years old and, since bridge deck life commonly averages 35 years, are due for major rehabilitation or replacement.
A conventional method of repairing concrete bridges involves strengthening or stiffening weak or damaged concrete portions by bonding steel plates thereto with an epoxy. This method has the potential to allow for repair of a concrete bridge without major interruption of the use of the bridge. However, corrosion at the epoxy/steel interface leads to a reduced bond strength and an increased likelihood of structural failure. Additionally, the steel plates are cumbersome, heavy, and generally difficult to handle.
The use of light weight corrosion resistant composite plates as a means of rehabilitating cracked beams in box beam bridges has been studied by Chajes et al., "Rehabilitation of Cracked Adjacent Concrete Box Beam Bridges" 13 th Structures Congress, American Society of Civil Engineers (Boston, Mass. 1995). However, Chajes et al. do not suggest any method by which the composite plates can be effectively bonded to the concrete beams in the field, have observed delamination and peel-type failures between the composite plate and the concrete, and have noted that thorough studies are needed to discover an appropriate method of bonding the composite plates to a structure under field conditions.
Accordingly, there is a need for a method of effectively bonding composite plates to a structure to reduce the likelihood of delamination and peel-type failure. Further, there is a need for a means by which a composite plate can be successfully adhered to a structure in an in-situ environment and a non-intrusive manner.
SUMMARY OF THE INVENTION
This need is met by the present invention wherein structural members are externally reinforced with reinforcing material cured against or adhered to the structural member through the use of a prefabricated vacuum bag assembly.
In accordance with one embodiment of the present invention, a method of reinforcing structural members is provided comprising the steps of: providing a reinforcement material to be bonded to a reinforcement surface of a structural member, positioning a vacuum assembly adjacent to an exposed surface of the reinforcement material so as to create an inner space between an exterior surface of the vacuum assembly and the reinforcement surface, and creating a partial vacuum in the inner space so as to force the vacuum assembly and the reinforcement material towards the reinforcement surface.
The positioning step preferably includes sealing a peripheral portion of the vacuum assembly against the structural member, enveloping the reinforcement material with the vacuum assembly, and/or securing the vacuum assembly to the structural member along a continuous path surrounding a periphery of the reinforcement material. The inner space is preferably occupied by the reinforcement material, a porous release film, and a breather element.
The vacuum assembly may comprise a porous film of flexible material, a non-porous film of flexible material, and a sheet of flexible breather material positioned between the porous film and the non-porous film. The porous film may comprise an adhesive release film. The sheet of breather material is preferably adhered to the porous film and the flexible non-porous film. The flexible non-porous film may comprise a plastic film selected from the group consisting of a plastic film including one vacuum port, a plastic film including a plurality of vacuum ports, a plastic film including two symmetrically positioned vacuum ports, and a plastic film including a plurality of symmetrically positioned vacuum ports. The flexible non-porous film may include a peripheral portion defined by a portion of the flexible non-porous film extending beyond the periphery of the sheet of breather material and the peripheral portion may include a continuous sealant. The force is preferably substantially equivalent to a pressure of about 8-12 psi applied uniformly over a predetermined area.
The providing step preferably includes curing the reinforcement material between porous curing release plies to impart a rough surface texture to the reinforcement material.
The method of reinforcing structural members may further comprise the step of mechanically abrading the reinforcement surface, and/or treating the reinforcement surface with an acetone rinse. The method of reinforcing structural members may also further comprise the step of applying an adhesive material between the reinforcement surface of the structural member and an adhesion surface of the reinforcement material. The reinforcement material may comprise a support plate.
In accordance with another embodiment of the present invention, a vacuum enclosure is provided comprising: a porous film of flexible material, a non-porous film of flexible material, and a sheet of flexible breather material positioned between the flexible porous film and the flexible non-porous film. Preferably, the porous film comprises an adhesive release film. The sheet of breather material may be adhered to the porous film and to the non-porous film. The non-porous film preferably comprises a plastic film selected from the group consisting of a plastic film including one vacuum port, a plastic film including a plurality of vacuum ports, a plastic film including two symmetrically positioned vacuum ports, and a plastic film including a plurality of symmetrically positioned vacuum ports. The non-porous film may include a peripheral portion defined by a portion of the non-porous film extending beyond a periphery of the sheet of breather material. The non-porous film preferably has width and length dimensions substantially greater than the width and length dimensions of the porous film and the sheet of breather material.
In accordance with yet another embodiment of the present invention a process of forming a vacuum assembly is provided comprising the steps of: providing a flexible film of porous material, providing a flexible sheet of breather material, providing a flexible film of non-porous material, adhering a first major surface of the sheet of breather material to the porous film, and adhering a second major surface of the sheet of breather material to the non-porous film. The process of forming a vacuum assembly may further comprise the step of fusing first and second longitudinal edges of the porous film and the non-porous film.
Accordingly, it is an object of the present invention to provide a means by which composite plates can be conveniently, efficiently, and effectively bonded to a structure in need of reinforcement.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1 and 2 are side and bottom views, respectively, illustrating the composite plate bonding process according to the present invention; and
FIG. 3 illustrates the process for forming a vacuum enclosure used in the bonding process of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
A method of reinforcing structural members according to the present invention will be described with reference to FIGS. 1 and 2, where like structural elements are indicated with like reference numerals. The structure illustrated in FIGS. 1 and 2 comprises: a composite support plate 10; a concrete structural beam 12 in need of reinforcement or repair and having a reinforcement surface 14, i.e, a beam surface to which the support plate 10 is to be bonded; a layer of adhesive material 16 positioned between the reinforcement surface 14 and an adhesion surface of the support plate 10; a vacuum bag assembly 18 including a porous adhesive release film 20, a breather element 22, vacuum ports 24, and a flexible exterior non-porous plastic film 26; and, a peripheral sealant 28.
The composite support plate 10 is used to reinforce the concrete beam 12 by bonding the support plate 10 to the reinforcement surface 14 of the beam 12 according to the methodology described below. Preferably, prior to bonding, the reinforcement surface 14 is prepared for bonding by removing loose concrete with a wire brush.
The support plate 10 comprises a carbon fiber reinforced plastic (CFRP) plate. One such suitable plate is a graphite/epoxy composite system available from Hercules, Inc., as product number AS4C/1919, and having a ply thickness of 0.007 inches (0.18 mm). The composite plate 10 comprises multiple plies fabricated with 0/0, 0/0/0/0/0, or 0/90/0 lay-ups. For example, the 0/90/0 plate comprises a first 0.007 inch (0.18 mm) ply having fibers substantially aligned parallel to the longitudinal direction of the support plate 10, a second ply having fibers substantially aligned in a width direction of the support plate 10, i.e. oriented 90° from the direction of the first ply, and a third ply having fibers substantially aligned parallel to the fibers in the first layer. The 0/0/0/0/0 plate comprises five 0.007 inch (0.18 mm) thick plies each having fibers substantially aligned parallel to the longitudinal direction of the support plate 10.
Preferably, the fiber content of the CFRP plate is approximately 60% of the plate volume; however, it is contemplated by the present invention that a variety of fiber volumes and a variety of composite materials may be utilized in the support plate 10 without departing from the scope of the present invention.
It is contemplated by the present invention that an uncured reinforcement material, e.g., an uncured resin, or a non-rigid reinforcement material, e.g., an fibrous matt, or a combination of both, may be substituted for the support plate 10 as long as a means is provided whereby the reinforcement material can become cured or rigid after adhesion to the reinforcement surface 14. For example, where a fibrous matt is provided as the reinforcement material the layer of adhesive material 16 is selected such that it will commingle with the fibrous matt and add rigidity to the fibrous matt upon curing of the adhesive. Alternatively, the layer of adhesive material itself could be selected so as to function as the reinforcement material after cure.
To achieve an improved bond between the adhesion surface of the support plate 10 and the reinforcement surface 14, the plate 10 is cured between porous adhesive curing release plies to impart a rough surface texture to the support plate 10. Additionally, the surface of the support plate 10 is mechanically abraded with 240 grit sand paper, and/or rinsed with an acetone rinse.
To facilitate bonding, an adhesive 16 is applied to the reinforcement surface 14 and overlaid with the support plate 10. Two epoxy adhesives which cure above approximately 50° F. (10° C.) are EA9460 from Dexter Hysol, Inc., and Sikadur 31 from Sika Corp., are suitable for use with the present invention. It is contemplated by the present invention that a variety of adhesives 16 may be utilized without departing from the scope of the present invention, including adhesives which cure at other than ambient conditions.
The non-porous plastic film 26 forms a vacuum membrane and is sealed against, and adhered to, the concrete beam 12 around a periphery of the support plate 10 with the peripheral sealant 28 such that the non-porous plastic film 26 encloses an inner space 30 between the flexible exterior non-porous plastic film 26, and the reinforcement surface 14 of the concrete beam 12. The entire support plate 10 is enveloped by the vacuum assembly 18. The peripheral sealant 28 permits adhesion of the non-porous plastic film 26 to, and clean removal from, the concrete beam 12. A suitable peripheral sealant is a polysiloxane based adhesive tape, e.g., the GS B55 sealant tape available from Airtech Int'l. Inc., Carson, Calif. It is contemplated by the present invention that the non-porous plastic film 26 may be sealed against the concrete beam 12 around a periphery of the support plate 10 by any means whereby the vacuum assembly 18 forms a seal against the concrete beam. For example, the vacuum assembly 18 may be forcibly, uniformly, and continuously urged against the concrete beam 12. When sealed against the concrete beam, the non-porous plastic film 26 is sufficiently non-porous so as to enable the maintenance of a significant atmospheric pressure difference between the inner space 30 and the ambient, as described below.
The vacuum assembly 18 includes the porous release film 20, the breather element 22, the vacuum ports 24, and the flexible exterior non-porous plastic film 26. The vacuum ports 24 are created in the plastic film 26 and couple the inner space 30 to vacuum pumps (not shown). In the embodiment shown in FIGS. 1 and 2, two vacuum ports 24 are symmetrically positioned with respect to the support plate 10 to ensure uniform distribution of a compressive bonding force, described below. It is contemplated by the present invention that a single vacuum port, a centrally located vacuum port, a plurality of vacuum ports, or a plurality of symmetrically positioned vacuum ports 24 may be utilized without departing from the scope of the present invention. Further, it is contemplated by the present invention that vacuum ports may be provided in the peripheral sealant 28, the structure to be reinforced, or in any location as long as a vacuum pump is in communication with the inner space 30.
The porous release film 20 act as a clean release barrier between the vacuum assembly 18 and stray adhesive material 16 to prevent adhesion of the vacuum assembly 18 to any adhesive 16 not confined between the support plate 10 and the concrete beam 12 and to the support plate 10 itself. Preferably, the porous release film 20 comprises a halogenated material (Teflon®) and extends at least as far as the breather element 22 and substantially farther than the support plate 10. A perforated release film available from Airtech Int'l. Inc., Carson, Calif., as item number A4000RP, is an example of a suitable material for the porous adhesive release film 20. Air Weave N7, available from Airtech Int'l. Inc., is a 0.25 inch (0.1 mm) thick non-woven polyester fiber matt suitable for use as the breather element 22. Wrightlon 8400, available from Airtech Int'l. Inc., is a nylon bagging film suitable for use as the flexible non-porous plastic film 26.
With the adhesive 16 applied to the reinforcement surface 14 and overlaid with the support plate 10, and with the non-porous plastic film 26 sealed against, and adhered to, the concrete beam 12, as described above, a pressure difference is created between the inner space 30 and the ambient by partially evacuating the inner space 30 through the vacuum ports 24. The porous release film 20 and the breather element 22 permit gaseous/volatile matter present in the inner space 30 to pass through the vacuum ports 24. A compressive bonding force results from the pressure difference and is exerted by the plastic film 26 in the general direction of the reinforcement surface 14. The breather element 22 has dimensions large enough to cover most of the support plate 10 and acts to distribute the compressive bonding force evenly across the support plate 10. It is contemplated by the present invention that the breather element 22 may cover all of the support plate 10 or extend beyond the boundaries of the support plate 10.
The inner space is evacuated to create a force substantially equivalent to a pressure of about 8-12 psi (55-85 kPa) applied uniformly over a the support plate area. The partial vacuum is preferably maintained until the adhesive has cured to its full strength. After the appropriate vacuum period has passed, the temporary nature of the peripheral sealant 28 permits removal of the vacuum assembly 18 from the concrete beam 12. The support plate 10 remains in contact with the reinforcement surface 14 after the vacuum assembly 18 is removed from the concrete beam 12 and functions to add strength and rigidity to the concrete beam 12. It is contemplated by the present invention that the vacuum assembly 18 may or may not be removed from the concrete beam 12 and that the peripheral sealant 28 may be a permanent adhesive if clean removal of the vacuum assembly 18 is not desired. Further, because of practical limits in practicing the present invention, it is contemplated by the present invention that the vacuum may merely be maintained for a portion of the adhesive cure time, e.g., 6 or 24 hours where the substantial full strength cure time of the adhesive is 72 hours. Finally, depending upon the type of adhesive used, the strength of the non-porous plastic film 26, the strength of the peripheral sealant, and the power of the vacuum pumps, it is contemplated by the present invention that the degree of evacuation in the inner space 30 may be altered to create a variety of pressures applied uniformly over the support plate area and to ensure adequate bonding between the support plate 10 and the reinforcement surface 14.
The structure and assembly of a prefabricated vacuum bag or vacuum assembly 18' will be further described with reference to FIG. 3, where like elements are referenced with like reference numerals. To form the prefabricated vacuum assembly 18', the porous release film 20, the breather element 22, and the flexible non-porous plastic film 26 are initially drawn separately through a set of feed rollers 32. The length and width dimensions of the breather element 22 are less than the length and width dimensions of the porous release film 20 and the non-porous plastic film 26 such that, when the layers 20, 22, and 26 are joined in the manner described below, the breather material is not present along an entire outer periphery of the prefabricated vacuum assembly 18'. Similarly, the length and width dimensions of the porous release film 20 are less than the length and width dimensions of the non-porous plastic film 26 such that, when the layers 20, 22, and 26 are joined as described below, the porous release film 20 is not present along an entire outer periphery of the prefabricated vacuum assembly 18'. Preferably, at least approximately 2-4 inches of the outer periphery of the prefabricated vacuum assembly 18' is not occupied by the breather material 22 or the porous release film 20.
The breather element 22 is secured to the porous release film 20 and the flexible non-porous plastic film 26 by applying an adhesive to first and second major sides of the breather element in an adhesive application area 36. The adhesive may be applied through spray application, as a bead, or otherwise, as long as the breather element 22 is prevented from shifting within the prefabricated vacuum assembly 18'. The hot rollers 34 fuse first and second longitudinal edges of the porous release film 20 and the non-porous plastic film 26 by compressing an adhesive bead applied between the release film 20 and the non-porous plastic film 26. It is contemplated by the present invention that the adhesive bead need not be utilized if the temperature of the hot rollers is high enough to cause the release film 20 to adhere to the non-porous plastic film 26. It is also contemplated by the present invention that the longitudinal edges of the porous release film 20 and the non-porous plastic film 26 need not be fused at all if the bond created by the adhesive applied to the first and second major sides of the breather element is sufficiently strong to secure the porous release film 20 and the breather element 22 to the non-porous plastic film 26.
A sheet cutter 38 is provided for cutting the prefabricated vacuum assembly 18' to a predetermined length. Alternatively, a perforator is positioned in place of the cutter 38 so as to permit formation of a continuous length of detachable prefabricated vacuum assemblies. The prefabricated vacuum assembly 18', constructed as described above, is designed to be securely sealed along its outer periphery to the concrete beam 12 to facilitate evacuation of the inner space 30 and bonding of the support plate 10 to the reinforcement surface 14. The vacuum ports 24 are created by punching holes in the flexible non-porous plastic film 26. It is contemplated by the present invention that holes may be punched in the non-porous plastic film 26 manually, following production of the prefabricated vacuum assembly 18', or automatically, at any point in the production process. It is also contemplated by the present invention that a variety of shapes and sizes of vacuum assemblies may be produced and used according to the present invention.
It is contemplated by the present invention that the prefabricated vacuum bag 10' may be used to reinforce structural members, as described above, and may also be used in any process requiring constrictive compression of a single material or a plurality of materials. For example, the prefabricated vacuum bag may be used in element-to-element bonding processes, composite curing processes, single element curing processes, tool forming processes, and adhesive curing processes.
Having described the invention in detail and by reference to preferred embodiments thereof, it will be apparent that modifications and variations are possible without departing from the scope of the invention defined in the appended claims.
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A structural member is reinforced by applying an adhesive material between a reinforcement surface of the structural member and an adhesion surface of a support plate, positioning a vacuum assembly adjacent to an exposed surface of said support plate so as to create an inner space between an exterior surface of said vacuum assembly and said reinforcement surface, and creating a partial vacuum in said inner space so as to force said vacuum assembly and said plate towards said reinforcement surface. A prefabricated vacuum assembly is a vacuum assembly comprising a flexible porous film, a flexible non-porous film, and a flexible sheet of breather material positioned between said porous film and said non-porous film.
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DESCRIPTION
BACKGROUND OF THE INVENTION
The present invention relates to a post puller which may be operated as a jack to provide great leverage for pulling posts or the like from the ground. More particularly it relates to a fence post puller adapted for lifting metal posts of the studded or plain T-type, angletype or U-shaped from the ground.
Metal fence posts often called "steel posts" are employed in many applications such as on farms, ranches, or construction sites for fences and along highways for signs, markers or snowfencing. They are relatively easy to install but sometimes need to be removed or repositioned. Removal or repositioning of the depth of a steel post is difficult without a post puller.
Various prybars and long handled jacks have been employed to lift fence posts out of the ground. Known fence post pullers tend to be large and clumsy or offer little mechanical advantage. One major problem with known fence post pullers is their inability to adequately grip a fence post. Slippage between the fence post puller and the post to be pulled can be dangerous or at the least very frustrating. Another disadvantage of known fence post pullers is the inability to attach to posts having an attached fence fabric such as barbed wire.
SUMMARY OF THE INVENTION
The present invention offers a fence post pulling apparatus having a handle acting as a lever pivotally attached to a ground engaging fulcrum stand with a clevis attached to the end of the lever handle nearest the fulcrum stand. The clevis encircles and engages a central portion of the post. Downward motion on the lever arm causes the clevis to positively engage the post pulling it upward. When the lever arm is raised, the clevis releases its grip on the post sliding down in a ratchet-like fashion to a lower point on the post, reengaging it in a non-slipping manner.
The fulcrum stand terminates in a foot which is disk shaped having an outer circumferal lip. The disk shape stabilized the stand in contact with the ground while the circumferal lip prevents the stand from sinking too deeply into the ground.
The post puller is light weight, being small in size and foldable for easy storage or carrying.
BRIEF DESCRIPTION OF THE FIGURES
A detailed description of one preferred embodiment of the POST PULLER is hereafter described with specific reference being made to the drawings in which:
FIG. 1 is a side-elevation of a fence post puller constructed in accordance with the present invention applied to a post to extract the same from the ground;
FIG. 2 is an enlarged top-view of the post engaging clevis of the present invention;
FIG. 3 is a sectional view of the base stand of FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now more particularly to the drawings, in FIG. 1 is shown a well known type of studded T-post 2 having raised studs 4. The post puller, comprising the invention, includes a handle 10 acting as a lever pivotally connected with fulcrum stand 12 having a ground engaging dish-shaped foot 14. Mounting 16 serves to pivotally attach the handle 10 via pin 18 to the stand 12 and additionally mounts clevis 20 via pin 22 to lever handle 10.
Clevis 20 is made up of straps 24 shaped in the form of a U and held together by spacer block 28 through which pin 22 would be positioned. As shown in FIG. 2 which is a top view of the clevis, pin 26 slidably mounts the clevis to the post to be pulled. Pin 26 is held captive within a tubular holder 30 which has a spring 34 which urges pin 26 to its outward extended position. In use pin 26 is pulled back by pin handle 32 and the jack is placed in a position to allow the clevis to encircle the post to be pulled and pin handle 32 is released which allows spring 34 to push pin 26 from one side of the clevis through the other side. This unique arrangement allows for a quick and easy engagement of the clevis to a central portion of the post to be pulled relieving the need for manual insertion, prevents fumbling with pin 26 or the possibility of losing it.
An additional feature of the clevis are the crossplates or jaws 40 which are placed there to restrict the size of the opening of the clevis and to allow the same clevis to be used on many different shapes of posts, particularly U-shaped posts used along highways for signs and markers or in older fence lines. Space or slot 42 between crossplates 40 adapts the clevis for use with T-shaped and angle posts. The crossplates 40 are mounted on top of clevis straps 24 typically by welding and provide for early contact to the post 2 to clamp the post between the crossplates and post engagement pin 26.
In the use of the device, the post puller is first placed in a position adjacent to the post to be pulled. Then, Pin 26 is drawn back by handle 32 and the clevis placed in engagement with the post. The clevis is attached directly at the proper jacking height without the need to slip the clevis over the top of the post. It is desirable that the jack be used in as near an upright position as possible but would work in a reasonably inclined position also. Next the handle end of the lever is oscillated vertically. As the handle is depressed, the clevis will tend to pivot upon pin 22 so that pin 26 and crossplates 40 engage against their respective adjacent faces of the post, clamping the post at the postconfronting end of the lever handle. Downward movement of the handle raises the post. As the handle-end of the lever is moved upwardly, the frictional engagement of the clevis with the post will tend to retard downward movement thereof with the result that the pivot point at pin 22 will move downward with respect to the clevis 20 thereby disengaging pin 26 and crossplates 40 from the post so that the clevis 20 falls freely downardly to a lower position on the post. The whole operation of the post puller is in a ratchet-like manner alternately gripping and releasing the post.
Shown in FIG. 3 is an expanded cross-sectional view of foot 14. The shape of the foot 14 is in the form of a dish to allow self-centering of the stand to prevent movement when it is placed upon the ground. The outer edge of the foot 14 is in the shape of a flattened circumferal lip as shown by numeral 52. If jack is operated in loose or soft earth, the dish-shaped of 14 will settle into the earth making the stand very stable to lateral movements but not to vertical sinking into the ground. To prevent sinking into the ground, soil that does move out of the way of dish shape 14 is caught by lip 52 and this tends to retard any further vertical settling into the ground due to the pressure exerted upon the fence post puller by lever handle 10. Reinforcement of the stand to foot connection is accomplished by angle braces 50.
The invention is able to engage a post without having to remove any fence wire or fabric being held by the post. The clevis as presently designed is able to handle various sizes and shapes of posts. It is anticipated that if the present clevis is not adequate for a certain shape or size of post that a redesign could be made including the features of the invention as described. Since the construction hereinbefore set forth is capable of a certain range of change or modification without materially departing from the spirit of the invention, I do not limit myself to such specific structure except as hereinafter claimed.
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A post puller having substantially universal application for pulling posts of various cross-sectional configurations and characterized by a pair of transversely spaced jaws carried by the pulling clevis opposite the clevis pin, the clevis being pivotally connected adjacent one end of a lever handle which is pivotally supported by a stand, the space between the jaws accommodating the leg of T-shaped posts, and the jaws engaging the base of the U-shaped posts, during the pulling operation.
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BACKGROUND OF THE INVENTION
The present invention relates to a three-dimensional scanning probe microscope, and more specifically, is directed to such a three-dimensional scanning probe microscope capable of acquiring a plurality of types of physical information of a sample during a single scanning operation or single pass.
As a method for observing a shape of a sample surface and a physical amount characteristic of the sample surface using a conventional scanning probe microscope, an observation method is mainly subdivided into a method for observing a sample while a probe is brought in contact with the sample, and another method for observing a sample while a probe is not brought in contact with the sample.
When a sample is observed by way of the former method, for instance, concave/convex images of a surface of the sample and friction images thereof can be separately observed. On the other hand, when a sample is observed by way of the latter method, physical information emitted from a surface of the sample, for example, a magnetic distribution image and an electrostatic distribution image of the sample can be observed.
In the above-described observation methods, the sample surface is scanned in a two-dimensional manner by the probe so as to be observed, while the probe is brought in contact with the sample surface, or is separated from the sample surface by a predetermined distance. As a result, data which is acquired during a single observation operation merely corresponds to a single physical amount contained in a sample. These observation methods are not especially designed to be capable of acquiring a plurality of physical amounts during a single observation operation. Also, in the conventional observation methods, for instance, in such a case that a magnetic distribution image of a sample is observed, although the two-dimensional magnetic distribution image of the sample where the probe is at a position separated from this sample by a preselected distance can be observed, there is a problem. That is, a three-dimensional magnetic distribution image of the sample cannot be observed. This three-dimensional magnetic distribution image is produced by adding a magnetic distribution of a height direction of the sample to this two-dimensional magnetic distribution image.
The present invention has been made in view of the shortcoming of the above-described conventional techniques, and provides a three-dimensional scanning probe microscope capable of observing a plurality of physical amounts of a sample while an observation is carried out in one pass. Another object of the present invention is to provide a three-dimensional scanning probe microscope capable of acquiring a physical characteristic of a sample in a three-dimensional manner.
SUMMARY OF THE INVENTION
To achieve the above-explained objects, a three-dimensional scanning prove microscope, according to a first feature of the present invention, is featured by being a three-dimensional scanning probe microscope equipped with a probe capable of performing relative scanning operations along an x direction and a y direction in parallel to a surface of a sample, and also a moving operation along a z direction perpendicular to the sample surface with respect to the sample surface, wherein the probe is moved along the z direction at a second frequency in such an amplitude at least defined from a first position where the sample surface is depressed by the probe up to a second position where the probe is not influenced by atomic force with respect to the sample surface so that a plurality of data characteristics can be acquired during the movement of the probe. Also, a second feature of the present invention is featured by that the probe is vibrated at a first frequency (first frequency>second frequency) which is resonated, or forcibly vibrated with the probe.
In accordance with the present invention, since the probe can be periodically and relatively moved from a position where the probe is separated from the sample up to another position where the probe is depressed into this sample with respect to the sample, plural sorts of physical information of the sample can be acquired while the probe is moved within 1 time period. Also, since the information acquired within this 1 time period can be used as the information about one pixel, this scanning operation by the probe is extended over the entire check region of the sample. As a consequence, the plural sorts of physical information of this sample can be acquired during one scanning operation (one pass). Also, since the resultant plural sorts of physical information are acquired from the same point of the sample, these plural sorts of physical information own relative relations with each other, which may contain valuable information.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic block diagram for indicating an arrangement of an embodiment of the present invention.
FIGS. 2A-2D are waveforms charts of signals of major portions in FIG. 1 .
FIG. 3A is a waveform chart of a signal outputted from a second oscillator of FIG. 1, and
FIG. 3B is a diagram for representing a relationship between a sample and a probe operated in response to this signal.
FIG. 4 is a diagram for representing a relationship between the probe and the sample, and a relationship between the probe and data acquired from this probe.
FIG. 5 is a block diagram for representing one example of functions of a control unit shown in FIG. 1 .
FIG. 6 is a block diagram for showing an example of a circuit for measuring a dynamic viscous/elastic characteristic.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the attached drawings, the present invention will be described in detail. FIG. 1 is a schematic block diagram for indicating an arrangement of an embodiment of the present invention.
In this drawing, reference numeral 1 shows a piezoelectric scanning apparatus in which an electrode 1 a used for a z-fine moving operation, 4-split electrodes 1 b , 1 c , 1 d , 1 e ( 1 d and 1 e are not shown) for an x-scanning operation and a y-scanning operation are provided on a cylindrical surface of a cylindrical piezoelectric element. A sample 2 to be monitored is mounted on an upper surface of this piezoelectric scanning apparatus 1 . Above this sample 2 , a cantilever 3 having a probe located opposite to the sample 2 is provided. A vibrating element 4 is fixed on one end of the cantilever 3 , and this vibrating element 4 causes the cantilever 3 to be resonated upon receipt of a signal having a first frequency outputted from a first oscillator 5 . As shown in FIG. 2A, a signal having an amplitude A1 (1 nm≦A1≦500 nm) and a frequency f1 equal to a resonant frequency of the cantilever 3 is outputted from this first oscillator 5 . It should be understood that as this frequency f1, such a frequency may be employed by which the cantilever 3 is forcibly vibrated.
A distortion amount of the above-described cantilever 3 is detected by measuring an incident position of laser light 7 outputted from a laser generator 6 by a position detector 8 . The position detector 8 is constructed by, for instance, a four-segment optical detecting electrodes. This position detector 8 is positioned in such a manner that when the distortion amount of the cantilever 3 becomes 0, the spot of the laser light 7 is located at a center of these four-segment electrodes. As a result, when distortion occurs in the cantilever 3 , the spot of the laser light 7 is moved on the four-segment electrodes, and a difference is produced in voltages outputted by the four-segment electrodes. This voltage difference is amplified by an amplifier 9 to become a signal “a”. The signal “a ” is inputted to a control unit 10 .
As shown in FIG. 2B, the second oscillator 11 outputs such a signal having an amplitude A0 (10 nm≦A0≦3,000 nm) and a frequency f2 (f2<f1). The signal outputted from this second oscillator 11 is added by an adder 13 to a feedback signal outputted from a z-servo system 12 . The added signal is applied to the z-fine-moving electrode 1 a of the piezoelectric scanning apparatus 1 .
An x, y scanning unit 21 produces an x scanning signal and a y scanning signal. The x scanning signal is applied to the electrodes 1 b and 1 d for the x scanning operation, whereas the y scanning signal is applied to the electrodes 1 c and 1 e for the y scanning operation. Also, these x and y scanning signals are sent to a computer 39 . Reference numerals 31 to 34 show A/D converters for converting the input data into digital signals. Reference numerals 35 to 38 indicate memories for storing thereinto the digital data outputted from these A/D converters 31 to 34 , and are, for example, frame memories. A calculating/image displaying computer 39 selectively reads the digital data stored in the memories 35 to 38 , and calculates these digital data to be converted into image display data. Then, the calculating/image displaying computer 39 sends out the image display data to an image display device 22 . The image display device 22 displays a physical characteristic of the sample 2 .
Next, the operations of the three-dimensional scanning probe microscope shown in FIG. 1 will now be summarized with reference to FIGS. 3A and 3B, while paying an attention to a distance between the sample 2 and the above-described probe. In FIGS. 3A and 3B, the same reference numerals shown in FIG. 1 indicate the same, or similar elements. FIG. 3A shows 1 time period “T” of a signal outputted from the second oscillator 11 . This signal may be expressed by, for instance, A0 cos 2 π ft (not the symbol “f” is a frequency, and symbol “t” denotes time) equal to a cosine function. Alternatively, this signal may be expressed by a signal having another waveform.
At a time instant {circle around ( 1 )} when the amplitude of this signal is maximum, as represented by {circle around ( 1 )} in FIG. 3B, the sample 2 is located at the lowermost position, and the distance between the probe and the sample 2 becomes maximum. As previously explained, since the amplitude A0 is sufficiently large, at this time, the probe is located at a reference position sufficiently separated from the sample surface. At a time instant {circle around ( 2 )} of this signal, the sample 2 is lifted up to such a position as represented as {circle around ( 2 )} of FIG. 3B, and thus the probe is made in contact with the surface of the sample 2 . At a time instant {circle around ( 3 )} of the signal, the sample 2 is located at the uppermost position where the probe is depressed into the deepmost position in this sample 2 . At this time, the cantilever 3 is bent to one side.
At a time instant {circle around ( 4 )} of this signal, the sample 2 descends up to the substantially same height as that of the above-described time instant {circle around ( 2 )}. At this time, the depression force by the probe against the sample 2 becomes substantially zero. At time instants {circle around ( 4 )} to {circle around ( 5 )} of the signal, since the sample 2 further descends, the probe is tried to be separated from the sample 2 . However, due to the adsorption force of the sample 2 , the probe is set under such a condition that this probe cannot be separated from the sample 2 . The cantilever 3 is bent to the other side. Then, at a time instant {circle around ( 5 )}, the probe is separated from the sample 2 by releasing the adsorption force of the sample 2 . At a time instant {circle around ( 6 )}, the probe is returned to the original reference position. At the time instant {circle around ( 1 )} of the end of the above-described 1 time period T, the sample 2 is returned to the original position (height).
As indicated in FIG. 3A, a time period defined between the time instant {circle around ( 1 )} and the time instant {circle around ( 2 )} may be referred to as a “non-contact time period”; another time period defined between the time instant {circle around ( 2 )} and the time instant {circle around ( 5 )} may be referred to as a “contact time period”, and another time period defined between the time instant {circle around ( 6 )} and the time instant {circle around ( 1 )} may be referred to as a “non-contact time period”.
When the above-described operation for 1 time period T is accomplished, the probe can acquire the data for 1 pixel among the detected image information of the sample 2 displayed on the image display device 22 .
A waveform of FIG. 2C indicates a waveform of an output signal (waveform at point A) from the position detector 8 of FIG. 1 . Numerals surrounded by circles shown in FIG. 2C correspond to numerals surrounded by circles indicated in FIGS. 3A and 3B. FIG. 2D denotes a relative position of the cantilever 3 in such a case that the sample 2 is fixed at a position of a point “0”.
As shown in FIG. 2 C and FIG. 2D, during a time period defined between a time instant {circle around ( 1 )} and a time instant {circle around ( 2 )}, in response to the signal derived from the first oscillator 5 , while the probe is vibrated at the resonant frequency of the cantilever 3 , this probe approaches to the surface of the sample 2 . At this time, when a certain physical amount (for example, magnetic field, electric field, adsorption force, surface reacted force, electric double layer force in fluid, etc.) is produced from the surface of the sample 2 , this probe is influenced by this physical amount, so that a phase shift occurs in the phases of the resonant frequency. When this phase shift is detected, the physical amount derived from the surface of the sample 2 can be detected as a function of a distance measured from the sample surface.
Next, in another time period defined between a time instant {circle around ( 2 )} and a time instant {circle around ( 3 )}, since the probe is depressed into the sample 2 , hardness information of the sample 2 can be acquired by calculating an inclination of a waveform shown in FIG. 2C during the time period defined between the time instants {circle around ( 2 )} and {circle around ( 3 )}. Next, the feedback control by the z-servo system 12 shown in FIG. 1 is performed in such a manner that the depression distance “hmax” of the probe 2 into the sample 2 at the time instant {circle around ( 3 )} becomes constant, so that the shape information of the surface of this sample 2 can be acquired from the information of this probe.
Furthermore, since a waveform during a time period defined between a time instant {circle around ( 4 )} and a time instant {circle around ( 5 )} is produced by such a fact that the sample 2 absorbs the probe, the viscous information related to the adsorption layer of this sample 2 can be acquired from the inclination of this waveform. Also, at a time instant {circle around ( 6 )}, namely when the probe is separated from the surface of the sample 2 and thereafter is returned to the reference position thereof, the information related to the adsorption force of the above-described adsorption layer can be acquired. FIG. 4 illustrates that the above-explained physical information which can be acquired by the probe during 1 pixel period is indicated at the respective numerical points.
As previously described, according to the present invention, more than 5 types of these physical characteristics of this sample 2 can be acquired by merely scanning the probe only one time with respect to the sample 2 . Also, since the above-described plural types of information are not separately acquired, but can be obtained from the same place at the same time, this acquired information may give rise to very important physical characteristic of the sample 2 .
It should be noted that the time instants indicated in FIG. 2D except the time instant “τn” are indicated while the time instant “t0” at the maximum point of the output signal (FIG. 2B) derived from the second oscillator 11 is set as a reference (namely, t0=0); a time instant “tc” indicates time defined until the probe is made in contact with the sample 2 ; a time instant “Tc” indicates time defined until the probe is depressed into the sample 2 and then reaches the deepmost point; a time instant “Tr” indicates time defined until the probe is separated from the sample 2 ; and also a time instant “tn” shows time 0≦tn<tc. The time instant “τn” denotes time 0<τn<(Tc−tc). The above-explained various time will be used in the below-mentioned description.
Referring now to FIG. 1 and FIG. 5, an arrangement and operations of an apparatus, according to an embodiment, capable of acquiring the above-explained physical information will be described. FIG. 5 is a block diagram for indicating a function of a control unit 10 shown in FIG. 1 .
When a signal “a” shown in FIG. 2C corresponding to the output signal of the position detector 8 is entered into the control unit 10 , this signal “a” is inputted into a low-pass filter 41 , a root-mean-square detector 42 , a phase comparator 43 , and a maximum/minimum value detecting circuit 44 .
The low-pass filter 41 extracts a low frequency component of the signal “a” in order that a frequency component f1 of this signal is eliminated, and then supplies the filtered signal to a sample/hold circuit 48 . When the root-mean-squared calculation value of the signal “a” becomes lower than, or equal to a threshold value, namely a very small amplitude, the root-mean-square detector 42 triggers a trigger signal generator 46 . This trigger signal generator 46 outputs a time signal of the above-described time tc. The timing signal of this time tc is supplied to a second sampling pulse generator 54 so as to initiate this second sampling pulse generator 54 . When the second sampling pulse generator 54 is initiated, the above-described time signals τ1 to τn are outputted.
The phase comparator 43 compares the phase of the signal “a” with the phase of the output signal (FIG. 2A) derived from the first oscillator 5 , and then outputs a phase difference signal to the sample/hold circuit 45 a to 45 d . The maximum/minimum value detecting circuit 44 detects such timing when the signal “a” becomes maximum and minimum, and then outputs the detected timing to the trigger signal generator 47 . The trigger signal generator 47 supplies, for instance, a clear rectangular trigger signal to the sample/hold circuit 49 at such timing Tr when the maximum value of the signal “a” is detected, and supplies a trigger signal to the sample/hold circuit 50 at such timing Tc when the minimum value is detected.
On the other hand, the signal (FIG. 2B) outputted from the second oscillator 11 is processed in a maximum value detecting circuit 51 in such a manner that timing at which this signal becomes maximum is detected. At this detection time instant t0, the trigger signal generator 52 outputs a trigger signal. This trigger signal triggers a first sampling pulse generator 53 , and also resets the sample/hold circuits 45 a to 45 d , 55 a to 55 d , and 48 to 50 .
The first sampling pulse generator 53 outputs time signals t1 to tn (tn<tc) having a preselected time interval in synchronism with this trigger signal. When these time signals t1 to tn are entered into the sample/hold circuits 45 a to 45 d , these sample/hold circuits 45 a to 45 d sample/hold the phase difference signal outputted from the phase comparator 43 at the respective timing thereof. The sample/hold circuits 45 a to 45 d output sampled/held phase difference signals φ1 to φn.
On the other hand, the second sampling pulse generator 54 outputs time signals τ1 to τn (0<τ1, τn<(Tc−tc)) having a preselected time interval in synchronism with this time signal tc. When these time signals τ1 to τn are entered into the sample/hold circuits 55 a to 55 d , these sample/hold circuits 55 a to 55 d sample/hold the low frequency signal outputted from the low-pass filter 41 at the respective timing thereof. The sample/hold circuits 55 a to 55 d output sampled/held values h1 to hn of the signal “a” during the time period defined between the time instant {circle around ( 2 )} and the time instant {circle around ( 3 )}.
A first arithmetic circuit 61 subtracts the value held by the sample/hold circuit 48 from the value held by the sample/hold circuit 49 to thereby produce the above-explained value hrmax. Also, a second arithmetic circuit 62 subtracts the value held by the sample/hold circuit 48 from the value held by the sample/hold circuit 50 to thereby produce the above-described value hmax. It should be noted that since a value obtained at a time instant {circle around ( 4 )} is substantially equal to a value obtained at a time instant {circle around ( 2 )}, the value obtained at the time instant {circle around ( 2 )} may be substituted by the value obtained at the time instant {circle around ( 4 )}.
Next, the physical amount of the sample 2 acquired in accordance with this embodiment will now be explained in detail.
In accordance with this embodiment, the below-mentioned data (1) to (4) may be acquired every pixel (xi, yi) during the above-described 1 time period (1 pixel data acquisition time) T:
(1) hmaxxiyi: a signal of the cantilever 3 for a pixel (xi, yi) at a time instant Tc.
(2) hrmaxxiyi: a signal of the cantilever 3 for the pixel (xi, yi) at a time instant Tr.
(3) φxiyi (t1) to φxiyi (tn): a phase difference between an output signal of the cantilever 3 and an output signal of the first oscillator 5 for the pixel (xi, yi) at a time instant ti.
(4) hxiyi (tc+τ1) to hxiyi (tc+τn): a signal of the cantilever 3 for the pixel (xi, yi) at a time instant tc+τi.
The data hmaxxiyi of the above item (1) is supplied to the z-servo system 12 of FIG. 1 . The z-servo system 12 supplies a feedback signal produced based on this data hmaxxiyi to the z-fine-moving electrode 1 a of the piezoelectric scanning apparatus 1 so as to control that the distance between the probe and the sample 2 becomes constant. At this time, the control values of the z-servo system 12 are converted into digital values by the A/D converter 34 every pixel. These digital control values are stored in the memory 38 . When the signals stored in the memory 38 are displayed on the image display device 22 , the surface shape of the sample 2 can be displayed.
Next, the data hrmaxxiyi of the above-described item (2) are converted into digital values by the A/D converter 31 , and these digital values are stored into the memory 35 . When the digital signals stored in the memory 35 are displayed on the image display device 22 , an adsorption distribution image of the adsorption layer of the sample 2 can be obtained.
Next, the data φxiyi (ti) to φxiyi (tn) of the above-described item (3) are converted into digital values by the A/D converter 32 , and these digital data are stored into the memory 36 . These data φxiyi (ti) to φxiyi (tn) are processed by the calculating/image displaying computer 39 in accordance with the following data converting process operation.
Assuming now that the resonant frequency of the cantilever 3 is “fr”, the below-mentioned formula may be satisfied:
Formula 1
2π fr=ωr={square root over (k/Meff)}
K: spring constant of cantilever
Meff: effective mass of cantilever.
At this time, when the cantilever 3 vibrated at the resonant frequency is positioned close to the surface of the sample 2 , this resonant frequency is influenced by force F of the surface of the sample 2 , so that this resonant frequency “ωr” is changed into ωr′. This resonant frequency ωr′ may be expressed by the below-mentioned formula. It should be noted that as this force F, there are magnetic force, electrostatic force, and Van der Waals force.
Formula 2
Sin ω r′t =Sin(ω rt−φi )=Sin{square root over (( k−∂F/∂hi +L )/ Meff +L )}·t ωr′t=ωrt−φi={square root over (( k−∂F/∂hi +L )/ Meff +L )}·t
φi: phase difference between signal of cantilever 3 and output signal of first oscillator 5 at height “hi” from sample surface;
hi: height from sample surface
∂F/∂hi: differential field at height “hi” from sample surface.
Accordingly,
ω r′= {square root over (( k−∂F/∂hi +L )/ Meff +L )}
As a consequence, ∂ F ∂ hi = k - ω r ′2 Meff
In the above formula, “K” and “Meff” are constant values. As a consequence, a distribution of force F at the distance hi from the surface of the sample 2 with respect to the each of the pixels (xi, yi) can be obtained from the above formula. In other words, a distribution of the formula F along a depth direction from the surface of the sample 2 , namely a distribution of the above-described magnetic force, electrostatic force, and Van der Waals force can be obtained.
It should be noted that the distance hi between the probe and the sample 2 at a time instant “ti” may be expressed by the below-mentioned formula:
hi=|A 0cos (2π tc/T )− A 0cos (2π ti/T )|
where symbol “tc” represents a time instant when the probe is made in contact with the sample surface, and is defined by ti<tc.
Subsequently, the data hxiyi (tc+τ1) to hxiyi (tc+τn) of the above-described item (4) are converted into digital values by the A/D converter 33 , and then the digital values are stored into the memory 37 . As to these data hxiyi (tc+τ1) to hxiyi (tc+τn), the calculating/image display computer 39 executes the below-mentioned data converting process operation.
Considering now a time range during which the probe is depressed into the sample 2 , namely (tc+τ1) to (tc+τn). As a result, a depression distance hpi (tc+τi) of the probe at the time instant (tc+τi) is defined by the following formula:
hpi ( tc+τn )= A 0cos (2π tc/T )= A 0cos {2π( tc/τi )/ T}
As a consequence, force Fpi by the probe which depresses the surface of the sample 2 at the item instant (tc+τi) is given as follows, assuming now that the spring constant of the cantilever 3 is “K”:
Fpi=K·hpi ( tc+τi ).
This force Fpi can be balanced with the reaction force produced from the surface of the sample 2 . As a result, assuming now that a localized spring force of the sample surface is “ks”, the actual move amount of the probe is given as follows, since the signal from the cantilever 3 is equal to hxiyi (tc+τi):
Fpi=K·hpi ( tc+τi )= K·hxiyi ( tc+τi )+ Ks ( tc+τi )· hxiyi ( tc+τi )
Accordingly,
ks ( tc+τi )= K ( hpi ( tc+τi )− hxiyi ( tc+τi ))/ hxiyi ( tc+τi )
The localized spring constant “ks” of the sample surface is calculated in the above manner, and when these data are displayed on the image display device 22 , the hardness distribution of the surface of the sample 2 can be acquired.
Also, a dynamic viscous/elastic characteristic of the sample 2 can be acquired as follows. That is, the probe is made in contact with the sample surface, and while the cantilever 3 is fine-vibrated during a certain section (namely, from time instant {circle around ( 2 )} to time instant {circle around ( 4 )} in FIG. 2C) in the sample, the phases of the vibrations of the cantilever and the phases of the oscillator 5 are measured in the time sequences τ1′ to τn′. Then, phase differences φ1′ to φn′ measured to acquire this dynamic viscous/elastic characteristic of the sample 2 . As readily a circuit for measuring this dynamic viscous/elastic characteristic, a circuit shown in FIG. 6 is merely added to the circuit indicated in FIG. 5 . This measuring circuit may be arranged by a sampling pulse generator 71 for generating sampling pulses τ1′, τ2′, τ3′ and τn′; sample/hold circuits 72 to 75 for sampling/holding the output signal from the phase comparator 43 at the respective timing of these sampling pulses τ1′, τ2′, τ3′ and τn′; an A/D converter 76 for A/D-converting the phase differences φ1′ to φn′ corresponding to the outputs from these·sample/hold circuits 72 to 75 , namely for A/D-converting the viscous/elastic data; and further a memory 77 . The data stored in this memory 77 are then supplied to the computer 39 . In accordance with this circuit, it is possible to acquire viscous data φixiyi (τi′) at a depth point hi′ of a certain point (xi, yi) on the sample surface.
The above-described embodiment has be described based on such an apparatus that the sample 2 is mounted on the piezoelectric scanning apparatus 1 , and this sample 2 is moved along the upper/lower directions. However, the present invention is not limited thereto, but may be modified. For example, the cantilever 3 is fixed on this piezoelectric scanning apparatus 1 , and while the cantilever 3 may be scanned along the x/y directions, this cantilever 3 may be moved in the fine mode along the z direction.
As is readily apparent from the above-described explanations, according to the present invention, the probe is moved along the z direction at the first frequency with such an amplitude defined from the position where at least the sample is depressed by the probe up to the position where the probe does not receive the atom reacted force with respect to the sample surface, and the data are acquired while this probe is moved. As a consequence, there is such an effect that the distributions of the physical amounts (for example, magnetic field, electric field, atom reacted force, etc.) distributed from this sample surface along the depth direction can be monitored in the three-dimensional manner.
Also, there is another effect that plural sorts of data involved by one point of the sample can be simultaneously acquired while the probe is reciprocated in one turn along the z direction, namely while the data of 1 pixel are acquired. Furthermore, this operation is continued over the entire observation region of the sample, so that the natures of the entire sample can be checked in the multiple aspects. There are further effects that since these plural sorts of data are acquired within 1 scanning operation, these plural sorts of data own the mutual relationships, and also the probe microscope with high operability can be provided.
Also, there is a further effect that as the plural sorts of data, at least two sorts of data can be acquired. Concretely speaking, there are the depth-direction distribution of the physical amount (for instance, magnetic field, electric field, atom reacted force, electric double layer force in fluid, etc.) irradiated from the sample surface; the sample hardness information; the surface shape information of the sample; and the information (for instance, viscous degree and adsorption force of adsorption layer) related to the adsorption layer of the sample.
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A signal having a resonant frequency of a cantilever is output by a first oscillator, and supplied to a vibrating element and a control unit to oscillate a probe. A low frequency signal having a large amplitude is output by a second oscillator and supplied to a piezoelectric scanning apparatus. The probe is periodically and relatively moved with respect to the sample between a position where the sample surface is penetrated by the probe and another position where the probe does not penetrate the sample surface and is outside the range of atomic forces caused by the sample. During this movement, the probe movement may be analyzed to obtain a plurality of physical characteristics about the sample, e.g., hardness information of the sample, surface shape information, information related to an adsorption layer of the sample, and information related to physical qualities (for example, electromagnetic field, adsorption force, surface reaction force, electric double layer force in fluid) irradiated from the sample surface along a depth direction.
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This Application claims priority to U.S. Provisional Application Ser. No. 60/522,490, filed Oct. 6, 2004.
BACKGROUND OF THE INVENTION
Many people now routinely carry mobile devices such as mobile phones, personal digital assistants, integrated phones/PDAs or other mobile devices with calendar functions. Existing calendars and personal information management systems are useful to leave reminders for appointment dates and times, but are ignorant of physical location. The lives of everyone, from a busy business executive to a salesperson to a student are not dictated solely by date and time. How much time is wasted when you search for you car in a large parking lot? How often do you pass by an important building, only to make another trip later? How many trips past the grocery store does it take to remember to pick up that required ingredient? Outstanding tasks in our lives are almost always tied to a physical location, yet we have no simple way to leave reminders.
A need exists for help to organize our lives around both time and space. A device and/or service that takes advantage of its location can remind us when we need to pick up an important item from the approaching store, allow us to quickly recall notes about a client site, and allow us to keep track of useful information associated with specific places.
SUMMARY OF THE INVENTION
The number of mobile devices is increasing rapidly. The spatial calendar of the present invention utilizes these mobile devices as platform to address the need for a personal information management system that is aware of the path it travels through both space and time. The spatial calendar utilizes these currently deployed handheld tools to augment both our memory and our perception. Reminders will be provided when you approach an important location, notifications will be sent when you need to do something nearby, and you will be able to easily track down difficult to find items.
The system is mainly a software module that can deliver the functionality described herein as long as it is executed on a device that can supply it with GPS (or other source) reading of its current location. For example, the device can be a GPS-enabled phone, a car navigation system, a cellular phone that can obtain GPS location using cellular-GPS capabilities, a laptop, desk computer, pocket computer, a Palm or BlackBerry Device.
Utilizing the spatial calendar, the user can associate an event reminder to a location in space (Space to Event Association (SEA)). The location can be fed into the device manually, from the map unit, GIS address book unit, or from the current reading of the GPS unit, as well as any other source of GPS location media.
An event reminder can be text and/or audio to remind the user of a specific thing to do or pick once he or she approaches the location. Examples: once at the parking lot of an airport (inside the car or in the vicinity of the car), the user can activate the SEA function to associate a reminder (text, audio, or visual) to the location of his/her vehicle at the airport. In this case the system will automatically read the GPS location of the car and will prompt the user to enter an audio or text event reminder.
The user can create a library of audio and text event reminders and use them in association with geographical locations.
As another example, at home the user can associate an event reminder to the address of a store in his/her way. The reminder message can be simply to pickup milk from a grocery store once the system realizes that the user is in the vicinity of any grocery store or a specified grocery store (specified from map, address, or GPS).
Reminder Triggering: The system keeps a memory of event reminders in conjunction with their GPS locations. The user can specify at what distance from the location of an event the reminder should be triggered. For example, the user can specify that the event reminder “car parking” be triggered once the user is within 500 m from the car. Another example, the user can specify that if he is driving with 2 km distance from a given grocery store a reminder of the event “Pick up diapers on your way home”.
The user provides a functionality that allows the user to combine temporal (time) events with location events. For instance, the user can specify triggering a certain location event reminder can only happen after 7 PM. The same for time events.
Navigation to location events: The invention includes a navigation module which guides the user towards a location event. For instance, the module can guide the user using an onboard map, directional arrow, or clock numbering system (e.g., “the car is at 1 O'clock from you”).
Reminders Retrieval and Display: The invention includes a module that allows the user to display, and scan through stored event reminders, to delete or modify them.
Location Labeling and Storing: The user can label his/her current location with a text description of the location (e.g, Toronto airport, my-favorite JC Penny-), or an audio or visual description. This information is stored in the system's Location Address Book.
Location Address Book: Contains locations labeled and stored by the user, or acquired from other sources (e.g., Locations of places such as parking areas, hotels, parks, gas stations, grocery stores, press stands, etc., or Location Address Books supplied by other users of similar device)
For example, if you open the last container of milk while preparing breakfast, a few quick taps on your mobile device serves as a reminder to yourself. Later that day, on the way home from work, your mobile device notices that you are approaching a grocery store. It has been a long day and you forgot all about breakfast. A pleasant reminder is spoken to you about the milk you need to pick up, with simple directions to the approaching grocery store. You conveniently make a stop at the store to pick up the required milk.
As another example, you return from a pleasant flight, only to be faced with the daunting task of finding your vehicle. As you walk outside, you turn to your mobile device for a little help, and ask it where your vehicle is located. It quickly notifies you to turn left and find your vehicle about 500 m ahead. Your mobile device continues to assist with a “radar” display as you walk toward your destination.
As yet another example, as you enjoy the road ahead, you completely forget about the remaining fuel in your vehicle. Luckily, your mobile device reminds you about the approaching gas station far enough ahead of time for you to exit the highway and stop for gas.
BRIEF DESCRIPTION OF THE DRAWINGS
Other advantages of the present invention can be understood by reference to the following detailed description when considered in connection with the accompanying drawings wherein:
FIG. 1 is a schematic of a spatial calendar system implemented with a limited function mobile phone.
FIG. 2 is a schematic of the spatial calendar system of FIG. 1 implemented with a full function mobile phone/PDA.
FIG. 3 illustrates a space-time event stored in the spatial calendar of FIG. 1 or FIG. 2 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
One embodiment of the spatial calendar system 10 of the present invention is shown in FIG. 1 for use with a limited capability mobile device 12 (e.g. simpler cell phone). The spatial calendar system 10 is shown in FIG. 2 in use with a more capable and independent mobile device 12 a , where some of the services previously performed by the server 24 are performed on the mobile device 12 a . Except where otherwise indicated, the following description applies to both embodiments of the system 10 , 10 a , which will be referenced generically as system 10 , for use with limited and full capability mobile devices 12 , 12 a , which will be referenced generically as mobile device 12 .
The proposed modular architecture of the spatial calendar system 10 shown in FIGS. 1 and 2 is designed to support a simple, transparent user interface on everything from a limited capability mobile device 12 (such as a traditional mobile phone) ( FIG. 1 ) to an integrated PDA/phone to a standalone PDA/GPS device 12 a ( FIG. 2 ).
User Interface: The primary user interface 14 for the user is the mobile device 12 itself, where space-time events can be created, located, and used for automatic notification. The mobile device 12 user interface 14 should be as simple as or simpler than a pen and a pad of paper. The user interface 14 presents notifications from the event management service 16 in addition to event creation, modification, and search.
Event Management Service: The event management service 16 is responsible for monitoring the state of space-time events. This service is also responsible for sending reminders to the user interface 14 at the appropriate places and times when event conditions are satisfied. Knowledge of the maximum speed, time, location, and active space-time events allows the event management service to put the device into low-power mode when event conditions are guaranteed to be false for extended periods of time.
Locator Service: The locator service 18 is responsible for estimating the position of a mobile device 12 (and ideally, the associated user). The physical source 19 of position information is abstracted by this service to both keep the system flexible and robust. Flexibility to incorporate additional or alternate sources of position is important to improve accuracy and coverage. Robustness is achieved by decoupling the decision process from the physical source of position information. The locator service 18 will provide estimates of both position and a measure of accuracy when a physical position source is temporarily unavailable. This service provides both current and historical location information to the event management service 16 . The sources 19 of position information can include: AFLT (Advanced Forward Link Trilateration), or other methods for determining mobile device location using cell towers on a mobile phone network; AGPS (Assisted Global Positioning System), where a bare minimum of data (i.e. one satellite) is received by the phone and sent to the wireless network provider, where cell site location information and phone details are combined to reduce time required for the initial position lock and minimize mobile device power consumption; GPS and Bluetooth (i.e. proximity to other Bluetooth devices with known positions, or where proximity to these devices is relevant in itself). Other sources of position information could be used and will no doubt be implemented in the future.
Database: All space-time event information must be reliably maintained in a personal space-time database 20 for effective notification and future use. Required information can be grouped by visibility: public information 22 a available to everyone, and private information 22 b . The space-time database 20 is maintained on a fixed server 24 in wireless communication with the mobile device 12 .
Public Information 22 a is available to everyone and includes the locations of relevant buildings (grocery store, gas station, post office), and street address details. This public information 22 a may be provided by a third party database or service, such as Microsoft Location Services.
Guaranteed privacy of private information 22 b is very important to most end-users. Space-time event information for one individual will be maintained in isolation from other individuals unless explicit permission is granted.
Mobile Service Components in this architecture are not tied to a specific processor or machine. To take advantage of the full spectrum of mobile devices, from low-end mobile phone to high-end PDA, the event management and locator services are distributed between a fixed hardware platform and the mobile device 12 itself. Operating the event management service 26 and locator service 28 locally on the fully-capable mobile device 12 a results in improved coverage where wireless network connectivity is not available ( FIG. 2 ). Operating the event management services 26 and locator services 28 on the fixed server 24 ( FIG. 1 ) is required to provide notification capabilities on mobile devices 12 with limited capabilities (J2ME/Bell).
In FIG. 2 , an intermediate mobile space-time data cache 30 is used to keep the logic between mobile event management service 26 and locator service 28 consistent with their counterparts on the server 24 . This mobile data cache 30 also helps to minimize response time by avoiding wireless communication when local memory permits. Queries against large datasets, including address lookups may be passed directly through to the fixed server 24 .
A space-time event 40 is shown in FIG. 3 . A simple set of outstanding space-time events 40 is maintained for each individual in the personal space-time database 20 ( FIGS. 1 and 2 ). Each space-time event 40 may be associated with any combination of location region and/or time interval for future notification. Examples of these space-time event descriptions include; pick up cereal whenever you are near a grocery store (associated with any grocery store—i.e. the event is associated with a generic category of locations, not a specific geographic location), pick up prototype from Bob the next time you visit (associated with Bob at your remote office), or visit the fireworks if you are in Niagara Falls on a Friday night.
Each space-time event 40 is associated with a specific user 42 (or with a specific mobile device 12 ( FIGS. 1 and 2 )) and includes a simple human-readable description 44 . This description 44 does not have to be meaningful to the software, only to the user. The description 44 can be text, an audio clip, video clip, image and or combination of these.
The space-time event 40 also includes space condition(s) 46 , which can be a single physical location or a set or category of locations. A fixed location is defined by latitude, longitude, and a description of the surrounding region. In the disclosed embodiment, the space conditions 46 may be circles centered on a location 48 (the latitude+longitude) and described by a radius 50 . A space condition 46 is considered satisfied when a predefined region around the mobile device 12 overlaps the region (defined by the radius 50 ) surrounding the fixed location 48 . A fixed location 48 can optionally include a human readable description or address used to resolve the latitude+longitude. Examples of fixed locations include a specific store (i.e. Zehrs #45), one office, or a known address, a set of locations defined by a human readable description (i.e. “Grocery stores”, or “Gas stations”) and one or more fixed locations. When measuring the distance or finding directions to a set of locations, the closest fixed location 48 is considered.
Each space-time event 40 can optionally include time conditions 56 . Time conditions 56 can be specified as a fixed absolute time interval, relative time interval (do this event AFTER some other event is completed), or sets of time intervals. Time intervals require at least one bound (i.e. anytime after Nov. 2, 2004). A relative time interval is specified using an offset from the completion time of another space-time event 40 . (i.e. go back to collect a soil sample 7 days after the last time you collected a sample). A set of time intervals can be used to define recurring or regular events. Arbitrary sets of time intervals can be defined, in addition to time intervals that are repeated after fixed durations (i.e. weekly, daily). Repeated time intervals can include “repeat until” and “start repeating from” times.
Each space-time event 40 includes a status 60 (Completion). The number of times an event has been triggered is maintained, along with the corresponding dates and times. This information distinguishes events just entered into the system from old events, and may be useful for the user to filter information and also for the trigger type logic. The date and time the event was created or modified is also maintained.
The user configures the notification rules 62 of the space-time event 40 to notify the user: a) the first time all of its conditions are satisfied; b) each time all of its conditions are satisfied; or c) never.
The space-time event 40 can include associated notes 66 . A note 66 is useful to leave a long reminder for a future visit. The note 66 can be text, audio, image and/or video.
The user can create, remove, and modify all space-time events 40 directly from the mobile device 12 .
The user can create a “thumbtack on the map,” or location marker at the user's current location with minimal user interaction (this is particularly useful to remember where you left your car). This action creates a space-time event 40 with a space condition 46 , a reasonable default radius 50 , and no trigger for notification in the notification rules 62 . Uses for an event 40 with only a space condition 46 include helping to remember where a vehicle was parked in an airport or other large parking space, and also to leave location specific notes 66 as useful reminders for future visits. More complex events can be created by completing the space-time event 40 description 44 . An event 40 must have at least one of: description 44 , space condition 46 , time condition 56 . All other event information is optional.
Space conditions 46 can be entered: a) Automatically using the current location+a reasonable default radius 50 that the user can override and modify; b) Resolved from an address or range of addresses (postal code)+a reasonable default radius (perhaps based on building density) that the user can override and modify; c) Selected on a map (including radius), or d) Selected from known locations or location sets (presented in a way to minimize effort—perhaps ordered by favorites, most frequently used, most recently used, proximity to current location, and/or some combination of these). Known locations will include a default radius. The user can override a default radius 50 with a few predefined alternate values or with a manually specified radius.
An event 40 can be modified either directly when its conditions are met and the user is notified, or indirectly by first searching for the event. Events 40 can be sorted by name, proximity, date entered, date last triggered, time condition, and filtered by: a) Freeform text (in description, address, or notes); b) Proximity to a given location (specify location as address or using a map). The relative age of locations on a map will be indicated (i.e. brighter=newer, darker=older). c) Date entered; d) Date triggered; e) Time condition (an interval). Once an event is located, any of its details can be modified or the event itself can be removed. If the conditions of an event are modified, the event is considered a new event for the purposes of the trigger type “the first time all the conditions are met.”
The user will be notified as soon as all of the space conditions 46 and time conditions 56 of an event 40 are satisfied. Notification methods include optional audible prompts, vibration, and visual details about the space-time event 40 . An event 40 with no trigger, such as a location marker where you left your car in the parking lot, will only generate passive visual messages when its conditions are satisfied. Events with triggers may also generate audible prompts or vibration when their conditions are satisfied. The desired notification rules 62 (audible, silent, display only) can be set by the user and remain in effect for all future notifications until changed. When an event's conditions are met, the user can (easily): a) Silence/Acknowledge.; b) Postpone. (Postponing an event will notify the user again after either a user specified reasonable time duration (e.g. 15 minutes) or when the conditions are about to change from true to false, whichever occurs first); c) Do nothing; d) Change the event's trigger type (fire the next time, always, never); e) Delete; or f) Edit or view further event details (notes, last trigger, etc.)
Unnecessary notifications are avoided to prevent false alarms, by using hysteresis around space conditions 46 and/or a minimum time or distance between successive notifications. The velocity of the user and precision of location measurements may also be used to determine if space conditions 46 are satisfied. Velocity and precision is important to accommodate both travel by foot and travel by vehicle. A region around the user that includes a predicted path over a short time period will be considered. If any part of the region around the user overlaps with any part of the region defined in a space condition, the space condition 46 is satisfied. When event notifications occur at the same time (all conditions are met for more than one event), the most recent event is shown to the user with an indication that multiple events occurred.
Lost (but previously marked) locations are found using the same mobile device interface. The same search options exist whether modifying an event or trying to find a lost location. Events with associated space conditions are included in the search, along with known locations (gas stations, grocery stores, other points of interest). Once a location is selected, either relative arrows and distance or cardinal direction and distance will be provided, depending on availability of orientation information. The user can then request map directions (obtained using an existing navigation application). Depending on accuracy and availability of location information, the mobile device can also be used to help find a marker with a regular audible (i.e. “Geiger counter mode”) or visual (“radar mode”) indication of proximity while the user is moving. An event can be directly modified or removed at any time after it is selected. A map with road directions can be provided on traditional mobile phones by integrating with Microsoft's Map Location Service.
The user does not need to sift through unnecessary information. Predefined sets of locations are provided, including grocery stores, gas stations, and hotels, but the user can: a) Define personal sets of locations. This can be useful for a real-estate agent to add sets of houses they are trying to push, or an individual that prefers certain types of grocery stores. b) Hide/remove predefined sets that are of no use to the individual c) Define aliases or abbreviations for commonly used locations (“Moe's”, or “office”) d) Define aliases or abbreviations for commonly used time intervals (“morning” or “after dinner” have different meanings depending on an individual's schedule) Aliases and custom/personal sets of locations can be used to minimize data entry time.
Preferably, the management of space-time events 40 can also be done using a desktop PC and/or a web interface.
A space condition 46 can be added that is tied to another mobile device 12 (phone, vehicle), not to a fixed longitude/latitude. For privacy reasons, the user of a mobile device 12 must explicitly grant permission to expose their location to other mobile devices 12 . Uses for mobile locations include specifying events as “remember to pick up the briefcase the next time you are in the car” (with an appropriate bluetooth-enabled car), or notification when a delivery vehicle arrives for a pick-up or delivery. Minor adjustments to this can also provide virtual fence functionality for pets/hunters/people.
The user can also send or share some or all of his personal space-time events 40 with others. For example, by choosing to “Share an Event,” shared events allow any person in a group of mobile device 12 users to accomplish the task. Some form of task selection/assignment should be possible, and once a shared item is marked completed, it should be marked completed for everyone.
The user can also send a space-time event 40 to another user, so that the space-time event 40 will be added to their personal space-time events 40 . The user can also send location details via SMS, instant messaging, or email to users without direct access to the system 10 . The user can also leave a virtual note in a public place for future interested visitors (e.g. graffiti without property damage, or food reviews left at the restaurant by previous customers).
Realistically, a person will not spend the time and effort to manage more than one organizer/PIM system. Synchronizing space-time events with existing desktop applications (e.g Outlook) is one option to reduce double-entry. It may be difficult to preserve the space information of events 40 , but use of contact names is useful for address lookups by name.
The system 10 also may utilize predictive reasoning. Knowing the location and time of events 40 allows your mobile device 12 to also predict how long it will take for you to travel to a meeting or other scheduled appointment from the user's current location. Reminders should take this time into consideration and notify the user, giving enough time for the user to actually travel to their appointment. One approach to include predictive reasoning is to add a new trigger type for an appointment or meeting, and include relevant logic in the event notification service.
The system 10 also provides inter-device communication. Modern phones and vehicles communicate without user intervention to use the vehicle sound system for hands free communication. The device 12 can also take advantage of passing devices to help determine location. For example, the device keeps track of when the user leaves their vehicle and automatically stores a “thumbtack” to help find it later (no user effort/time).
With an integrated camera, the mobile device 12 can also take images with embedded location information. store and find images based on where they were taken.
In accordance with the provisions of the patent statutes and jurisprudence, exemplary configurations described above are considered to represent a preferred embodiment of the invention. However, it should be noted that the invention can be practiced otherwise than as specifically illustrated and described without departing from its spirit or scope. Alphanumeric identifiers in method steps are for ease of reference in dependent claims and do not signify a required sequence unless otherwise specified.
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Utilizing a spatial calendar device and service, the user can associate an event reminder to a location in space. The location can be fed into the device manually, from the map unit, GIS address book unit, or from the current reading of the GPS unit, as well as any other source of GPS location media. An event reminder can be text and/or audio to remind the user of a specific thing to do or pick once he or she approaches the location. Examples: once at the parking lot of an airport (inside the car or in the vicinity of the car), the user can associate a reminder (text, audio, or visual) to the location of his/her vehicle at the airport. In this case the system will automatically read the GPS location of the car and will prompt the user to enter an audio or text event reminder.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This present application is a continuation of PCT/RU2004/000396, filed Oct. 8, 2004, and which claims the benefit of Russian application No. 2003129927, filed Oct. 10, 2003, all of which are hereby incorporated by reference in their entirety.
FIELD OF THE INVENTION
[0002] The invention relates to methods and devices for forming wavy (wavelike) patterns with a period of about 100 nm or less on the surface of materials using ion fluxes and devices for surface polishing.
BACKGROUND OF THE INVENTION
[0003] A large variety of applications in semiconductor and optoelectronics industries can benefit from development of efficient methods for forming wavelike patterns on the surface of semiconductor materials. While different applications require different degrees of coherency, the structures with higher coherency and smaller feature size are usually associated with higher performance.
[0004] A method for forming wavelike patterns upon silicon surface as a nanostructure was disclosed in Russian Patent Application RU 99124768. In this method, silicon is sputtered with a homogeneous ion flux (flow) of molecular nitrogen N 2 + until a periodic wavelike nanostructure with the nanostructure wave crests orientated perpendicular to a plane of ion incidence is formed.
[0005] First, a set of parameters, defining the geometry of an emerging wavelike nanostructure and the sputtering depths D m and D F , corresponding to the commencement and completion of the growth of nanostructure wave amplitude, is selected. This set of parameters includes ion energy, an angle of ion incidence upon the silicon surface, silicon temperature, and a depth of ion penetration into the silicon. All these parameters are selected based upon a wavelength of the nanostructure. The method uses a N 2 + —Si system to form a wavelike nanostructure.
[0006] It is also known that gallium arsenide sputtered with O 2 + ions (O 2 + —GaAs system) leads to formation of a wavelike nanostructure (Karen A., Nakagawa Y., Hatada M., Okino K., Soeda F., Ishitani A. Quantitave Investigation of the O 2 + -Induced Topography of GaAs and other III-V Semiconductors: an STM Study of the Ripple Formation and Suppression of the Secondary Ion Yield Change by Sample Rotation.—Surf. and Interf. Anal., 1995, v. 23, p. 506-513). A useful property of the said nanostructure is a sufficiently high aspect ratio (i.e. the ratio of wave amplitude to wavelength or a wave period). However, the degree of coherency and planarity of wavelike nanostructures being formed in the O 2 + —GaAs system is low.
[0007] It is also known that sputtering of silicon with a flux of molecular oxygen ions (O 2 + —Si system) leads to a formation of a wavelike pattern structure (Vajo J. J., Doty R. E., Cirlin E. H. Influence of O 2 + energy, flux and fluency on the formation and growth of sputtering-induced ripple topography on silicon.—J. Vac. Sci. Technol. A, 1996, v. 14, No 5, p. 2709-2720).
[0008] Using scanning electron microscopy (SEM) the inventors have learned that at a certain depth of the silicon sputtering D m corresponding to the commencement of an intensive growth of amplitude of a wavelike pattern structure a low-amplitude structure pattern is formed in the O 2 + —Si system. These early-stage structures exhibit higher coherency and larger uninterrupted length of the wave structures as compared with the N 2 + —Si system. However, continued sputtering with oxygen ions in the O 2 + —Si system, while increasing amplitude of the waves, results in a considerable deterioration of coherency and planarity of the structure. On the contrary, a wavelike pattern structure formed in N 2 + —Si is notable for a high degree of planarity extending to the sputtering depths equal to 3*D F .
[0009] A prior art system having a plasma electrode with a matrix of apertures for forming an ion beam matrix out of general plasma was described in a U.S. Pat. No. 6,486,480 and a paper (K. L. Scott, T.-J. King, M. A. Lieberman, K.-N. Leung “Pattern generators and microcolumns for ion lithography”—Journal of Vacuum Science and Technology B, v. 18 (6), 2000, pp. 3172-3176.) The system described in these references is not capable of producing the patterns with required minimum size.
[0010] Another prior art system for forming patterns on surfaces of wafers was disclosed in Russian Pat. No. RU 2,180,885. It has a block for forming a matrix of oblique linear ion beams implemented as a plasma electrode with the matrix of linear apertures positioned according to the required disposition of the arrays of nanolines on the silicon surface and a precision stage for transferring of a wafer across the sheet ion beams. However this device requires a complex system for controlling and focusing ion beams.
[0011] Therefore there remains a need for effective and relatively inexpensive techniques and devices for forming highly coherent wavelike nanostructures.
SUMMARY OF THE INVENTION
[0012] An important technical result achieved by implementation of one of the preferred embodiments of the proposed technique is a substantial improvement of the coherency of a wavelike structure being formed.
[0013] This can be achieved by using gallium arsenide instead of the silicon and sputtering it with N 2 + -ion flux. In other words, instead of N 2 + —Si system, N 2 + —GaAs system is used. Thus, the gallium arsenide irradiation with N 2 + leads to the formation of wavelike nanostructures with much higher coherency.
[0014] Preferably, layers of amorphous gallium arsenide are used. Preferably, the layers of amorphous gallium arsenide are formed by magnetron sputtering.
[0015] Preferably, the N 2 + -ion incidence angle is selected in the 55° to 60° range relative to the normal to the GaAs surface.
[0016] Preferably, the N 2 + -ion energy is selected in the 6 to 8 keV range.
[0017] Preferably, the GaAs is sputtered with N 2 + -ions up to a depth D F =1 micron.
[0018] Preferably, to increase the amplitude of a wavelike nanostructure formed in a N 2 + —GaAs system, an additional sputtering is carried out with O 2 + ion flux in a bombardment plane coinciding with the bombardment plane of the N 2 + ions.
[0019] Preferably, the energy and the angle of bombardment with O 2 + ions in the additional sputtering is selected in such a way that the wavelengths in N 2 + —GaAs and O 2 + —GaAs systems are equal.
[0020] Preferably, the amplitude growth of a wavelike nanostructure under the additional sputtering with O 2 + ions is controlled by the secondary-emission signal.
[0021] Preferably, the signals of secondary electron, ion or photon emission are used as a secondary-emission signal.
[0022] Preferably, the additional irradiation with O 2 + ions is carried out only until the moment when the secondary-emission signal is saturated.
[0023] Another important technical result achieved by implementing a second preferred embodiment also results in an additional improvement of the coherency of a wavelike pattern structure being formed. This can be achieved by carrying out the silicon sputtering in two stages. First, a low-amplitude wavelike nanostructure with an increased coherency at the sputtering depth D m is formed with O 2 + ion flux in an O 2 + —Si system and subsequently a further silicon sputtering with N 2 + ions in the N 2 + +—Si system is carried out until the growth of the amplitude of a wavelike nanostructure at the sputtering depth D F is saturated. Meanwhile, the bombardment planes for O 2 + and N 2 + ions coincide and the energy and the angle of ion bombardment are selected in such a way that the wavelengths of the wavelike pattern structure in O 2 + —Si and N 2 + —Si are equal.
[0024] Preferably, the layers of amorphous silicon are used.
[0025] Preferably, the formation of a wavelike nanostructure is controlled by the secondary-emission signals.
[0026] Implementation of the third preferred embodiment also resulted in an improvement of the coherency of a wavelike pattern structure being formed. This can be achieved through carrying out of a preliminary directional polishing of the silicon surface. After that a wavelike pattern structure in N 2 + —Si system is formed so that the orientation of the wave crests coincide with the polishing direction.
[0027] Preferably, abrasives containing small particles, such as alumina, silica and chromium oxide are used for directional polishing.
[0028] An implementation of the fourth preferred embodiment results in the elimination of the system for deflection and focusing of the sheet ion beams and allows forming arrays of nanolines with a normal incidence of the sheet beams.
[0029] This can be achieved by the use of a block for forming a matrix of sheet ion beams that assures a normal incidence of beams upon the silicon surface. The device could be used for forming coherent wavelike nanostructures upon silicon surfaces with a period much smaller than the width of an ion beam. It makes the device different from the known prior art applied in ion beam projection lithography, i.e. forming the lines in the resist with a width comparable with a diameter of an ion beam. In addition, the preferred embodiments implement a matrix of the sheet beams instead of a matrix of circular beams. A precision stage can be used to transfer the wafer across the sheet of beams.
[0030] Preferably, the width of sheet ion beams is about 0.5 micron and their ion energy should be approximately equal to 5 keV.
[0031] Preferably, the precision stage transfers the wafer at a velocity determined by the following formula:
[0000] V =( I L ·Y·A )/( p·D F ·N A ·e )
[0032] where I L is a linear current density of sheet ion beam, A/cm;
[0033] Y is a sputtering yield as calculated with respect to one atom of nitrogen;
[0034] A is a molecular mass of the silicon, gram;
[0035] D F is a coherent wavelike structure formation depth, cm;
[0036] N A is Avogadro's number, 6.022·10 23 mole −1
[0037] e is the electron charge, 1.6·10 −19 C.
[0038] Preferably, a precision stage for a wafer transfers the wafer at a velocity controlled by a secondary electronic emission signal from a test cell set up on the precision stage.
[0039] An implementation of another preferred embodiment results in a novel design of a device for directed wafer polishing. This result can be achieved by implementing a wafer holder to hold a wafer in a fixed position with respect to the direction of the band movement.
BRIEF DESCRIPTION OF DRAWINGS
[0040] FIG. 1A schematically illustrates a process of formation of a coherent low-amplitude wavelike nanostructure upon a gallium arsenide surface by sputtering with N 2 + ions and the geometry of an individual wave.
[0041] FIG. 1B schematically illustrates the process of formation of a coherent wavelike nanostructure upon a gallium arsenide surface with increased amplitude resulting from additional sputtering with O 2 + ions and the geometry of an individual wave.
[0042] FIG. 1C shows a SEM-image of a coherent nanostructure formed in N 2 + —GaAs with a subsequent additional sputtering with O 2 + ions.
[0043] FIG. 1D shows a SEM-image of a coherent nanostructure formed in N 2 + —GaAs with a subsequent additional sputtering with O 2 + ions.
[0044] FIG. 2A shows a SEM-image of a wavelike nanostructure formed in a N 2 + —Si system.
[0045] FIG. 2B shows a SEM-image of a wavelike nanostructure formed in an O 2 + —Si system at a depth D m after a subsequent additional sputtering with N 2 + ions.
[0046] FIG. 3A shows a SEM-image of a wavelike nanostructure formed in a N 2 + —Si system.
[0047] FIG. 3B shows a SEM-image of a wavelike nanostructure formed in N 2 + —Si system with preliminary directed surface polishing with the GOI paste.
[0048] FIG. 4A schematically illustrates a cross-section of a block for forming a matrix of sheet beams.
[0049] FIG. 4B schematically illustrates a view from above of a plasma electrode.
[0050] FIG. 4C schematically illustrates a device for forming coherent wavelike nanostructures.
[0051] FIG. 5 schematically illustrates a device for directed polishing.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0052] Detailed descriptions of the preferred embodiments are provided herein. It is to be understood, however, that the present inventions may be embodied in various forms. Therefore, specific implementations disclosed herein are not to be interpreted as limiting.
[0053] FIG. 1A schematically shows a process of forming a wavelike nanostructure in a N 2 + —GaAs structure. An ion beam is scanned in a raster pattern on the surface of the material to provide for a homogeneous ion flux. FIG. 1A shows a view coinciding with a plane of ion bombardment i.e. with a plane of ion incidence, the plane which is defined by a normal to the surface of the material and a vector oriented in the direction of the ion beam i.e. ion flow. For example, a highly coherent wavelike nanostructure with a wavelength of λ=130 nm is formed by choosing the angle of ion bombardment relative to the normal of a GaAs surface in the range approximately equal to θ=55-58° with the N 2 + ion energy about E=8 keV and a sputtering depth D F of about 1 micron. This nanostructure has almost no wave abruptions and a very small number of wave intersections. The wave crests are oriented perpendicular to a plane of ion bombardment. With an increase of the irradiation dose, up to a sputtering depth of 35 micron the nanostructure does not undergo any significant transformations. Observation through a scanning electron microscope (SEM) of a GaAs crystal sample with a wavelike nanostructure obtained at E=8 keV and θ=56° allowed observation of the geometry of an individual wave. The wave amplitude was 13 nm at λ=130 nm. The wave's slopes were inclined by 8-9° relative to the horizontal direction. Consequently, the local angles of bombardment of waves' slopes are equal to 47° and 65° and protracted sputtering does not alter these angles.
[0054] In this particular N 2 + —GaAs system a wavelike nanostructure observed through a SEM is not formed at angles θ>60° (E=8 keV) as well as at the ion energy E<6 keV and θ=56°. However, at E=6 keV and θ=56° a wavelike nanostructure with λ=123 nm is formed. In the absence of a wavelike nanostructure at θ>60°, solitary cone-shaped formations are observed at the bottom and the slopes of a crater formed by ion sputtering. At E=8 keV in the angles range of θ=45-55°, a low-coherent, low-amplitude periodic nanostructure is formed. It undergoes a progressing perturbation when the dose of ion irradiation is increased. A similar progressing perturbation is also typical for O 2 + —GaAs and O 2 + —Si systems.
[0055] No influence of a process of forming a wavelike nanostructure upon an emission of Auger-electrons was detected; consequently, in situ registration of this process was not made possible.
[0056] Through SEM observation of a surface of the ion beam etched craters formed by N 2 + ions at a GaAs surface at E=8 keV and θ=55° and at various irradiation doses, a depth of the wavelike nanostructure formation of 1 micron was ascertained.
[0057] For the purpose of increasing the amplitude of the wavelike nanostructure formed in N 2 + —GaAs system and for increasing a tilt angle of the wave slopes, experiments with a two-stage formation of a wavelike nanostructure were carried out. At the first stage, a wavelike nanostructure with λ=128 nm at a sputtering depth of 1.5 micron under the conditions of E=8 keV and θ=56.7° was formed in a N 2 + —GaAs system. These conditions provided for maximum coherency of the nanostructure. Thereupon, a sputtering of this wavelike nanostructure was performed with O 2 + ions under the conditions of E=5.5 keV and θ=39° with various ion irradiation doses. The process of an additional sputtering of a wavelike nanostructure is illustrated in FIG. 1B . The bombardment planes of O 2 + and N 2 + ions were coincident. A dose of irradiation with O 2 + ions was selected based on the time during which a secondary-emission signal of GaO + ions reached a saturation point. This growth and saturation of the emission signal reflects the growth and saturation of a tilt angle of the wave slopes of a nanostructure. This relationship was also observed with As + or AsO + secondary ions in the O 2 + —GaAs system.
[0058] In these experiments the growth of the GaO + emission signal reached saturation within 4 minutes. FIGS. 1C and 1D show SEM-images of wavelike nanostructures with λ=123 nm formed as a result of a two-study process with a consequent sputtering with O 2 + ions for a period of 1.5 and 2.5 minutes accordingly. The contrast amplification of a SEM-image in a secondary electron emission with the increase of O 2 + ion irradiation dose indicates an increase of a tilt angle of the wave slopes. The comparison of FIGS. 1C and 1D shows that an increase of a dose of irradiation with O 2 + ions does not significantly influence the ordering of an initial wavelike nanostructure obtained in the N 2 + —GaAs system.
[0059] For certain applications it is preferable to form layers of amorphous GaAs on surfaces of various materials by means of GaAs target magnetron sputtering.
[0060] SEM observations of an evolution of the morphology of the ripples shows that it is possible to achieve higher coherency of the waves at a sputtering depth D m . As compared to the N 2 + —Si system, in the O 2 + —Si system wavelike nanostructures formed at depths of D m have considerably fewer wave abruptions. These considerations suggest a method for forming highly coherent wavelike nanostructures based on a two-stage formation process. In one preferred embodiment, at the first stage, in the O 2 + —Si system, a wavelike nanostructure was formed with λ=130 nm at E=4 keV and θ=47° at a sputtering depth D m =1350 nm. The parameters for the second stage were selected to achieve equal wavelengths in the O 2 + —Si and the N 2 + —Si systems. At the second stage, the wavelike nanostructure was sputtered with N 2 + ions at E=8 keV and θ=43° up to a final depth D=1670 nm. The depth of the additional sputtering in the N 2 + —Si system is equal to 320 nm and shows the conditions for the second stage of forming the wavelike nanostructure. The bombardment planes for O 2 + and N 2 + ions coincided. The two-stage process resulted in a wavelike nanostructure with λ=140 nm shown in FIG. 2B . For comparison purposes, FIG. 2A shows the image of a wavelike nanostructure formed in the one-stage process in N 2 + —Si system at E=8 keV and θ=43°. A statistical analysis of SEM-images with a size of 6.77×9 micron 2 was carried out by counting the number of waves in the 1.3 by 6.5 micron 2 frames oriented by a long side perpendicular to the wave's crests and each containing 50 waves. The number of the waves passing from one long edge of the frame to the other without abruptions and intersections (a quantity of good waves), the number of waves crossing one of the edges but not reaching the other edge (a quantity of the wave abruptions) and the number of waves intersecting inside the frame were counted. The results showed that a two-stage process of forming a N 2 + -[O 2 + —Si] wavelike nanostructure decreases the number of wave abruptions by 5.4 times, the wave intersections by 2.9 times, and increases the quantity of good waves by 2.4 times. Thus, a method for forming a wavelike nanostructure using a two-stage process with improved wave ordering was developed. The nanostructures produced by this method combine increased wave longitude as in O 2 + —Si system at a sputtering depth D m and planarity of the N 2 + —Si system.
[0061] In the N 2 + —Si system that does not possess a natural ordering (high coherency) property, the degree of coherency of a wavelike nanostructure can be increased by a preliminary mechanical processing of the silicon surface.
[0062] In one preferred embodiment, an oriented polishing (polishing the surface in one preferred direction) of the silicon surface with a GOI paste containing Cr 2 O 3 particles was used as a preliminary step before the formation of a wavelike nanostructure in the N 2 + —Si system. The N 2 + ion flux was oriented perpendicularly to the direction of movement of abrasive particles relative to the silicon surface. The results proved that the introduction of the preliminary oriented polishing step leads to a considerable increase in a degree of orientation of the nanostructure along the polishing direction. The parameters for forming the nanostructure (E=8 keV, θ=43°, D F =360 nm, λ=150 nm) are close to those used without polishing. Analogous results showing an improvement of the nanostructure orientation as a result of the preliminary polishing with a GOI paste were obtained for the layers of amorphous silicon. It has also been demonstrated that a variety of water based or alkaline slurries containing small particles (such as alumina, silica, or chromium oxide) can be used for preliminary polishing instead of a GOI paste. This class of slurry systems is already used in a different industrial polishing application of the wafers in semiconductor manufacturing.
[0063] An additional preferred embodiment relates to a novel device for forming highly coherent wavelike nanostructures. The principle of operation of this device is illustrated by FIGS. 4A-4C . FIG. 4A shows a block for forming a matrix of sheet beams. The block comprises a matrix of linear apertures 2 in a plasma electrode 3 , electrodes 4 for switching on and switching off the sheet beams and insulators 5 . A nanostructure 6 is formed upon the silicon wafer 10 with an ion beam 1 .
[0064] FIG. 4B shows a view from above a plasma electrode 3 (view A), with crystal 12 and arrays of nanolines 14 .
[0065] FIG. 4C shows a device for forming coherent wavelike nanostructures on the surface of a material comprising a block 11 for forming a matrix of sheet beams, magnets 15 , a plasma chamber 16 with a system of the nitrogen discharge and exhaustion (not shown on the drawing), testing cells 17 , a secondary electrode detector 18 , a precision stage 19 for a wafer 10 , a vacuum chamber 20 with a system of exhaust and introduction of the wafer into a chamber (not shown on the drawing), a silicon wafer 10 , and a computer with interface (not shown on the drawing).
[0066] The device operates as follows. A wafer 10 is installed at a precision stage 19 . A vacuum chamber is pumped to an operational pressure. Nitrogen is supplied through a discharge system into a plasma chamber for obtaining the nitrogen ion flux. A charge is ignited in a plasma chamber. The plasmas operational potential relative to the ground is approximately U=+5 keV, therefore, the chamber 16 should be properly electronically insulated from chamber 20 . A plasma electrode 3 has potential U+U 1 , electrodes 4 have potential U−U 1 when the beams are switch-on and potential U+U 1 when the beams are switched-off. The electrodes 4 are insulated from the electrode 3 by an insulator 5 . Potential U 1 is on the order of +100V. The movement of the precision stage 19 is controlled by a computer and interface and by the secondary electron signal detector from a test cell 17 . Velocity of the stage movement is decreased proportionately to the current of the secondary electron emission registered by a detector 18 from a test cell 17 . A production rate of 6 wafers per hour, when the wafer is 100% covered with nanolines, can be achieved under the following conditions: the density of ion current in plasma is 250 mA/cm 2 , the velocity of the wafer movement is 2.5 micron/s and the distance between the sheet beams is 1 mm.
[0067] The linear apertures 2 in the plasma electrode 3 are carried out along the rows with a period d being a whole number of times less than size S of the crystal 12 on the wafer 10 . This allows to completely cover the crystal with arrays of nanolines 14 while moving over a distance, which is S/d times less than crystal size. The plasma electrode is made of a highly alloyed silicon wafer of n-type conductivity and of about 20 micron thickness. A part of a block forming the matrix of linear beams 11 , containing electrodes 3 and 4 can be made using the planar silicon technology with the insulators 5 made from silicon nitride. The part 11 , facing the wafer 10 , can be covered with a layer of amorphous silicon or a low-conductivity carbon.
[0068] In all the previously disclosed embodiments, the ion flux falls obliquely upon the wafers. However, these are homogeneous ion fluxes. In case of a running sheet ion beam, as shown in FIG. 4A , an area of the sputtered surface 7 is inclined towards the ion flux direction. As it progresses along the silicon surface 10 , the beam 1 sputters silicon and leaves behind an ordered nanostructure 6 . The surface level with a nanostructure is lower than the level of the initial surface. The width of the obliquely sputtered area of the surface 7 is equal to the width of the beam 1 . Therefore, while the ion flux 1 falls normally upon the initial surface 10 , the process of forming a nanostructure 6 is carried out by tilt bombardment of the surface of the area being sputtered.
[0069] An additional study of the properties of the N 2 + —Si system lead to a conclusion that a preliminary directional polishing of the silicon surface in a direction of the wave crests of a wavelike structure formed thereupon considerably increases a degree of the pattern orientation, i.e. its coherency.
[0070] An example of a device for wafer polishing used in semi-conductor manufacturing is disclosed in the US Pat. Application No. 2002/0142704. This device comprises a wafer holder for a wafer rotation around its axis, a constantly running band held by a support in a place where the wafer surface contacts with the band, motors for enabling the wafer holder rotation and the band movement, devices for supplying a polishing mixture onto the band, and devices for supplying air through the system of apertures to enable the band support and even distribution of the wafer pressure on to the band. However, this device is not designed to be used for directional polishing.
[0071] An additional preferred embodiment is a device which is effective for implementation of the oriented polishing step. Devices for chemical-mechanical polishing are widely used for polishing wafers in semiconductor manufacturing and some contain a continuously miming belt (see for example an application for U.S. Patent Application Publication No. 2002/0142704). The primary purpose of these devices is to reduce the thickness of the substrate without providing an orientation to the polishing. A device for oriented polishing can be manufactured by implementing the following changes in a previously known design: eliminating rotation of the wafer holder around its axis and securing the holder in the necessary position relative to a direction of the running band. FIG. 5 shows a device for directional wafer polishing. It consists of a wafer holder 101 , shown in an inoperative position. The holder is used for wafer installation. In an operative position 102 , the holder presses the wafer 103 to a continuous band 104 , set in motion by rolls 105 . The wafer holder provides for a fixed position of the wafer 103 relative to a direction of the band 104 . A support 106 keeps the band 104 and the wafer holder in the operative position. The support has a system of apertures to let the compressed air flow through, thus providing for an even distribution of the pressure of the wafer on to the band. In addition, a polishing slurry is supplied onto the band ( FIG. 5 does not show a device for supplying slurry). The rolls 105 and a lower part of the band 104 can be submerged into a polishing slurry bath. A selection of an appropriate abrasive for the polishing slurry, (for example, silica or alumina are widely used for polishing in semiconductor manufacturing), may help to achieve maximum coherence of a wavelike nanostructure after a subsequent ion sputtering step.
[0072] The invention can be used for forming patterns on the surface of the silicon and the gallium arsenide with the lines width of 10 to 60 nm. It also can be used in for forming nanowires for nanoelectronics and optoelectronics devices.
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The method for forming wavelike coherent nanostructures by irradiating a surface of a material by a homogeneous flow of ions is disclosed. The rate of coherency is increased by applying preliminary preprocessing steps.
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BACKGROUND OF THE INVENTION
The present invention relates to an apparatus of forming an electrode with gas assist deposition using a charged particle beam and a method of using the same.
In recent years, a technology of fabricating an integrated circuit is remarkable, and an integration degree is significantly promoted. Further, in order to realize more highly integrated formation, basic researches on molecule elements and single electron elements have been promoted.
In developing the molecule element, in order to grasp properties of the molecule, it is necessary to measure a conduction property thereof. Hence, electrodes having a gap of a molecule size (about 1 nm) therebetween are fabricated, a molecule is interposed in the gap, and various properties are measured.
As a method of fabricating a narrow gap, for example, there is a method of using a sputtering etching technology of a focused ion beam. According thereto, an electric wire comprising a conductive substance formed on an insulating film is etched by using a focused ion beam and an argon ion beam to form electrodes having a width of a gap of 5 nm therebetween (refer to Nonpatent Reference 1).
[Nonpatent Reference 1] “Fabrication of nano-gap electrodes for measuring electrical properties of organic molecules using a focused ion beam”, Solid Thin Film 438-439 (2003) 374-377
However, according to the method of fabricating a narrow gap by using a sputtering etching of a focused ion beam, there poses a problem that a lower limit of a width of the gap formed is rectified by a beam diameter of the focused ion beam.
It is a problem of the invention to resolve the above-described problem to form a pair of electrodes having an extremely narrow gap width equal to or smaller than a beam diameter of a focused ion beam.
SUMMARY OF THE INVENTION
In order to resolve the above-described problem, a charged particle beam apparatus according to the invention is constituted by a charged particle source, a focusing lens system for focusing a charged particle beam drawn out from the charged particle source, a blanking electrode for making the focused charged particle beam ON/OFF on a sample, a deflection electrode for deflecting to scan the focused charged particle beam, a movable sample stage mounted with the sample irradiated with the focused charged particle beam, a gas gun for locally blowing a gas to a position of irradiating the focused charged particle beam on a surface of the sample, a secondary charged particle detector for detecting a secondary charged particle generated by irradiating the focused charged particle beam to the sample, two pieces of probers brought into contact with two points on the surface of the sample, a voltage source for applying a constant voltage between the two points with which the probers are brought into contact, and an ammeter for measuring a current flowing between the two points.
As operation of principal means having the above-described constitution, the electrodes having the extremely narrow gap therebetween can be formed without depending on a size of a beam diameter of the focused charged particle beam by forming a deposition film between the two points of the surface of the sample with which the probers are brought into contact by scanning to irradiate the focused charged particle beam while blowing a gas to the surface of the sample from the gas gun, applying the constant voltage between the two points with which the probers are brought into contact, measuring the current flowing between the two points, detecting that the current value becomes larger than a predetermined value, and making the focused charged particle beam irradiated to the surface of the sample OFF by the blanking electrode based on a signal thereof.
As described above, according to the apparatus and the method of the invention, when the electrodes are formed by CVD using the charged particle beam, the conductive film is formed to narrow the interval between the electrodes, the interval is controlled by measuring the current flowing between the electrodes at this occasion and therefore, the electrodes having the gap therebetween equal to or smaller than 1 nm can be fabricated for evaluating electric properties of an extremely small substance of a molecule, a gene or the like. Thereby, researches and industrialization of a molecule element or biotechnology are promoted.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a constitution example of an apparatus according to the invention.
FIGS. 2A-2C show an example of a method of fabricating a sample used in the invention.
FIG. 3 shows an example of a method of fabricating an electrode according to the invention.
FIGS. 4A-4B show examples of scanning an ion beam in fabricating the electrode according to the invention.
FIGS. 5A-5B show a sectional shape of a sample used in the invention.
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of the invention will be explained in details in reference to the drawings as follows.
FIG. 1 shows an example of a focused ion beam apparatus according to the invention.
A focused ion beam lens-barrel mainly comprises an ion source portion 11 , a condenser lens 12 , a blanking electrode 13 , a movable diaphragm 14 , a deflection electrode 15 , an object lens 16 , and an optical axis correcting electrode, an astigmatism correcting electrode and the like, not illustrated.
It is general to use liquid metal gallium for the ion source. Liquid metal gallium stored in a holding portion is supplied to an emitter in a needle-like shape by a surface tension. Further, a gallium reservoir, the emitter are made to be able to be heated by a filament. The emitter portion is applied with an electric field by a single or a plurality of electrodes, and gallium stored in the emitter portion is drawn out as an ion beam. Since the emitter is applied with a high voltage of about +30 kV relative to the ground potential, the ion beam is accelerated by the electric field.
The ion beam is focused by the condenser lens 12 , and focused on a surface of a sample 20 by the object lens 16 . The blanking electrode 13 is made to be able to generate a large electric field between two sheets of electrodes opposed to each other. When the respective electrodes are applied with the same potential, normally, the ground potential, the ion beam reaches the sample 20 . However, when a large electric field is generated by applying signals having a large potential difference therebetween to the respective electrodes of the blanking electrode 13 , the ion beam is considerably deflected to impinge on a blocking member of the movable diaphragm 14 or the like and the ion beam does not reach the surface of the sample 20 .
The deflection electrode 15 is constituted by at least two sets of electrodes comprising two electrodes opposed to each other, and a trajectory of the ion beam is two-dimensionally controlled by electric fields generated between the respective electrodes.
Respective power sources for generating signals applied to the respective electrodes, the movable diaphragm are controlled by an apparatus control computer.
Further, a detector 17 detects secondary charge particles generated when the ion beam is irradiated to the surface of the sample 20 to convert to an electric signal. An output signal thereof is inputted to the apparatus control computer, and by storing the output signal along with a position of irradiating the ion beam, the surface of the sample 20 can be observed.
A sample stage 19 is movable at least in three axes of horizontal X, Y and vertical Z. The horizontal direction X-Y axes are used for observing the sample and determining a machining position. Further, the Z axis is used such that a height of the surface of the sample is always disposed at a position optimum for irradiating the focused ion beam. Otherwise, an inclining T axis, a rotating R axis or the like can also be provided.
A thin film is fabricated by a beam assisted CVD method by a compound vapor blowing apparatus 18 mounted to the focused ion beam apparatus. In the beam assisted CVD method, there is used compound vapor including a material of the thin film deposited on the surface of the sample 20 . The compound vapor is blown to the surface of the sample 20 by the compound vapor blowing apparatus 18 . The compound vapor blown to the surface of the sample 20 is adsorbed by the surface of the sample 20 . When the focused ion beam is irradiated under the state, the compound vapor is decomposed by kinetic energy thereof or energy of second electrons generated in accordance with irradiation of the focused ion beam. A decomposed gas component is exhausted to outside of a sample chamber 22 by a vacuum pump 21 , and a solid component thereof remains on the surface of the sample by constituting the thin film. At this occasion, the focused ion beam executes also sputter etching simultaneously with deposition. Therefore, it is necessary to control an amount of introducing the compound vapor and an amount of irradiating the focused ion beam such that a rate of fabricating the thin film by deposition becomes higher than a rate of machining by sputter etching.
Further, although a single one of the compound vapor blowing apparatus 18 is illustrated in the drawing, a plurality of compound vapor blowing apparatus may be used such that gasses can properly be used in accordance with objects.
The sample chamber 22 and the focused ion beam lens-barrel are vacuumed by the vacuum pump 21 . Further, although not illustrated, there can also be provided a load/lock chamber for putting in and out a sample to and from the sample chamber without exposing the sample chamber to the atmosphere.
Further, there is mounted a manipulator 23 capable of being brought into contact with two portions of the surface of the sample 20 . A voltage source 24 and an ammeter 25 are connected between two electrodes, and a resistance between two points is made to be able to be measured. When a value of the ammeter 25 becomes larger than a predetermined value, an input signal to the blanking electrode 13 is controlled based on the signal to thereby prevent the focused ion beam from reaching the surface of the sample 20 .
Successively, the sample will be explained in reference to FIGS. 2A-2C .
As a material of a board, a silicon plate having face orientation of <100> is used. However, the face orientation is not particularly limited to <100>. A groove is formed in the silicon board 31 by using an MEMS technology. As shown by FIG. 2A , for example, a silicon oxide film or a silicon nitride film is formed as a mask member 32 to cover the silicon board 31 , further, a window 33 is formed by using a photolithography technology.
Further, as shown by FIG. 2B , a membrane 34 is formed by anisotropic etching based on the face orientation by dipping the board into an alkali solution of potassium hydroxide solution or the like. At this occasion, although a thickness of the membrane is preferably as thin as possible, the thickness is preferably, for example, equal to or smaller than several micrometers.
Successively, as shown by FIG. 2C , a through hole 35 is formed at the membrane portion by using the focused ion beam. The through hole is preferably a long hole having a width equal to or smaller than 1 micrometer and a length of several micrometers. Further, a total of the board is covered with an insulating film and electrodes 36 are formed by interposing the through hole.
The electrodes having a narrow gap are formed by using the sample.
Although in FIGS. 2A-2C , a penetrated hole is used at the groove, a hole which is not penetrated can also be used. In this case, as shown by FIGS. 5A-5B , an inner wall of the hole becomes wider than an inlet thereof and in fabricating the electrodes, the inner wall is prevented from being formed with a deposition film.
The sample 20 is mounted to the focused ion beam apparatus shown in FIG. 1 .
Needles of the manipulator 23 are brought into contact with the electrodes 36 of the sample. Under the state, as shown by FIG. 3 , a machining frame 37 is set to ride over the through hole 35 and connect the electrodes 36 , and the focused ion beam is irradiated simultaneously with blowing a gas of hexacarbonyltungsten constituting a raw material of tungsten deposition to the surface of the sample 20 by using the gas introducing apparatus 18 . At this occasion, the focused ion beam may be scanned in one direction in the machining frame as shown by FIG. 4A , or may be scanned while reciprocating in the machining frame as shown by FIG. 4B .
A tungsten film is formed to ride over the through hole by scanning to irradiate the focused ion beam. The tungsten film is formed from both sides of the through hole. At this occasion, a potential difference is provided to the respective electrodes 36 by the voltage source 25 . Further, when the gap between the electrodes becomes a nanometer order in accordance with growth of the tungsten film, a tunnel current is made to flow. For example, when the focused ion beam is prevented from reaching the surface of the sample 20 by controlling a control signal of the blanking electrode 13 when the potential difference becomes 2 mV and the tunnel current becomes 2 nA, the gap between the electrodes can be controlled to be equal to or smaller than 1 nm.
The tungsten film is formed by irradiating the focused ion beam while monitoring the ammeter by control means 41 , and when the tunnel current becomes 2 nA, the focused ion beam is stopped to irradiate by the control signal from the controlling means 41 .
Further, an arbitrary gap can reproducibly fabricated by controlling the applied voltage and the control current value.
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A focused ion beam apparatus having two pieces of probers brought into contact with two points of a surface of a sample, a voltage source for applying a constant voltage between the two points with which the probers are brought into contact, and an ammeter for measuring a current flowing between the two points, in which a conductive film is formed to narrow a gap thereof between the two points by operating a deflection electrode and a gas gun and the current flowing between the two points is monitored, and when the current becomes a predetermined value, a focused charged particle beam irradiated to the surface of the sample is made OFF by the blanking electrode.
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PRIORITY CLAIM
[0001] This application is a continuation of pending International Application No. PCT/EP2013/065806 filed on Jul. 26, 2013, which designates the United States and claims priority from European Application No. 12178841.8 filed on Aug. 1, 2012, both of which are incorporated herein by reference in their entireties.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to a LED (Light Emitting Diode) light unit and specifically to a housing for a LED light unit.
[0004] 2. Description of Relevant Art
[0005] In LED light units, a plurality of LEDs may be mounted to a printed circuit board. This circuit board is often covered by a cover which may also act as a lens for guiding light to the outside of the light unit.
[0006] The European patent application publication EP 1 821 030 A1 discloses a LED light unit, where LEDs are mounted to a heat sink. Furthermore, the LEDs are embedded by a cover element and a housing to form an integral part which is water-tight.
[0007] US 2012/0188788 A1 discloses a LED-light assembly. The LED light assembly has a housing with a transparent front cover being screwed to a back cover. A sealant may be inserted in an annular through between the front cover and the back covering after the screws have been fastened. At the rear side of the back cover are fins rendering the back cover into a heat sink. The housing accommodates a printed circuit board, the latter supporting LEDs.
[0008] A disadvantage of these LED light units is their respective complex and thus expensive design. With respect to EP 1 821 030 A1 the cover element embeds the LEDs which may affect optical characteristics.
SUMMARY OF THE INVENTION
[0009] The problem to be solved by the invention is to design a sealed LED light module which is sealed against dust, dirt, water and/or humidity, which has excellent long term stability and which can be manufactured by an automated process in large volumes at low costs.
[0010] The problem is solved by an embodiment with a base plate supporting at least one LED and/or further electronic components which may be required for driving/controlling the at least one LED. The base plate may be a printed circuit board. It may also comprise a printed circuit board. Preferably, the base plate is a heat conducting plate which may be made of a metal, like aluminum, and which further preferably comprises laminated electrically isolating and current-conducting structures. Preferably, the base plate is at least essential planar, as expressed in the word “plate”. The base plate is positioned on a cover through which light may be emitted from the at least one LED to the outside of the light module. The cover may have at least one lens for guiding and/or directing the light emitted by the at least one LED. Preferably, the cover is made of a clear and/or transparent and/or semitransparent material, preferably a plastic material. The cover preferably has at least one base plate support. Such a base plate support may be a strut or a protrusion from the inner surface of the cover.
[0011] Preferably, the base plate support is a bar or a barrier, preferably surrounding at least a part of the base plate. It is further preferred, if the cover has at least one sidewall which forms a trench together with the at least one base plate support. Most preferably this trench is surrounding the baseplate and/or the cover.
[0012] At least one edge of the base plate, preferably all edges of an e.g. rectangular base plate are held within a sealing. The sealing seals a slit between the base plate and the cover and preferably fixes the base plate to the cover. In other words, the mechanical connection of the base and the cover is provided by said sealing. The base plate and the cover are so to speak attached to each other by said sealing. The sealing preferably is the only connecting means between the base plate and the cover. Accordingly there is no screw, rivet or clip in between or surrounding the base plate and the cover. The sealing may be a mold or cast or glue. It preferably is at least a semi-elastic plastic material. Preferably, the sealing is contained within the trench defined by at least one base plate support and a sidewall of the cover. Preferably the sealing is processed by low pressure injection molding. It may be a hot-melt which may be based on polyamide.
[0013] Preferably, the base plate and the cover form a hermetically sealed unit which preferably is water tight and which preferably cannot be opened and need not to be opened for service. This prevents the penetration of dust and debris into the optical system which also extends lifetime and improves quality. Most preferably the base plate has no further holes or openings except holes which are sealed and ventilation holes. Due to the elastic properties of the seal, different thermal expansion of the base plate and the cover may be equalized, therefore preventing cracks or even bending of the unit at extreme temperatures.
[0014] To easy assembly, the cover may be placed with its inside up on a flat surface. Then, the base plate may be placed on the cover. The base plate is preferably held at a correct distance to the cover by the at least one base plate support. There may be further notches or holes in the base plate, interacting with protrusions in the base plate support to ensure a correct location of the base plate on the cover. After placement of the base plate on the cover, sealing is filled and/or molded to the edges of the base plate, preferably filling the at least one trench. Here, the at least one trench may act as a molding form which holds the sealing when it is in a semi-liquid or liquid condition.
[0015] In a further preferred embodiment, there is at least one sealing sidewall located between the cover and the base plate for sealing the inner space between the cover and the base plate containing the at least one LED against the outer environment. The sealing sidewall may enclose an area within which a further hole or opening may be provided in the base plate and/or the cover. Such an opening may be used for contacting an electrical connector and/or for inserting a screw. The sealing sidewall may be extending from the cover and may be of the same material as the cover. In an alternative embodiment, the sidewall may be of a material which is the same as the sealing. There may be any combination of the sealings disclosed herein with a connector. Generally such a sealed opening prevents any debris or contamination from the connector to penetrate into the optical system.
[0016] In a further embodiment, there may be an upper sealing which further seals parts of the outer side of the base plate. This upper sealing preferably is of the same material as the first sealing. To simplify molding, it may be connected by at least one bar to the first sealing. The upper sealing may also extend from the outside of the base plate through the inner space between the base plate and the cover to the inner side of the cover, therefore also sealing the inner space against the environment.
[0017] In a further embodiment, there are cut-outs and/or protrusions at the edges of the base plate.
[0018] In another embodiment, the edges of the base plate are bent to further in-crease mechanical strength of the connection to the sealing and to increase the mechanical stability of the mechanical contact between the base plate and the sealing.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] In the following, the invention will be described by way of example, without limitation of the general inventive concept, on examples of embodiment and with reference to the drawings.
[0020] FIG. 1 shows a sectional view of the sealed LED light module.
[0021] FIG. 2 shows a sectional view with sealing sidewalls extending from the cover to the surface of the base plate.
[0022] FIG. 3 shows a different embodiment of the sealing sidewall.
[0023] FIG. 4 shows an embodiment providing a cut-out in the cover.
[0024] FIG. 5 shows an embodiment with an upper sealing to seal the outer side of the base plate.
[0025] FIG. 6 shows a further sealing protruding to the cover.
[0026] FIG. 7 shows a modified upper sealing protruding to the cover.
[0027] FIG. 8 shows an embodiment with a base plate having bent sidewalls is dis-closed.
[0028] FIG. 9 shows an embodiment of bent sidewalls of the base plate.
[0029] FIG. 10 shows a top view of the light module.
[0030] While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the drawings and detailed description thereto are not intended to limit the invention to the particular form disclosed, but on the contrary, the intention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the present invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0031] In FIG. 1 , a sectional view of a first embodiment of the invention is shown. A cover 100 holds a base plate 200 , whereas fixing and sealing between the cover and the base plate is done by a sealing 300 . The base plate has an outer side (on top in the figure) and an inner side directed towards the cover, the inner side holds at least one LED (Light Emitting
[0032] Diode) 210 , 220 , and optionally further electronic components. The LEDs radiate light from the bottom side through the cover 100 to the outside of the light module. For better holding of the base plate, preferably at least one base plate support 130 , 131 are provided within the cover. They are preferably protruding from the surface of the cover. Furthermore, it is preferred, if the cover has at least one sidewall 110 , 111 , which preferably forms at least one trench 141 which may be filled with sealing 300 which preferably seals the edges 206 , 207 of the base plate 200 . Between the base plate 200 and the cover 100 , there is a sealed inner space 140 . Furthermore, there is at least one sealing sidewall 150 , 151 between the cover 100 and the base plate 200 . This at least one sealing sidewall encloses a section of the base plate which may contain an opening 230 , through which a connecting plate 260 may penetrate to enter into electric contact with at least one electrical connector ( 240 , 250 ). By this way, electrical connection may be made from the LEDs at the base plate to an external power supply. In combination with an opening in the cover 100 , which may be similar to opening 180 from FIG. 4 , but with shortened inner walls, to allow access to the base plate 200 , a connector may be inserted from the front side of the cover. This may allow external access e.g. for diagnosis or control like dimming of the lamp and/or the power supply. The connector may also be extending from the power supply though the base plate to be accessed from the front side of the cover. It is further preferred to have guiding elements for the connector at least in one of the cover, base plate or inner walls. Preferably these guiding elements allow insertion of the connector from at least one side, preferably from both sides.
[0033] In FIG. 2 , a further embodiment is disclosed. Herein, the opening in the base plate 230 is larger and may be used for a different purpose than inserting a connecting plate as disclosed before. In this embodiment, the sealing sidewalls preferably protrude from the cover 100 into the direction of the base plate 200 and end at the inner side of the base plate 200 , which is bearing the at least one LED. It preferably comprises the same material as the cover 100 .
[0034] In FIG. 3 , a different embodiment of sealing sidewalls 150 , 151 is disclosed. Here, the sealing sidewalls 150 , 151 protrude from the cover 100 to the outside of the base plate 200 , therefore providing a better sealing of the base plate.
[0035] In FIG. 4 , a further embodiment is shown which provides an opening 180 in the cover. For this purpose, the sealing sidewalls 150 , 151 extend from the cover 100 throughout the base plate 200 . Contact of the sealing sidewalls may also be done as disclosed in FIG. 2 . Such a cut-out in the cover may be used for gaining access to an electrical contact or to a screw.
[0036] In FIG. 5 , a further embodiment is disclosed having an upper sealing 190 to seal an area at the rear side of the base plate 200 . To simplify molding and to have a connection between the upper sealing which preferably is made of the same material as the sealing 300 , at least one bar 191 may be provided. This kind of sealing may be combined with any other kind of sealing sidewalls disclosed before.
[0037] In FIG. 6 , a further sealing is disclosed which protrudes through the cover 100 and therefore seals or encapsulates the whole inner space.
[0038] In FIG. 7 , a modified upper sealing is disclosed which protrudes through the cover 100 and therefore seals or encapsulates the whole inner space.
[0039] In FIG. 8 , a modified embodiment is disclosed. Herein, the base plate 200 has bent sidewalls 201 . These bent sidewalls further increase mechanical stability and stiffness of the base plate. They further increase the mechanical retention force of the base plate within the sealing 300 and therefore within the cover 100 , further increasing mechanical stability of the sealed LED light module. It is obvious that this specific embodiment may be combined with all other embodiments shown herein.
[0040] In FIG. 9 , a top view of a base plate 200 is shown. Herein, there are bars 202 connecting the bent sidewall 201 to the base plate 200 . Between the bars, there are cut-outs 203 . The sealing 300 penetrates through the cut-outs and therefore increases the retention of the base plate 200 within the sealing 300 , further increasing mechanical stability. It is obvious that this specific embodiment may be combined with all other embodiments shown herein.
[0041] In FIG. 10 , a top view of the light module is shown. The base plate 200 is placed on cover 100 and is sealed by sealing 300 . Here, the second sidewall 111 and a third sidewall 112 can be seen. On top of the base plate 200 , there is an upper sealing 190 connected by a bar 191 to the sealing 300 . There may be a vent hole 205 in the base plate allowing for equalization of air pressure. This hole may have a filter, a membrane or other means for directing or selecting flow of vent exchange of gases, preferably preventing the intrusion of liquids or humidity. First protrusions 172 and second protrusions 174 may be provided for aligning the light module within a lamp case. Furthermore, it is preferred, if at least one clamp 170 is provided to fix the light module within a lamp case.
[0042] It will be appreciated to those skilled in the art having the benefit of this disclosure that this invention is believed to provide a sealed LED light module. Further modifications and alternative embodiments of various aspects of the invention will be apparent to those skilled in the art in view of this description. Accordingly, this description is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the general manner of carrying out the invention. It is to be understood that the forms of the invention shown and described herein are to be taken as the presently preferred embodiments. Elements and materials may be substituted for those illustrated and described herein, parts and processes may be reversed, and certain features of the invention may be utilized independently, all as would be apparent to one skilled in the art after having the benefit of this description of the invention. Changes may be made in the elements described herein without departing from the spirit and scope of the invention as described in the following claims.
LIST OF REFERENCE NUMERALS
[0000]
100 cover
110 first sidewall
111 second sidewall
112 third sidewall
130 first base plate support
131 second base plate support
140 inner space
141 trench
150 first sealing sidewall
151 second sealing sidewall
170 clamp
172 first protrusions
174 second protrusions
180 opening in cover
190 upper sealing
191 bar
200 base plate
201 bent sidewall
202 bar
203 cutout
205 vent hole
206 , 207 edges of the base plate
210 , 220 LEDs/components
230 opening in base plate
240 first connector
250 second connector
260 connecting plate
300 sealing
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A sealed LED light module comprises a base plate, having at least one LED, and a cover providing a base plate support. The base plate is located on the cover to define an inner space which is sealed against the environment. For sealing the cover has at least one sidewall, which defines a trench together with at least one base plate support, and the trench holds a seal which interacts with at least one edge of the base plate and the surface of the trench to seal the inner space against the environment.
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FIELD
The present disclosure relates generally to statistical data learning.
BACKGROUND
Telematics units within vehicles provide subscribers with connectivity to a telematics service provider (TSP). The TSP provides subscribers with an array of services ranging from emergency call handling and stolen vehicle recovery to diagnostics monitoring and turn-by-turn navigation. Telematics units are often provisioned and activated at a point of sale when a subscriber purchases a telematics-equipped vehicle. Upon activation, the telematics unit can be utilized to provide a subscriber with the telematics services.
A convenient way for a user to control a telematics unit while operating a vehicle is through speech. In order to provide accurate responses to vocal commands, it is advantageous for a telematics unit to have access to a well-developed language model. However, conventional language modeling requires complex, time-consuming, and/or unsecure procedures that are difficult or costly to implement and that may expose users' private information.
The inventors have created the above body of information merely for the convenience of the reader; the foregoing is a discussion of problems discovered and/or appreciated by the inventors, and is not an attempt to review or catalog the prior art.
SUMMARY
In an implementation, the present invention provides a computer-implemented method for statistical data learning under privacy constraints. The method includes: receiving, by a processor, a plurality of pieces of statistical information relating to a statistical object, wherein each piece of statistical information includes an uncertainty variable, the uncertainty variable being a value determined from a function having a predetermined mean; and aggregating, by the processor, the plurality of pieces of statistical information so as to provide an estimation of the statistical object, wherein the number of pieces of statistical information aggregated is proportional to the reliability of the estimation of the statistical object.
In a further implementation, the present invention is implemented as computer-executable instructions stored on a tangible, non-transitory computer-readable medium.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
While the appended claims set forth the features of the present invention with particularity, the invention, together with its objects and advantages, may be best understood from the following detailed description taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of an operating environment for a mobile vehicle communication system usable in implementations of the described principles;
FIG. 2 is a diagram illustrating processes for updating a language model in accordance with an implementation of the described principles;
FIG. 3 is a flowchart illustrating a process for maintaining users' privacy by adding an uncertainty value to frequency or probability data in accordance with an implementation of the described principles;
FIGS. 4-6 are graphs illustrating examples of probability density functions associated with transmitted word or combination probability including added Gaussian error.
DESCRIPTION
Before discussing the details of the invention and the environment wherein the invention may be used, a brief overview is given to guide the reader. In general terms, not intended to limit the claims, implementations of the present invention are directed towards cost-effectively constructing a reliable language model in a short amount of time based on statistics collected from many users without jeopardizing any individual user's privacy. These exemplary implementations are discussed within the context of language modeling for vehicles equipped with telematics units. However, it will be appreciated that the principles described herein are not limited to language modeling or telematics units, and may be applied to other models (e.g., with respect to vehicle parameters) and contexts as well (e.g., personal mobile devices such as cellular phones).
An exemplary computing and network communications environment is described hereinafter, it will be appreciated that the described environment is an example, and does not imply any limitation regarding the use of other environments to practice the invention. With reference to FIG. 1 there is shown an example of a communication system 100 that may be used with the present method and system and generally includes a vehicle 102 , a mobile wireless network system 104 , a land network 106 and a communications center 108 . It should be appreciated that the overall architecture, setup and operation, as well as the individual components of the communication system 100 is generally known in the art. In accordance with an illustrative example, the communication center 108 includes a GNSS control center 109 incorporating functional components facilitating over-the-air configuration of GNSS receivers integrated with/within telematics units such as a telematics unit 114 . Thus, the following paragraphs provide a brief overview of an exemplary communication system 100 . However, other systems are contemplated that are capable of incorporating the described GNSS receiver and GNSS control center functionality described herein.
The vehicle 102 is, for example, a motorcycle, a car, a truck, a recreational vehicle (RV), a boat, a plane, etc. The vehicle 102 is equipped with suitable hardware and software that configures/adapts the vehicle 102 to facilitate communications with the communications center 108 via mobile wireless communications. The vehicle 102 includes hardware 110 such as, for example, the telematics unit 114 , a microphone 116 , a speaker 118 and buttons and/or controls 120 integrated with the telematics unit 114 .
The telematics unit 114 is communicatively coupled, via a hard wire connection and/or a wireless connection, to a vehicle bus 122 for supporting communications between electronic components within the vehicle 102 . Examples of suitable network technologies for implementing the vehicle bus 122 in-vehicle network include a controller area network (CAN), a media oriented system transfer (MOST), a local interconnection network (LIN), an Ethernet, and other appropriate connections such as those that conform with known ISO, SAE, and IEEE standards and specifications.
The telematics unit 114 provides a variety of services through communications with the communications center 108 . The telematics unit 114 includes an electronic processor 128 , electronic memory 130 , a mobile wireless component 124 including a mobile wireless chipset, a dual function antenna 126 (both GNSS and mobile wireless signal), and a GNSS component 132 including a GNSS chipset. In one example, the mobile wireless component 124 comprises an electronic memory storing a computer program and/or set of computer-executable instruction sets/routines that are transferred to, and executed by, the processing device 128 . The mobile wireless component 124 constitutes a network access device (NAD) component of the telematics unit 114 . The telematics unit 114 may also communicate with other telematics-equipped vehicles using the aforementioned communications components.
The telematics unit 114 provides, for users, an extensive/extensible set of services. Examples of such services include: GNSS-based mapping/location identification, turn-by-turn directions and other navigation-related services provided in conjunction with the GNSS component 132 , and airbag deployment notification and other emergency or roadside assistance-related services provided in connection with various crash and or collision sensor interface modules 156 and crash sensors 158 located throughout the vehicle.
GNSS navigation services are, for example, implemented based on the geographic position information of the vehicle provided by the GNSS component 132 . A user of the telematics unit 114 enters a destination, for example, using inputs associated with the GNSS component 132 , and a route to a destination may be calculated based on the destination address and a current position of the vehicle determined at approximately the time of route calculation. Turn-by-turn (TBT) directions may further be provided on a display screen corresponding to the GNSS component and/or through vocal directions provided through a vehicle audio component 154 . It will be appreciated that the calculation-related processing may occur at the telematics unit or may occur at a communications center 108 .
The telematics unit 114 also supports information-related services whereby music, Web pages, movies, television programs, video games and/or other content is downloaded by an infotainment center 136 operatively connected to the telematics unit 114 via the vehicle bus 122 and an audio bus 112 . In one example, downloaded content is stored for current or later playback.
The above-listed services are by no means an exhaustive list of the current and potential capabilities of the telematics unit 114 , as should be appreciated by those skilled in the art. The above examples are merely a small subset of the services that the telematics unit 114 is capable of offering to users. Moreover, the telematics unit 114 includes a number of known components in addition to those listed above that have been excluded since they are not necessary to understanding the functionality discussed herein below.
Vehicle communications use radio transmissions to establish a communications channel with the mobile wireless network system 104 so that both voice and data signals can be sent and received via the communications channel. The mobile wireless component 124 enables both voice and data communications via the mobile wireless network system 104 . The mobile wireless component 124 applies encoding and/or modulation functions to convert voice and/or digital data into a signal transmitted via the dual function antenna 126 . Any suitable encoding or modulation technique that provides an acceptable data rate and bit error can be used. The dual function antenna 126 handles signals for both the mobile wireless component 124 and the GNSS component.
The microphone 116 provides the driver or other vehicle occupant with a means for inputting verbal or other auditory commands, and can be equipped with an embedded voice processing unit utilizing a human/machine interface (HMI) technology known in the art. The speaker 118 provides verbal output to the vehicle occupants and can be either a stand-alone speaker specifically dedicated for use with the telematics unit 114 or can be part of an audio component 154 . In either case, the microphone 116 and the speaker 118 enable the hardware 110 and the communications center 108 to communicate with occupants of the vehicle 102 through audible speech.
The hardware 110 also includes the buttons and/or controls 120 for enabling a vehicle occupant to activate or engage one or more components of the hardware 110 within the vehicle 102 . For example, one of the buttons and/or controls 120 can be an electronic push button used to initiate voice communication with the communications center 108 (whether it be live advisors 148 or an automated call response system). In another example, one of the buttons and/or controls 120 initiates/activates emergency services supported/facilitated by the telematics unit 114 .
The audio component 154 is operatively connected to the vehicle bus 122 and the audio bus 112 . The audio component 154 receives analog information via the audio bus, and renders the received analog information as sound. The audio component 154 receives digital information via the vehicle bus 122 . The audio component 154 provides AM and FM radio, CD, DVD, and multimedia functionality independent of the infotainment center 136 . The audio component 154 may contain a speaker system 155 , or may utilize the speaker 118 via arbitration on the vehicle bus 122 and/or the audio bus 112 .
The vehicle crash and/or collision detection sensor interface 156 is operatively connected to the vehicle bus 122 . The crash sensors 158 provide information to the telematics unit 114 via the crash and/or collision detection sensor interface 156 regarding the severity of a vehicle collision, such as the angle of impact and the amount of force sustained.
A set of vehicle sensors 162 , connected to various ones of a set of sensor interface modules 134 are operatively connected to the vehicle bus 122 . Examples of the vehicle sensors 162 include but are not limited to gyroscopes, accelerometers, magnetometers, emission detection and/or control sensors, and the like. Examples of the sensor interface modules 134 include ones for power train control, climate control, and body control.
The mobile wireless network system 104 is, for example, a cellular telephone network system or any other suitable wireless system that transmits signals between mobile wireless devices, such as the telematics unit 114 of the vehicle 102 , and land networks, such as the land network 106 . In the illustrative example, the mobile wireless network system 104 includes a set of cell towers 138 , as well as base stations and/or mobile switching centers (MCSs) 140 , as well as other networking components facilitating/supporting communications between the mobile wireless network system 104 with the land network 106 . For example, the MSC 140 includes a remote data server.
As appreciated by those skilled in the art, the mobile wireless network system includes various cell tower/base station/MSC arrangements. For example, a base station and a cell tower could be co-located at the same site or they could be remotely located, and a single base station could be coupled to various cell towers or various base stations could be coupled with a single MSC, to name but a few of the possible arrangements.
Land network 106 can be, for example, a conventional land-based telecommunications network connected to one or more landline end node devices (e.g., telephones) and connects the mobile wireless network system 104 to the communications center 108 . For example, land network 106 includes a public switched telephone network (PSTN) and/or an Internet protocol (IP) network, as is appreciated by those skilled in the art. Of course, one or more segments of the land network 106 can be implemented in the form of a standard wired network, a fiber or other optical network, a cable network, other wireless networks such as wireless local networks (WLANs) or networks providing broadband wireless access (BWA), or any combination thereof.
The communications center 108 is configured to provide a variety of back-end services and application functionality to the hardware 110 . The communications center 108 includes, by way of example, network switches 142 , servers 144 , databases 146 , live advisors 148 , as well as a variety of other telecommunications equipment 150 (including moderns) and computer/communications equipment known to those skilled in the art. These various call center components are, for example, coupled to one another via a network link 152 (e.g., a physical local area network bus and/or a wireless local network, etc.). Switch 142 , which can be a private branch exchange (PBX) switch, routes incoming signals so that voice transmissions are, in general, sent to either the live advisors 148 or an automated response system, and data transmissions are passed on to a modem or other component of the telecommunications equipment 150 for processing (e.g., demodulation and further signal processing).
The telecommunications equipment 150 includes, for example, an encoder, and can be communicatively connected to various devices such as the servers 144 and the databases 146 . For example, the databases 146 comprise computer hardware and stored programs configured to store subscriber profile records, subscriber behavioral patterns, and other pertinent subscriber information. Although the illustrated example has been described as it would be used in conjunction with a manned version of the communications center 108 , it will be appreciated that the communications center 108 can be any of a variety of suitable central or remote facilities, which are manned/unmanned and mobile/fixed facilities, to or from which it is desirable to exchange voice and data.
It will be appreciated by those of skill in the art that the execution of the various machine-implemented processes and steps described herein may occur via the computerized execution of computer-executable instructions stored on a tangible computer-readable medium. e.g., RAM, ROM, PROM, volatile, nonvolatile, or other electronic memory mechanism. Thus, for example, the operations performed by the telematics unit may be carried out according to stored instructions or applications installed on the telematics unit, and operations performed at the call center may be carried out according to stored instructions or applications installed at the call center.
With further reference to the architecture of FIG. 1 , and turning more specifically to FIG. 2 , processes 210 , 220 , and 230 are depicted for updating the language model of a telematics system. In process 210 depicted by FIG. 2 , a host user of a telematics unit 201 communicates via the telematics unit for example, using a vehicle spoken commands interface or making a call through the telematics unit. During this communication when the user uses a word or combination of words 211 , the language model is updated 212 based on the word's or combination of words frequency or probability of use over the course of the communication. For example, the initial probability for word w may be stored by the language model as P(w). When the user uses word w at a rate corresponding to a probability R(w) in a new communication, the language model is adjusted to factor in the new probability with the old based on the length of the new communication in comparison to the length of all prior communications. After factoring in the new probability R(w) with the old probability P(w) accordingly, the language model updates the probability of word w from P(w) to P′ (w). While the present example describes the language model in terms of probability, it will be appreciated that the language model may also be described in terms of frequency of word use or other similar parameters.
In addition to updating the language model used on a user communication from the user, process 220 depicted in FIG. 2 shows that a telematic unit's language model can be updated by querying other telematics units 202 in a distributed system (e.g., a system where language model data is aggregated through numerous encounters of telematics units with other telematics units). The telematics unit 201 queries other telematics units 202 of other vehicles at stage 221 , for example, when the telematics unit 201 detects that another telematics unit 202 is within range of the telematics unit 201 (e.g., within range of being able to communicate over short-range wireless protocols). The query sent from one telematics unit to another telematics unit at stage 221 can include a request to update a certain number of words or word combinations. For example, given a limited timeframe where vehicles are passing one another, the two telematics units could exchange information on a small number of words or combinations (e.g., the three most recent words or combinations used). In another example, where vehicles are stationary or moving slowly and within range of one another, a larger number of words or combinations may be exchanged.
At stage 222 , the telematics unit 201 receives frequency or probability data from other telematics units 202 , and the language model of the telematics unit 201 is updated. In this implementation each telematics unit serves as both an information provider and an information collector. While the telematics unit 201 is receiving frequency or probability data and updating its language model, it is also sending its own frequency or probability data to the other telematics units so they can update their language models. In a further implementation, it will be appreciated that the exchange of language model information may be triggered by detection of other telematics units within range.
Process 230 corresponds to an implementation involving a centralized information collector 203 , where the telematics unit 201 and other telematies units serve as information providers. The information collector 203 can be a call center 108 , or some other type of centralized database or information aggregator. In this implementation, the telematics unit 201 queries the information collector and/or sends language model information (frequency data) at stage 231 . The information collector then updates its database, which contains information collected from telematics unit 201 as well as other telematics units. At stage 232 , the centralized information collector 203 sends this data to the telematics unit 201 so that its language model is updated to correspond to the aggregation of information collected by the information collector 203 .
It will be appreciated that the telematics unit 201 may query the information collector 203 automatically or based on a predetermined trigger. It will further be appreciated that in some implementations, the telematics unit 201 does not have to send a query for information and instead receives pushed frequency or probability data that is transmitted or broadcast from the information collector 203 .
Process 220 corresponds to a distributed information aggregation system while process 230 corresponds to a centralized information aggregation system, but it will be appreciated that processes 220 and 230 may be combined in a hybrid information aggregation system, were a telematics unit updates its language model based on information received from other telematics units 202 as well as from a centralized information collector 203 . Thus, it will be appreciated that the information aggregation system can be centralized, distributed, or a hybrid that utilizes features of both the described centralized and distributed information aggregation systems.
It will further be appreciated that frequency or data information for building language models may be specific to a particular dialect, language, and/or geographic region. In one exemplary implementation, telematics units include associated type information (e.g., that identifies the dialect, language, or a geographic region) corresponding to language model information being transmitted, so that other telematics units 202 and/or the information collector 203 can properly process such information. For example, a vehicle with a driver that speaks one language may not need to exchange information with a vehicle of another driver that speaks a different language, and thus the telematics unit could be configured to ignore language model information associated with other dialects, languages, or geographic regions. In another example, the information collector 203 can separately aggregate information associated with dialects, languages, or geographic regions and develop separate sets of language model information for each category. Then, upon receiving a request from a telematics unit for language model information from one or more of those categories (e.g., a bilingual person that requires a telematics unit with a language model for two languages), the information collector 203 is able to send only the language model information that is responsive to that request (e.g., by sending the language model information for those two languages to the telematics unit of the exemplary bilingual person).
While FIG. 2 describes systems and methods through which an accurate and reliable language model can be developed through aggregation of frequency or probability information, specific users of telematics unit have a privacy interest in the frequency or probability information that can be associated with them. Thus, according to an implementation of the present invention, a process 300 depicted by FIG. 3 is provided to avoid interfering with the users' privacy.
As shown in FIG. 3 , a telematics unit receives a query for frequency or probability information at stage 301 . An uncertainty variable is added to the frequency or probability information at stage 303 before the frequency or probability information is transmitted to the entity performing the query (e.g., another telematics unit or a centralized information collector) at stage 305 . It will be appreciated that the frequency or probability information sent in response to a query or sent to a centralized information collector may include an entire language model, information corresponding to a set of requested words, randomly selected words, etc. it will further be appreciated that a query at stage 301 might not be required, for example, when a telematics unit is sending its language model information to a centralized information collector, which may or may not be in response to a query from the information collector. Additionally, limitations may be put in place to prevent a single word from being queried too frequently to avoid receiving redundant information.
To give an example, if Joe queries Bob to update the probability corresponding to the word “winning” in the language model of Joe's telematics device, Bob sends back to Joe a probability which is equal to the actual probability plus a random value or Gaussian noise factor. It will be appreciated that the probability corresponding to a word corresponds to the probability of that word being used, which, for example, can be measured as the number of times that word has previously been used out of the total number of times all words have been used. The noise can be more dominant than the original frequency itself and can even cause a probability to be transmitted that is outside of the range of 0 to 1. Specifically, in this example, the probability corresponding to the word “winning” in Bob's language model may be a value such as 0.3. Noise is added to that value from a fixed distribution with a known mean. In a particular example using a Gaussian noise distribution with a zero mean having a standard deviation of 1 (i.e., N(0,1)), a random number is added to the actual probability, for example, −0.4, so Bob transmits to Joe that the probability corresponding to the word “winning” is 0.3±(−0.4), which is −0.1. While this result, taken alone, would not make sense, after Joe has a large enough sample size (e.g., after Joe has queried thousands of other telematics units for the probability of the word “winning,” all of which have returned a probability with an added uncertainty values according to the Gaussian noise distribution, Joe's telematics unit is able to ascertain what the average probability associated with the word “winning” with a high degree of confidence. The uncertainty introduced by each individual response is cancelled out when a large number of responses is aggregated because the average added uncertainty approaches the zero mean with larger sample size. It will, be appreciated that non-zero means may also be used, which would involve subtracting the known non-zero means from the aggregated responses.
In another example, an uncertainty value is added to an actual probability based on a Gaussian probability density function (pdf). Graphs 400 , 500 and 600 of FIGS. 4 , 5 and 6 respectively depict exemplary probability density functions corresponding to situations where the actual probability corresponding to a word or combination is about 0.3, but a Gaussian distribution of noise is added to protect the user's privacy. In each of the graphs the y-axis represents a non-normalized pdf and the x-axis represents the transmitted probability for a word.
Graph 400 depicts the probability density function (pdf) corresponding to a word or combination with Gaussian noise added, taking into account the data from only a single vehicle. The peak of the pdf is at the actual probability, but there remains a significant likelihood that the actual value is not the value that is transmitted by that vehicle. Graph 500 depicts the probability density function corresponding to the same word or combination except in view of the data from two vehicles. As can be seen from graph 500 , the probability density function corresponding to that word or combination is now narrower, indicating that the degree of error is getting smaller and that the average of the data from the two vehicles has a higher peak (indicating that the actual average probability corresponding to the word or combination is more likely to be reliable than in the one vehicle scenario). Graph 600 shows the probability density function in view of the data from 20,000 vehicles, and with such a large sample size, the degree of error introduced by adding Gaussian noise to each individual probability has practically disappeared.
It will be appreciated that frequency or probability data can be collected from a variety of sources and is not limited to data from communications made in conjunction with a telematics unit. For example, frequency data can be collected from a communication on a cell phone outside of the range of the telematies unit and retrieved from the cell phone by the telematics unit to update the language model of the telematics unit.
It will also be appreciated that implementations of the present invention can be used to collect data in other contexts and is not limited to collecting data for language modeling. For example, the present invention can be used to collect data pertaining to average vehicle speed, mileage, RPM and other driver data, while protecting users' privacy.
It will thus be appreciated that the described system and method allows for the collection of data for language modeling while maintaining the privacy of users. It will also be appreciated, however, that the foregoing methods and implementations are merely examples of the inventive principles, and that these illustrate only preferred techniques.
It is thus contemplated that other implementations of the invention may differ in detail from foregoing examples. As such, all references to the invention are intended to reference the particular example of the invention being discussed at that point in the description and are not intended to imply any limitation as to the scope of the invention more generally. All language of distinction and disparagement with respect to certain features is intended to indicate a lack of preference for those features, but not to exclude such from the scope of the invention entirely unless otherwise indicated.
The use of the terms “a” and “an” and “the” and “at least one” and similar referents in the context of describing the invention (especially in the context of the following claims) are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. The use of the term “at least one” followed by a list of one or more items (for example, “at least one of A and B”) is to be construed to mean one item selected from the listed items (A or B) or any combination of two or more of the listed items (A and B), unless otherwise indicated herein or clearly contradicted by context. The terms “comprising,” “having,” “including,” and “containing” are to be construed as open-ended terms (i.e., meaning “including, but not limited to”) unless otherwise noted. Recitation of ranges of values herein are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited herein. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”) provided herein, is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention.
Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as permitted by applicable law. Moreover, any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.
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A computer-implemented method is provided for statistical data learning under privacy constraints. The method includes: receiving, by a processor, a plurality of pieces of statistical information relating to a statistical object and aggregating, by the processor, the plurality of pieces of statistical information so as to provide an estimation of the statistical object. Each piece of statistical information includes an uncertainty variable, the uncertainty variable being a value determined from a function having a predetermined mean. The number of pieces of statistical information aggregated is proportional to the reliability of the estimation of the statistical object.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates broadly to improvements in battens for sails of boats and other sailcraft. More particularly, it concerns novel forms of sail batten luff caps, improved sail battens comprising such caps and batten-sail combinations equipped with the improved sail battens.
2. Description of the Prior Art
As explained in my previous patent U.S. Pat. No. 4,335,669, the disclosure of which is incorporated herein by reference, battens are extensively used with sails for sailcraft, e.g., sailboats, iceboats, wind propelled scooters, sail-boards, etc., to support and/or shape the sails. The sails with which battens are used include lugsails, lateen sails, square-rigged sails, jib-headed (Marconi rig) sails and gaff rig sails. This invention pertains primarily to battens for jib-headed sails.
Jib-headed sails may be divided into several classes with respect to battens, namely, unbattened sails, partial batten sails and full battened sails. The battens serve to support roach (excess cloth) formed into the leech of the sail. Hence, sails, e.g., those used on cruising boats, made without roach do not need battens so are unbattened.
In racing sailboats, iceboats and other racing sailcraft, high performance is demanded of the sails. The sails for such sailcraft are usually made with a high degree of roach and require battens to provide proper leech shape. The partial batten type sails use a plurality of battens that are carried in pockets extending forward from the leech only a minor length of their chords of the sails. In contrast, full battened sails use a plurality of battens carried in pockets that extend all the way from the leech to the luff of the sail at spaced intervals between the foot and the head of the sail. The full type battens are longer than their respective pockets and by compressing such batten in their pockets between the luff and the leech, the battens can be caused to bow. The greater the compression, the greater the bow creating a larger draft in the sail. Hence, compression on the full type (FT) battens is used by the sailcraft operator to control sail shape to obtain maximum performance from the sail for the prevailing wind conditions.
Compression on the FT battens drives their fore ends into the leading edge of the batten pocket and into the sail luff. Consequently, the sail cloth in the pocket and the luff is subjected to excessive wear, often resulting in the batten producing a hole in the sail at the luff. Such damage to the sail is particularly severe where the fore ends of the FT battens are square. In order to reduce this form of sail damage, FT battens have been provided with rounded fore ends and/or rounded luff caps. Also, rigid cups made of plastic or the like have been riveted over the fore ends of the batten pockets. However, these modifications to FT batten arrangements have not fully eliminated the indicated batten compression damage to luff portions of sails in full battened sails for sailcraft.
OBJECTS
A principal object of the present invention is the provision of new improvements in sail battens. Further objects include the provision of:
(1) New forms of luff caps for battens.
(2) Improved forms of FT sail battens designed to mitigate compression damage to the luff portions of sails using FT battens.
(3) Novel sail batten pocket and sail batten combinations.
(4) Improved forms of full battened sails.
Other objects and further scope of applicability of the present invention will become apparent from the detailed description given hereinafter; it should be understood, however, that the detailed description, while indicating preferred embodiments of the invention, is given by way of illustration only, since various changes and modifications within the spirit and scope of the invention will become apparent to those skilled in the art from this detailed description.
SUMMARY OF THE INVENTION
These objects are accomplished in accordance with the present invention by the provision of sail battens provided at their fore ends with improved forms of luff caps. Basically, the new luff caps have a fore portion with a leading edge that for the majority of its length defines a straight line which will form an acute angle with the longitudinal axis of the batten to which they are fixed.
In their preferred embodiments, the means for fixing the new luff caps to battens is a slot in the aft portion of a size and shape to tightly envelope the fore ends of the battens, but other fixing means may be used. The fore portions of the new luff caps may be solid or, alternatively, they may be made with transverse openings to make them lighter.
Additionally, the invention objects are accomplished by provision of (a) new sail battens having the new luff caps as described fixed to their fore ends, (b) combinations of sail pockets and such new FT sail battens and (c) sails equipped with such sail pocket-batten combinations.
BRIEF DESCRIPTION OF THE DRAWINGS
A more detailed understanding of the new devices of the invention and their use may be had by reference to the accompanying drawings, in which:
FIG. 1 is a schematic prospective view of a catamaran sailboat equipped with a mainsail containing new FT battens of the invention.
FIG. 2 is a fragmentary, lateral view of a FT batten and sail combination of the invention.
FIG. 3 is a fragmentary, sectional view taken on the line 3--3 of FIG. 2.
FIG. 4 is a lateral, sectional view of a new batten luff cap of the invention.
FIG. 5 is an exploded, fragmentary, isometric view of a luff cap and batten combination of the invention.
FIG. 6 is a lateral view of a set of luff caps for a set of battens to used in a full battened sail such as shown in FIG. 1.
FIG. 7 is an isometric view of a modified form of luff cap of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring in detail to the drawings, a sail batten device 2 of the invention for a full battened sail 4 comprises a batten 6, new type luff cap 8 and batten constraining member 10.
The batten 6 has a fore portion 12 and an aft portion 14 joined integrally with a central body portion 16. The batten 6 may include strengthening ribs 18 that may extend the full length of the batten or, as illustrated in the drawings, the ribs may stop short of the ends to leave the fore portion 12 and aft portion 14 free of the ribs 18. This latter arrangement simplifies the fixing of the luff cap 8 to the batten 6 as explained below.
The luff caps 8 comprise a fore portion 20 and an integral aft portion 22 that contains a slot 24 which serves as means for fixing the caps 8 to battens 6. As illustrated, the slot 24 has a simple rectangular cross-section to mate with the unribbed, fore portion 12 of batten 6. Cement, adhesive, or the like may be applied between the slot inner-surface 26 and the outer-surface 28 of batten portion 12 to ensure permanent connection between the parts.
If the battens 6 have ribs (not shown) that extend the entire length of thereof, the slots (not shown) in the luff caps would be shaped as a female opening to sungly receive the batten fore portion. Also, other means for fixing the caps to the battens may be used, e.g., luff caps (not shown) with solid aft portions can be butt welded to the front edges of the battens.
The cap fore portion 20 has a leading edge 30 that for the majority of its length defines a straight line which forms an acute angle "a" with the longitudinal axis of slot 24 and, in turn, with the longitudinal axis of the batten 6.
The fore portion 20 of luff caps 8 consist of a solid section in the shape of a right triangle. In the modified form of luff caps 8a of FIG. 7, the fore portion 20a has a transverse opening 32 therethrough. This serves to lessen the cap weight without serious harm to the cap strength. The width of the fore portion 20a is also reduced relative to the width of the aft portion 22 also for weight reduction.
The full battened sailcraft sail 4 has a foot 34, luff 36, head 38 and leech 40. A series of batten pockets 42 are spaced apart along the sail 4 between the foot 34 and head 38. As seen in FIG. 1, each pocket 42 extends substantially the full distance between the luff 36 and leech 40 at the position in the sail where each pocket is located. In the construction of the full battened type (FBT) sails, such as sail 4, the battens are not all parallel nor is the longitudinal axes of the pockets 42 perpendicular to the sail luff 36. Hence, the longitudinal axis of at least some of the batten pockets 42 define, relative to the sail luff 36, a different acute angle "a" from that of other of the pockets in the sail 4.
The construction of the pockets 42 is not critical to the present invention, i.e., the new batten devices 2 are intended for use with sails and sail pockets of any conventional style of FBT sails. Typically, batten pockets of such sails comprise a layer 44 of sailcloth fixed to the sailcloth 46 of the sail 4 by stitching 48. Generally, such sails are made of a series of cloth panels with the pockets 42 located at the junctions of the panels.
The batten constraining device 10 shown is of the type described and claimed in U.S. Pat. No. 4,335,669, but any other type of constraining device for battens may be used in practicing the present invention.
The aft ends 50 of the pockets 42 are open and terminate at the sail leech 40. The fore ends 52 are closed and are adjacent the sail luff 36 and substantially parallel thereto. When installed properly in a sail pocket 42, the leading edges 30 of the new batten caps 8 bear against the fore ends 52 of the pockets 42 with these two parts in line-to-line contact.
In preferred forms of sail combinations of the invention, rigid caps 54 are fixed, e.g., by rivets 56, adjacent the sail luff 36 about the closed fore ends 52 of the pockets 42 to serve as bearing members for the luff caps 8 of the battens 6 carried in the pockets 42. The caps may be molded of rigid plastic, stamped from metal or made in any other suitable manner.
Since, a plurality of batten pockets in a sail will have longitudinal axes extending at different acute angles relative to the sail luff, a set of the new batten caps will be formed with various leading edge angles. FIG. 6 illustrates a set of luff caps for a typical sail. Cap 8b has a leading edge angle of 50°, while caps 8c, 8d, 8e, 8f and 8g have leading edge angles of 56°, 64°, 71°, 76° and 82° respectively. A typical set of caps may consist of, for example, one each of 8b, 8c, 8d and 8f plus two each of 8e and 8g.
The new luff caps are preferably made by injection molding from rigid plastic, e.g., nylon, ABS, etc., but they may also be made of any other suitable material, e.g., metal, wood, etc., by any desired fabrication method.
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Sail battens for full battened sails are provided on their fore ends with luff caps that have an angled leading edge. The improved battens are used in sail batten pockets that do not extend perpendicular to the sail luff to prevent the batten fore end from wearing holes in the batten pockets as occurs with battens having square ends when used in such angled batten pockets.
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CROSS REFERENCE TO RELATED PATENT APPLICATIONS
[0001] This application is related to, and claims the benefit of, U.S. Provisional Patent Application No. 61/663,891, filed Jun. 25, 2012. The above-identified priority patent application is incorporated herein by reference in its entirety.
FIELD
[0002] The present technology relates to a line hauler having a dualler plate and deflector to allow for hands free hauling of lines. More specifically, the technology is a kit comprising a dualler plate and a deflector as an improvement over existing line haulers.
BACKGROUND
[0003] Line haulers are used on commercial fishing vessels to haul in crab pots, prawn pots and fish. They are usually very large and have features that are necessary for hauling in very large catches. There are also line haulers for individuals to use on a much smaller scale. One such hauler is the Ace Line Hauler Brutus Plus 40®.
[0004] Regardless of the size of the hauler, there are a number of features that are common. A typical hauler generally has a motor for driving a sheave, which hauls the line in. The sheave is usually V-shaped sheave for gripping the line. Pulleys and various positioners are disclosed. Some have line coilers.
[0005] U.S. Pat. No. 4,354,667 discloses pivotal support bearings that permit the unit to revolve freely about a fixed bearing axis in addressing itself to the incoming line being hauled and that restrain the unit against other bodily motion.
[0006] The V-shaped sheave can cause the line to remain in the sheave, especially if there are knots along the line. U.S. Pat. No. 3,034,767 discloses a separator that projects upwardly into the sheave, to separate the line from the V groove of the sheave. It also comprises a sloping shoulder to deflect and direct the outgoing line from the bight before it leaves the sheave in the normal direction in which the sheave rotates.
[0007] One prior device for laying up hauled lines in coils is disclosed in U.S. Pat. No. 3,750,970. In that case the line fed downwardly into the receiving barrel or tub was guided through a rotating deflection tube or slinger directing the line outwardly by centrifugal force so as to form a descending spiral to make up the accumulating coil.
[0008] In U.S. Pat. No. 4,165,830 it is disclosed that the line thrust fed downwardly from a generally central position into a cylindrical bin by a combination of two sheaves and a pneumatic tire roller means will assume a coiled configuration in the container of sufficient orderliness for practical purposes and that in performing this operation the apparatus accommodates also the heavy and bulky shot-connecting knots, even at the highest hauling rates used in this fishery.
SUMMARY
[0009] A line hauler with dualler plate is provided to assist a user in hauling lines holding seafood traps. The line hauler reduces the need for the user to haul in the lines as it reduces or eliminates slippage of the line. The line hauler comprises a stand, a first pulley, a second pulley and a sheave, the sheave comprising two sides and a groove therebetween, a drive shaft, an electric motor for driving the sheave rotationally with the drive shaft, the improvement being a dualler plate and retainers, the dualler plate comprising a circular stainless steel plate, a central aperture for accepting the drive shaft and apertures corresponding to apertures in the sheave for accepting the retainers, the dualler plate dividing the groove into a first V-channel and a second V-channel, such that in use, a line is fed from the upper side of the first pulley to an upper side of the first V-channel, to a lower side of the second pulley, and returning to the sheave on an upper side of the second V-channel.
[0010] In use, the line hauler further comprises the line, the line being fed from the upper side of the first pulley to the upper side of the first V-channel, to the lower side of the second pulley, and returning to the sheave on the upper side of the second V-channel.
[0011] The V-channels of the line hauler are preferably 0.5 inches wide at the outer edge and about 1.5 inches deep.
[0012] It is preferred that the dualler plate is sized to match the plates, and is therefore about 8 inches to about 11 inches in diameter.
[0013] The line hauler preferably comprises a line coiler, the line coiler comprising a first section affixed to the line hauler, a second section at right angles to the first section, sloped about 16 to about 21 degrees towards the sheave and adjacent at least the second V-channel and an end section at about 43 to about 47 degrees to the second section, proximate the second V-channel and angled away from the sheave, wherein the line is threaded between the first V-channel and line coiler and is fed over the line coiler from the second V-channel, such that in use, the line coiler is urged to coil.
[0014] The line coiler can alternatively be described as having an attachment member attached to the line hauler, a directing member extending therefrom proximate the second V-channel and configured to direct a line from the second V-channel, and an end member extending from the second member, the end member essentially parallel to the V-channels.
[0015] The line coiler may also include an O-ring seated in the second V-channel.
[0016] As fishers may already have a line hauler, it is advantageous to provide a kit for use with a line hauler, the line hauler comprising a stand, a first pulley, a second pulley and a sheave, the sheave comprising two sides and a groove therebetween, a drive shaft, an electric motor for driving the sheave rotationally with the drive shaft, the kit comprising: a rotatable member for increasing friction on a line; retainers; and a line coiler.
[0017] The line coiler comprises a first section for affixing to the line hauler, a second section angled at about 85 degrees to about 95 degrees to the first section and a third section that is angled at about 43 to about 90 degrees from the second section to encourage a line to remain on the line coiler and return back over the second section, such that in use, the line coiler extends outward and downward from the line hauler.
[0018] More specifically, the rotatable member is a dualler plate, the dualler plate comprising a circular stainless steel plate, a central aperture for accepting the drive shaft and apertures corresponding to apertures in the sheave for accepting the retainers, the dualler plate for dividing the groove into a first V-channel and a second V-channel, such that in use, a line is fed from the upper side of the first pulley to an upper side of the first V-channel, to a lower side of the second pulley, and returning to the sheave on an upper side of the second V-channel.
[0019] The line coiler of the kit is further defined as follows: the first section is about 4 to about 6 inches long, the second section is at about 85 degrees to about 95 degrees to the first section, sloped about 16 to about 21 degrees from the plane of the first section and about 1.25 inches to about 2.25 inches long and the third section at about 43 to about 47 degrees to the second section and about 0.4 to about 1 inch long.
[0020] The kit of claim further comprises an O-ring for seating in the second V-channel.
[0021] A line coiler for use with a line hauler is also provided. The line coiler comprises a first section for affixing to the line hauler, a second section angled at about 85 degrees to about 95 degrees to the first section and a third section that is angled at about 43 to about 90 degrees from the second section to encourage a line to remain on the line coiler and return back over the second section, such that in use, the line coiler extends outward and downward from the line hauler.
[0022] A method of preparing and using a line hauler with a dualler plate is also provided, the method comprising:
attaching the dualler plate between a first plate and a second plate of a sheave to provide a first V-channel and a second V-channel; feeding a line over a first pulley to the first V-channel, to an upper side of the first V-channel, to a lower side of the second pulley, and returning to the sheave on an upper side of the second V-channel.
[0025] Preferably, the line hauler comprises a line coiler, and therefore the method further comprises threading the line between the line coiler and the first V-channel, to a lower side of the second pulley, returning to the sheave on an upper side of the second V-channel and over the line coiler.
FIGURES
[0026] FIG. 1 is a prior art line hauler.
[0027] FIG. 2 is a view of the sheave with dualler plate and line coiler.
[0028] FIG. 3 is a plan view of the dualler plate and the line coiler.
[0029] FIG. 4 is a view of the sheave with the dualler plate and line coiler.
[0030] FIG. 5 is a plan view showing routing of the line.
DESCRIPTION
[0031] A line hauler, generally referred to as 10 is shown in FIG. 1 . The line hauler has a stand 12 , a sheave 14 , a first pulley 16 , a second pulley 18 and a motor 20 . The stand 12 has a base plate 26 , a saddle 28 for mounting onto the base plate 26 and for adjustably mounting an upright 30 . The upright 30 is generally triangular in shape to accommodate the sheave 14 and motor 20 . An aperture 32 extends through the upright 30 to accept a drive shaft 34 . An arm 36 extends from the upright 30 and is braced with a brace 38 . The arm 36 is retained with a cotter pin 40 to allow for easy folding. An arm extension 42 is housed in a sleeve 44 at the distal end of the arm 36 . A cotter pin 46 retains the arm extension 42 .
[0032] A standard prior art sheave 14 , as provided by Ace Line Hauler™ can be seen in FIG. 2 . The sheave 14 has a first plate 50 and second plate 52 and a V-groove 54 therebetween. The groove is 1.5 inches deep and 1 inch wide at the outer edge 55 . The plates 50 , 52 are bolted to one another by a series of bolts 56 that fit through a series of apertures 58 . The drive shaft 34 is centrally located in the sheave 14 and is directly connected to the motor 20 to drive the sheave 14 . The sheave 14 , drive shaft 34 and motor 20 are mounted on the stand 12 .
[0033] Returning to FIG. 1 , a first pulley 60 is suspended from the distal end 62 of the arm extension 42 by a swivel 64 , link 66 and hanger 68 . A second pulley 70 is mounted on the upright 30 . The hanger 68 has an aperture 72 to accept a pulley axle 74 . The second pulley 70 is mounted on a pulley shaft 76 that is housed in an aperture 78 in the upright 30 .
[0034] As shown in FIG. 4 , the line hauler 10 is provided with a dualler plate 80 and a line coiler 82 . The dualler plate 80 is located between the first plate 50 and the second plate 52 and divides the V-groove 54 , hence providing two V-channels, a first V-channel 84 and a second V-channel 85 , each having a much reduced angle at the bottom 89 of the V-channel (rather than the angle defined as 1 inch wide at the outer edge 55 over 1.5 inches of depth, the angle is about 0.5 inch wide at the outer edge 55 over about 1.5 inches of depth) (see FIG. 4 where angle 200 is about 32 to about 35 degrees, preferably about 33 degrees and angle 300 [the angle without the dualler plate] is about 66 degrees). The dualler plate 80 is a flat 11 inch diameter by 1/16 inch thick stainless steel plate (essentially the same dimensions as the plates 50 , 52 of the sheave 14 ). As shown in FIG. 3 , apertures 90 are for aligning with the apertures 58 of the standard sheave 14 . A central aperture 59 is for accepting the drive shaft 34 . The second V-channel 85 may be provided with a 3/16 inch to about ¼ inch O-ring 87 that seats in the bottom 89 of the V-channel 85 .
[0035] The line coiler 82 is mounted on the motor frame 92 with 2.25 inch bolts 94 and nuts 96 , as shown in FIG. 4 . It extends straight from the frame 92 . As shown in FIG. 3 it has a first section 98 that is about 5 inches long by about 1.5 inches wide by about 0.25 inches deep, a second section 100 approximately at right angles to the first section 98 that is about 1.75 inches long by about 1.5 inches wide by about 0.25 inches deep and is sloped about 0.5 inch down over its width, in other words, is at about an 18 degree angle relative to the first section 98 , with the lower side 102 away from the sheave 14 and the upper side 104 proximate the sheave 14 , and an end section 106 that is about 0.5 inches long by about 1.5 inches wide by about 0.25 inches deep that is bent away from the sheave 14 at about a 45 degree angle. Returning to FIG. 4 , the line coiler 82 is positioned such that the second section 100 is aligned with at least the second V-channel 85 of the sheave 14 .
[0036] The first section 98 is sized to extend from the frame 92 a sufficient distance to allow the second section 100 to be in front of the sheave 14 , hence, depending on the mounting location, the section could be longer or shorter, but preferably it is about 4 inches to about 6 inches long, more preferably about 4.5 to about 6.5 inches long, and most preferably about 5 inches long. The second section 100 is sized to extend over at least the second V-channel 85 and therefore is about 1.25 inches to about 2.25 inches long, preferably about 1.5 inches to about 2 inches long and most preferably about 1.75 inches long. The end section 106 is designed to ensure that the line 110 does not skip over the end 112 and therefore it is at least about 0.4 inches long, preferably at least about 0.45 inches long and most preferably at least about 0.5 inches long. As it could catch a user's clothing, it is best to not be any longer than about 1 inch long. All the sections are made from 1.5 inch stock, however, the sections may be about 1 inch wide to about 2 inches wide, preferably about 1.25 inches to about 1.75 inches wide and most preferably about 1.5 inches wide. The thickness of the material should allow for bending of the stock and is therefore about 0.05 inches to about 0.15 inches thick, preferably about 0.07 to about 0.1 inches thick and most preferably about 0.09 inches thick.
[0037] The angle between the first section 98 and the second section 100 is disclosed as a right angle, which may be about 85 degrees to about 95 degrees, preferably about 87 degrees to about 92 degrees and most preferably about 90 degrees, however, if the first section 98 is mounted in an alternative location, the angle will be different and therefore is better described as an angle that permits mounting of the first section 98 such that the second section 100 is normal to the V-channels 84 , 85 .
[0038] The angle that the second section 100 is sloped away from the sheave 14 can be about 16 degrees to about 21 degrees, preferably about 17 degrees to about 20 degrees and most preferably about 18 degrees to about 19 degrees. The distance between the second section 100 and the outer edge 55 of the sheave is about 0.4 inches to about 0.7 inches, preferably about 0.5 inches to about 0.625 inches on the upper side 104 of the second section 100 and is preferably about 0.9 inches to about 1.35 inches, preferably 1 inch to about 1.25 inches on the lower side 102 of the second section 100 . This can also be described as the angle from the plane 99 of the first section 98 .
[0039] The angle between the second section 100 and end section 106 can be about 43 degrees to about 47 degrees, preferably about 44 degrees to about 46 degrees and most preferably about 45 degrees. The end section 106 , therefore, is essentially parallel to the V-channels 84 and 85 and to the line 110 as it leaves the sheave 14 .
[0040] The angle that the second section 100 is sloped and the angle of the end section 106 relative to the second section 100 determines the efficiency of the line coiler 82 . Experimentation has shown that the range of angles that can be used effectively is very small. Angles outside of the cited range will not result in the line coiling as it comes off the sheave 14 .
[0041] As shown in FIG. 5 , the line 110 is routed through the line hauler 10 as follows: The line 110 enters into the first pulley 60 on an upper side 120 and then enters the first V-channel 84 of the sheave 14 , which is the innermost V-channel, passing over the upper side 124 of the sheave 14 and down to the second pulley 70 on a lower side 122 . From the lower side 122 of the second pulley 70 , the line returns to the sheave 14 , entering the second V-channel 85 , passing over the upper side 124 of the sheave 14 . The line is then fed over the second section 100 of the line coiler 82 . The line 110 then self-coils on the floor of the boat, without requiring a bin or other circular vessel to assist in coiling the line 110 .
[0042] The path of the line 110 on the pulleys 60 , 70 and sheave 14 stops slippage of the line 110 , which can trap the line, and without any human intervention. The line coiler coils the line, again without human intervention. Therefore, the two components provide for “hands free” operation of a line hauler. Without the dualler plate and the rope coiler, a user who has 4 prawn traps with 400 ft of line on each trap, would have to assist normal hauler operation, moving their hands, arms and shoulders 1200 to 1600 repetitions, each time they pulled the traps.
[0043] The foregoing is a description of an embodiment of the present technology. As would be known to one skilled in the art, variations that do not alter the scope of the technology are contemplated. For example, the line coiler may be attached to another component, or a different frame and therefore may be attached to the side opposite the motor, the requirement being that the second section be adjacent the second V-channel and that the end section be proximate the second V-channel and be angled away from the sheave.
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An improved line hauler is provided that has a dualler plate located between the two plates of the sheave. The dualler plate creates two V-channels for the line and the line therefore can be directed on a path that results in a hands free line hauler that is slip free. A line coiler is also provided that promotes coiling of the line as it drops to the boat deck.
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DESCRIPTION OF THE BACKGROUND
The present invention relates to improved pipe coupling, and more particularly relates to improved construction of a pipe coupling made of a plug and socket separably assembled with each other.
Conventionally, metallic materials are in general used for major elements of a pipe coupling and assembly of these elements is mostly based upon screw engagements or projection-hollow engagements. Such manner of assembly requires application of delicate machining after initial shaping of the elements in manufacturing, and also requires complicated operation for assembly and disassembly of the pipe coupling in use.
In practice, it is often required to adjust flow rate of fluid passing through a piping system including the pipe coupling. Conventionally, a separate cock is connected to the pipe coupling in order to enable such adjustment of the flow rate. Addition of such a cock inevitably results in a complicated and enlarged construction of the pipe coupling and its related parts in the piping system.
SUMMARY OF THE INVENTION
It is one object of the present invention to provide a pipe coupling which can be manufactured very easily.
It is another object of the present invention to provide a pipe coupling which can be very easily operated in use.
It is the other object of the present invention to provide a pipe coupling which enables free adjustment of flow rate despite its very simple, light and compact construction.
In accordance with the present invention, there is provided a plug and a socket releaseably attached to the plug. The plug includes a tubular nose section having a front end, a rear end, an outer surface, an internal valve seat formed within the nose section between the front and rear ends thereof, an annular latching groove formed in the outer surface of the nose section between the front and rear ends thereof, an axial conduit extending through the nose section from the front end thereof to the valve seat and a conical flange projecting outwardly from the outer surface of the nose section between the latching groove and the front end of the nose section. The plug also includes a tubular tail section having a front end attached to the rear end of the nose section in a fluid-tight manner, a rear end, a fore conduit formed in the front end of the tail section and communicating with the axial conduit in the nose section and an aft conduit formed in the rear end of the tail section and communicating with the fore conduit formed in the front end of the tail section, and a valve. The valve has a main body moveably received in the fore conduit of the tail section and a tubular extension attached to the main body and slideably received in the axial conduit of the nose section, at least one radial opening formed in the extension adjacent to the main body, an axial opening formed in the extension and communicating at one end with the radial opening and at an opposite end with the axial conduit of the nose section and urging means for urging the main body from a first position in which the radial opening or openings communicate with the fore conduit of the tail section, whereby the axial and radial openings in the extension of the valve cooperate with the axial conduit in the nose section and the fore and aft conduits in the tail section to form a fluid flow path through the plug, towards a second position in which the main body engages the valve seat formed in the nose section, whereby the fluid flow path through the plug is closed.
The socket includes a tubular main member having a front end sized and shaped so as to releaseably receive the front end of the nose section of the plug, a rear end, an internal projection extending axially with the main member, an axial conduit extending between the projection and the rear end of the main member and communicating with the axial opening in the extension of the valve of the tail section of the plug and a substantially flat resilient tongue projecting outwardly from the front end of the main member. The socket also includes a tubular mantle member positioned over the front end of the main member so as to form an annular space between the mantle member and the front end of the main member and having a radial opening in alignment with the tongue of the main member. The socket also includes a latching member having a ring section positioned in the annular space for radial movement between a first position in which the annular ring engages the latching groove of the nose section of the plug, whereby the plug and the socket are coupled together, and a second position in which the annular ring disengages the latching groove of the nose section of the plug, whereby the plug and the socket may be uncoupled, and a tongue section positioned in the radial opening of the mantle member and supported by the tongue of the main member such that the ring section assumes its first position when the tongue of the main member is in an unflexed state and such that the ring section assumes its second position when the tongue of the main member is flexed as a result of the manual depression of the tongue section of the latching member of the socket.
In order to be able to regulate the flow rate of fluid flowing through the coupling, the projection of the main member of the socket is moveably positioned within the main member and the socket is provided with adjusting means for adjusting the position of the projection. More particularly, the projection engages the extension of the valve of the tail section of the plug to move the main body of the valve into its first position, thereby permitting fluid to flow through the coupling. In one embodiment, the adjusting means includes a pin inserted into a recess formed in the projection through a helical guide slot formed in the main member of the socket.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a sectional side view of one embodiment of the plug in accordance with the present invention.
FIG. 2 is a sectional side view of one embodiment of the socket in accordance with the present invention,
FIG. 3 is a section taken along a line III--III in FIG. 2,
FIG. 4 is a perspective view of the socket shown in FIG. 2 in a disassembled state,
FIG. 5 is a side sectional view of the pipe coupling made up of the plug in FIG. 1 and the socket in FIG. 2 in the firmly assembled state,
FIG. 6 is a side view, partly in section, of the pipe coupling in FIG. 5 in the state ready for disassembly,
FIG. 7 is a side sectional view of the other embodiment of the socket in accordance with the present invention,
FIG. 8 is a section taken along a line VIII--VIII in FIG. 7,
FIG. 9 is a section taken along a line IX--IX in FIG. 7;
FIG. 10 is a side view, partly in section, of the pipe coupling made up of the plug in FIG. 1 and the socket in FIG. 7 in one firmly assembled state in which the flow rate is highest,
FIG. 11 is a side view, partly in section, of the pipe coupling in FIG. 10 in another firmly assembled state in which the flow rate is minimal, more clearly naught, and
FIG. 12 is an outer view of the socket shown in FIG. 7.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As briefly described already, the pipe coupling of the present invention is made up of a plug and a socket detachably assembled with each other. In the following descriptions, the side of either of the elements adapted for assembly with another of the element will be referred to with words such as front and fore, and the opposite side with words such as back and rear.
One embodiment of the plug in accordance with the present invention is shown in FIG. 1. A plug 10 is made up of a tubular fore piece 14 and a tubular rear piece 18 fixedly coupled, preferably by fusion, to each other by means of a seal ring 20. The pieces 14 and 18 are both preferably made of a synthetic resin.
The fore piece 14 is provided with a nose section 12 to be inserted into a socket when the pipe coupling is assembled. Near the front end, the nose section 12 is externally provided with a seal ring 22, a conical flunge 24 and an annular latching groove 26 formed just on the back side of the flange 24. The fore piece 14 further internally defines an axial fore conduit 38 for the fluid flowing through the pipe coupling.
The rear piece 18 is provided with a tail section 16 adapted for connection with any suitable hose. The rear piece 18 is further internally defines an axial rear conduit 36 for the fluid flowing through the pipe coupling, and an intermediate conduit 37 of a larger diameter.
A valve 30 having a conical head is arranged about the junction between the pieces 14 and 18 with its seal ring 32 in pressure contact with a funnel-shaped seat 34 formed on the internal surface of the fore piece 14. This pressure contact is caused by a helical compression spring 28 interposed between the valve 30 and the rear end of the intermediate conduit 37. An axial projection 44 is formed on the rear end of the intermediate conduit 37 in order to limit excessive rearward movement of the valve 30. The valve 30 is provided with tubular front extension 42 slidably received in the fore conduit 38 of the fore piece 14. The front extension 42 terminates near the front opening of the fore conduit 38 and, at a position near the conical head of the valve 30, is provided with at least one radial opening 40.
One embodiment of the socket in accordance with the present invention is shown in FIGS. 2, 3 and 4. A socket 100 is made up of a tubular main piece 110, a latching piece 120, a mantle piece 130 and a stop piece 140. These pieces 110 and 140 are all preferably made of a synthetic resin. In particular, at least the main piece 110 should be made of a synthetic resin since it is required to be somewhat resilient as hereinafter described in more detail.
The main piece 110 is provided with a front nose section 111 adapted for accommodating the nose section 12 of the plug 10 and a tail section 112 adapted for connection with any hose. The nose section 111 is provided, near its periphery, with a tongue 113 projecting forwards, and, near its center, a center projection 114. The main piece 110 internally defines an axial conduit 115 which opens in the center projection 114.
The mantle piece 130 is internally designed so that, when it is inserted over and fixed to the nose section 111 of the main piece 110, an annular groove 131 is left in front of the front end of the nose section 111. A radial opening 132 is formed in the wall of the mantle piece 130.
The latching piece 120 includes a ring section 121 and a tongue 122 extending rearwards from the ring section 121 as best seen in FIG. 4. In the assembled state of the socket 100, the stop piece 140 is inserted over and fixed to the rear end portion of the nose section 111 of the main piece 110 in order to prevent falling of the mantle piece 130 inserted over the main piece 110. The tongue 122 of the latching piece 120 rests on the tongue 113 of the main piece 110 so that the latching piece 120 is suspensibly held by the main piece 110. In this state, the ring section 121 of the latching piece 120 is received partly in the annular groove 131 provided by the mantle piece 130 as shown in FIG. 2. Further, the tongue 122 of the latching piece 120 appears in the radial opening 132 of the mantle piece 130 with its outer surface substantially flush with that of the mantle piece 130.
Assembly of the pipe coupling using the plug 10 in FIG. 1 and the socket 100 in FIG. 2 is carried out as follows.
As the nose section 12 of the plug 10 is inserted into the nose section 111 of the main piece 110 of the socket 100, the ring section 121 of the latching piece 120 is depressed into the annular groove 131 due to pressure abutment with the conical flunge 24 of the plug 10 and the tongue 122 of the latching piece 120 sinks in the radial opening 132 of the mantle piece 130 while bending the resilient tongue 113 of the main piece 110. Due to the above-described pressure abutment with the conical flange 24 of the plug 10, the ring section 121 of the latching piece 120 is now fully placed in the annular groove 131 provided by the mantle piece 130 to allow further insertion of the plug 10 into the socket 100.
As the latching groove 26 of the plug 10 arrived at the position of the annular groove 131, the ring section 121 of the latching piece 120 automatically falls into the latching groove 26 of the plug 10 due to spring-back of the resilient tongue 113 which is now released from the pressure contact with the tongue 122 of the latching piece 120. Consequently, the plug 10 and the socket 100 are now firmly assembled together as shown in FIG. 5.
In this assembled state, the front end of the center projection 114 of the socket 100 abuts against the front end of the front extension 42 of the valve 30 and pushes the valve 30 rearwards off the seat 34 while overcoming the repulsion of the compression spring 28. Thus, a continuous flow passage is established through the pipe coupling, which includes the rear and intermediate conduits 36 and 37, a clearance formed between the conical head of the valve 30, the radial openings 40 in the front extension 42, the interior of the front extension 42, and the conduit 115 of the socket 100.
Under the condition shown in FIG. 6, the tongue 122 of the latching piece 120 is depressed by a finger F towards the axis of the pipe coupling while bending the flexible tongue 113 of the main piece. By this depression, the ring section 121 is brought out of engagement with the latching groove 26 of the plug 10 and placed fully within the annular groove 131 of the socket. Due to disappearance of the latching engagement, the plug 10 and the socket 100 can easily be disassembled from each other.
In accordance with the present invention, at least the main piece 110 of the socket 100, more preferably both the entire plug 10 and socket 100, is made of a resilient material such as synthetic resin. For example, the known plastic injection moulding may be used for manufacturing the pipe coupling. This greatly simplifies manufacturing of the pipe coupling whilst naturally causing corresponding lowering in manufacturing cost.
The latching piece 120 is suspensibly held by the resilient tongue 113 of the socket 100 with its outer surface being substantially flush with that of the socket. This flush construction successfully avoids accidental depression of the latching piece 120, i.e. accidental disassembly of the pipe coupling, by application of any unexpected external force. The flush construction further provides a simple outer design of the pipe coupling.
Disassembly of the pipe coupling is carried out utilizing the resilient nature of the tongue 113 of the socket without requirement for provision of any additional spring to that effect. This also contributes to lowering in manufacturing cost.
It will be well understood with the foregoing embodiment that the flow rate of the fluid passing through the pipe coupling in the assembled state is determined by the dimension of the annular clearance formed around the conical head of the valve 30 in FIG. 5. In the case of the foregoing embodiment, the dimension of this clearance is fixed once the mechanical design of the pipe coupling is fixed.
Another embodiment of the socket shown in FIG. 7 enables adjustment of the flow rate even with the fixed mechanical design of the pipe coupling.
A socket 50 includes a main piece 52, a mantle piece 58, a latching piece 62, a flow rate adjuster piece 86 and a valve pressor piece 70. At least the main piece 52 and the adjuster piece 86, more preferably all the pieces, are made of a resilient material such as synthetic resin.
The main piece 52 is provided with a nose section 53 adapted for receiving the nose section 12 of the plug 10, and a tail section 56 adapted for connection with any hose. The main piece 52 further internally defined a fore conduit 54 of a large diameter and a rear conduit 55 of a small diameter in axial communication with each other. At a position near the tail section 56, a small flange 84 is formed on the main piece 52 for snap coupling with the adjuster piece 86. The nose section 53 is provided with a tongue 69 projecting forwards. A guide slot 78 is formed through the wall of the main piece 52, which extends spirally over a prescribed length. A flow rate indicator band 98 is disposed to the outer surface of the main piece 52. This indicator band 98 extends in the peripheral direction and includes flow rate indications. One example of such an indication is shown in FIG. 12, in which H designates high flow rate.
The mantle piece 58 is fixedly inserted over the nose section 53 of the main piece 52 in an arrangement such that an annular groove 66 is left in front of the fore end of the nose section 53. A radial opening 59 is formed in the mantle piece 58 in order to receive the latching piece 62 as hereinafter described in more detail. An axial conduit 60 is formed in the mantle piece 58 in communication with the fore conduit 54 of the main piece 52.
The latching piece 62 includes a ring section 64 received in the annular groove 66 provided by the mantle piece 58, and a tongue 68 extending rearwards and located in the radial opening 59 of the mantle piece 58. Under the condition shown in the drawing, the tongue 68 of the latching piece 62 rests on the tongue 69 of the main piece 52. In other words, the latching piece 62 is suspensibly supported by the main piece 52 in the mantle piece 58 as shown in FIG. 8. Here, the exposed outer surface of the latching piece 62 is substantially flush with that of the mantle piece 58.
The valve pressor piece 70 is slidably inserted into the fore conduit 54 of the main piece 52 by means of seal rings 72. The pressor piece 70 is provided with a center projection 74 extending forwards, and an axial conduit 71 opening in the center projection 74. This pressor piece 70 is provided, in its outer surface, with a recess 76.
The flow rate adjuster piece 86 is inserted over the middle section of the main piece 52 and internally defines a guide groove 88 extending in the axial direction. A guide pin 82 is inserted into the recess 76 of the pressor piece 70 via the guide slot 78 of the main piece 52 with its head 80 being received in the guide groove 88 of the adjuster piece 86. The adjuster piece 86 is designed so that its inner surface is in tight pressure contact with the head 80 of the guide pin 82. Consequently, as the adjuster piece 86 is axially turned about the main piece 52, the guide pin 82 revolves helically about the axis of the main piece 52 due to the helical arrangement of the guide slot 78 and this helical revolution of the guide pin 82 causes axial movement of the pressor piece 70 by means of the engagement of the guide pin 82 with the recess 76 in the pressor piece 70.
As best seen in FIGS. 7 and 9, the adjuster piece 86 is further internally provided with a tongue 90 which extends forwards. Axially extending grooves 92a, 92b and so on are formed in the inner surface of the tongue 90 at prescribed, preferably equal, intervals in the periphery direction. A projection 94 is formed on the outer surface of the main piece 52, which is adapted for snap engagement with any of the grooves 92a, 92b and so on.
As an alternative, like grooves may be made in the outer surface of the main piece 52 and a like projection on the inner surface of the tongue 90.
At a position corresponding to the flow rate indicator band 98 on the main piece 52, a radial opening 96 is formed through the adjuster piece 86 so that each flow rate indication is visible from outside. It will be well understood that the interval between adjacent grooves, e.g. 92a and 92b, should be equal to that between the adjacent flow rate indications.
The socket 50 shown in FIG. 7 is adapted for assembly with the plug 10 shown in FIG. 1.
In order to assemble the pipe coupling, the nose section 12 of the plug 10 is inserted into the fore conduit 54 of the socket 50, the conical flange 24 of the plug 10 depresses the ring section 64 of the latching piece 62 into the annular groove 66 provided by the mantle piece 58 and the tongue 69 of the main piece 52 flexes towards the axis of the pipe coupling being pressed by the latching piece 62. This procedure is substantially same as that shown in FIG. 6, in which the latching piece 62 is depressed by the finger F.
Further insertion of the plug 10 brings the latching groove 26 in the plug 10 to the position of the annular groove 66. Then, the ring section 64 of the latching piece 62 automatically slips into the latching groove 26 in the plug 10 due to the spring-back of the resilient tongue 69 of the main piece 52. Thus, the plug 10 and the socket 50 are firmly assembled together as shown in FIG. 10.
Under this condition, the flow rate is set to the highest level and the indication H appears in the radial opening 98 of the adjuster piece 86 as shown in FIG. 12. The center projection 74 of the pressor piece 70 is inserted into the fore conduit 38 of the plug 10 and pushes the valve 30 rearwards off the valve seat 34 by means of the front extension 42 while overcoming the replusion of the compression spring 28. Consequently, a folw passage is established through the pipe coupling, which includes the conduits 36, 37 and 38 of the plug 10, the clearance between the conical head of the valve 30 and the valve seat 34, the axial conduit 71 of the pressor piece 70, and the conduits 54 and 55 of the socket 50.
As described already, the flow rate of the fluid passing through the pipe coupling is set to the highest level in the situation shown in FIG. 10. Assuming that the groove 92a in FIG. 9 corresponds to the highest folw rate level, and the groove 92b the lowest flow level, i.e. the naught flow rate, the axial position of the pressor piece 70 changes as the adjuster piece 86 is axially turned about the main piece 52. That is, the pressor piece 70 moves rearwards as the adjuster piece 86 is turned from the position shown in FIGS. 9 and 10. With this turning of the adjuster piece 86, different flow rate indications appear in the radial opening 98 in the adjuster piece 96 so that an operator can recognize the flow rate to be selected. The above-described axial movement of the pressor piece 70 is caused by engagement of the guide pin 82 with the recess 76 in the pressure piece 70 by means of the helical guide slot 78 in the main piece 52, and by the pressure contact of the guide pin 82 with the adjuster piece 86.
Under the condition shown in FIG. 11, the projection 94 on the main piece 52 is in engagement with the groove 92d in the tongue 90 of the adjuster piece 86 and the flow rate is set to naught. Possibly an indication such as "L" may appear in the radical opening 96 in the adjuster piece 86. In this situation, the pressor piece 70 is registered at the rearmost position and, despite the contact between the pressor piece center projection 74 and the valve front extension 42, the valve 30 remains in contact with the valve seat 34. In other words, passage of the fluid through the pipe coupling can be blocked even retaining the assembled state of the pipe coupling.
When the tongue 68 of the latching piece 62 is depressed by the operators finger F under the condition shown in FIG. 11, the ring section 64 of the latching piece 62 is forced to fully sink in the annular groove 66 of the socket 50 off the latching engagement with the latching groove 26 in the plug 10 so that the pipe coupling can easily be disassembled.
For flow rate adjustment in the prior art, it is necessary to attach an additional flow rate adjuster such as a cock to the pipe coupling and this caused a complicated and enlarged construction of the pipe coupling and its related parts in the piping system.
In accordance with the present invention, the valve is provided with the dual functions, one blocking and opening of the flow passage and the other adjustment of the flow rate. Such dual functions are provided by the related mechanism fully encased within the pipe coupling itself. This greatly simplifies and minimizes the construction of the pipe coupling and its related parts in the piping system.
It should be well appreciated also that, in accordance with the present invention, the above-described flow rate adjustment is carried out whilst causing no disassembly of the pipe coupling. Only a simple finger action for axially turning the adjuster piece 86 enables such flow rate adjustment.
As the guide pin 82 is tightly pressed by the inner surface of the resilient adjuster piece 86, accidental movement of the guide pin 82 is well avoided. Further, frictional contact between the seal rings 72 on the pressor piece 70 and the wall defining the fore conduit 54 of the socket 50 also hinders unexpected movement of the guide pin 82. In other words, except for the intended finger action on the adjuster piece 86, selected flow rate can be retained without any unexpected change.
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A pipe coupling made up of separably assembled plug and socket in which a latching piece is suspensibly held in the socket in latching engagement with the plug so that finger pressure on the latching piece drives it out of the latching engagement in order to enable easy disassembly of the pipe coupling. A flow rate adjuster piece may be incorporated into the socket so that its axial turing changes the extent of recession of a valve off a valve seat in the plug so that the flow rate can be adjusted while retaining the assembled state of the pipe coupling. Light, compact and cheap construction is assured with simple operation and free flow rate adjustment.
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BACKGROUND OF THE INVENTION
The present invention concerns a clothes washing machine having a foldable cover assembly.
Generally, a washing machine is automatically controlled by a microcomputer programmed to wash and rinse clothes, to discharge water, and to extract water from the soaked clothes. Referring to FIG. 6, such a washing machine comprises a water reservoir (not shown) fixedly mounted in a housing 10 for storing a given amount of washing water, a washing basket 12 mounted in the water reservoir with a pulsator 11, and a drive means (not shown) for supplying a drive power required for washing operation.
The housing 10 has at the top a cover frame 13 with an opening 14 for loading and unloading clothes, a control panel 15 for controlling the washing machine, and a water supply hose 16. The cover frame 13 is provided with a hinged cover assembly 20 for closing or opening the top opening 14.
The cover assembly 20 comprises a first plate member 21 and a second plate member 22 to facilitate the opening and closing. The second member 22 is hinged to the rear side of the cover frame 13 while the first and the second member 21 and 22 are connected foldably with each other by means of a hinge 23. In addition, a depressed grip 24 is provided at the central outside part of the first member 21.
When loading or unloading clothes into or from the washing basket 12, the first member 21 is raised upwardly by means of the grip 24 so that the first and second members 21 and 22 are folded toward each other about the hinge 23 for opening the cover assembly 20. On the contrary, for closing the cover assembly 20, the first member 21 is pulled downward by means of the grip 24 so that the first and second members 21 and 22 are unfolded and extended about the hinge 23.
Such a conventional washing machine suffers a drawback that the leading end 21A of the first member 21 is forcibly dragged making a great friction with the surfaces of the cover frame 13 so that the frictional parts are greatly damaged together with generating great frictional noises.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a washing machine with a means for facilitating the movement of the cover assembly upon loading or unloading clothes into or from the washing basket.
It is another object of the present invention to provide a washing machine with a means for preventing wear due to frictional contact between the cover assembly and the cover frame.
According to the present invention, a clothes washing machine comprises a housing with a top opening for loading and unloading clothes, a washing basket rotating on a vertical shaft and mounted in the housing, a cover frame formed on the top opening, the cover frame having a pair of inclined guide surfaces, and a cover assembly with foldable first and second member attached to the cover frame for closing or opening the top opening, wherein one end of the first member is attached to one end of the second member by means of a hinge, with the other end of the second member hinged at one side of the cover frame, and the other end of the first member having a pair of roll means for respectively rolling on the pair of guide surfaces so as to move the cover assembly to the opening or closing position.
Preferably, each of the roll means comprises a roll with a shaft arranged in parallel with the hinge axes, and a bracket inserted in the cover assembly for rotatably mounting the roll.
The present invention will now be described with reference to the drawings attached only by way of example.
BRIEF DESCRIPTION OF THE ATTACHED DRAWINGS
FIG. 1 is a perspective view for illustrating the inner surface of the cover assembly of a washing machine according to the present invention;
FIG. 2 is an exploded perspective view of the part indicated by symbol `A` in FIG. 1;
FIG. 3 is a schematic side elevational view for illustrating the open state of the cover assembly according to the present invention;
FIG. 4 is a view similar to FIG. 3 for illustrating an intermediate stage of the movement of the cover assembly according to the present invention;
FIG. 5 is a view similar to FIG. 3 for illustrating the closed state of the cover assembly according to the present invention; and
FIG. 6 is a perspective view for illustrating a conventional washing machine.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring to FIGS. 1 and 2, there is shown a first member 21, of which the leading end 21A cooperates with the upper surfaces of a cover frame 13 and has a pair of roll devices 100. Each of the roll devices 100 includes a roll 30 and a bracket 40 for mounting the roll. The bracket 40 is inserted into a pocket 50 formed in the leading end 21A.
The roll 30 comprises a hub 31 made of a plastic material and a roll part 32 made of a rubber with length sufficient to cover the periphery of the yoke 31. The rubber absorbs the vibrations generated by the operation of the washing machine. The hub has a central shaft hole 33 for freely receiving a shaft 60.
The bracket 40 has a pair of support plates 41 for supporting both ends of the roll 30 by means of the shaft 60 fixedly mounted through a pair of holes 42. The holes 42 formed in the support plates are formed adjacent to the outer edges 41E of the support plates 41 so that the roll 30 is somewhat protruded outwardly beyond those edges 41E. The rear side of the bracket 40 has a locking aperture 43 for receiving a locking protuberance 51 formed in the pocket 50.
The roll 30 is rotatably mounted on the bracket 40 by means of the shaft 60 fixed in the holes 42 while the bracket 40 is mounted in the pocket 50 formed in the leading end 21A of the first member 21. The locking protuberance 51 is formed on the rear wall of the pocket 50 so as to be locked in the locking aperture 43 of the bracket 40. The roll 30 is protruded outwardly i.e., downwardly in FIGS. 3-5 from the leading end 21A of the first member 21 so as to properly contact a pair of guide surfaces 13L and 13R formed on the cover frame 13 when the first member 21 rotates around the hinge 23.
The guide surfaces 13L and 13R are ultilized for guiding the rolls so as to smoothly open or close the cover assembly 20. They are sloped downwardly toward the front portion of the washer from the position at which the roll devices 100 are disposed when the cover assembly 20 is completely opened as shown in FIG. 3. The rear ends of the guide surfaces 13L and 13R maintain a slope enabling the roll devices 100 to contact the guide surfaces.
In operation, when loading or unloading clothes into or from the washing basket 12, the first member 21 is raised upwardly by grasping the grip 24 in the closed position of the cover assembly 20 as shown in FIG. 5, so that the first and second members 21 and 22 are folded by means of the hinge 23 as shown in FIG. 4, and additionally the second member 22 is pivoted upwardly by means of the hinge 22A, thus completely opening the cover assembly 20 as shown in FIG. 3.
In this case, the leading end 21A of the first member 21 is smoothly guided by the cooperation of the rolls 30 and the guide surfaces 13L and 13R of the cover frame 13, so that no frictional noise or damage occurs as could be caused by direct contact between the leading end 21A and the cover frame 13.
For closing the cover assembly 20, the first member 21 is pulled downwardly by pulling on the grip 24 so that the first and second members 21 and 22 are unfolded away from each other, and additionally the second member 22 is pivoted downwardly on the hinge 22A, thus closing the cover assembly 20 as shown in FIG. 5. Likewise, the first member 21 is smoothly guided by the cooperation of the rolls 30 of the leading end 21A and the guide surfaces of the cover frame 13.
When the cover assembly 20 is completely closed , the rolls 30 are respectively inserted into cup-shaped depressions 13A formed at the front ends of the guide surfaces 13L and 13R, as shown in FIG. 5 so that the cover assembly 20 may be in close contact with the cover frame 13. Additionally, the edge between the cup-shaped depression and the guide surface is rounded so as to facilitate the movement of the roll 30 from or into the depression 13A.
Thus, the present invention provides various advantages such as preventing frictional damage to the cover assembly, reducing noises, facilitating the movement of the cover assembly, preventing distortion of the cover assembly, etc. Moreover, the rolls and brackets may be easily replaced when damaged.
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The leading end of the first member (21) of a cover assembly (20) is provided with rolls (30) in order to smoothly guide the cover assembly along sloped guide surfaces (13L and 13R), so that frictional damages are prevented as well as noises.
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FIELD OF THE INVENTION
The invention concerns a device for cleaning a reactor.
The invention concerns more precisely a device for plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit.
The invention concerns the method of cleaning a reactor implemented with the device according to the invention.
In general terms, the invention applies to reactors using dry methods and the walls of which are covered with undesirable deposits.
The invention applies to the cleaning of deposition and surface treatment reactors.
This is the case, for example, with PACVD (plasma-assisted chemical vapour deposition) and PAPVD (plasma-assisted physical vapour deposition) reactors or etching reactors, in methods acting on the etching-deposition balance selective SiO 2 etching with respect to silicon, anisotropic etching by lateral passivation).
The invention can also apply to CVD (silicon, tungsten), laser deposition or MBE (molecular beam epitaxy) reactors, the walls of which it is necessary to clean periodically to prevent redeposition or dust on the surfaces.
PRIOR ART
The problem of the cleaning of reactors in general, and deposition reactors in particular, assumes crucial importance in electronics, optics and micro-nanotechnology, but also in surface treatments (metal spraying, or deposition of hard, tribological or anticorrosion layers) in very many industrial sectors. The cleaning time and therefore the time for immobilisation of the production reactors represents a significant cost. Despite this cost, the cleaning of the reactors is a necessity for preserving quality and reproducibility for the processes implemented.
For this reason, in microelectronics, the trend is for periodic cleaning (every “n” deposition, or even after each deposition), usually by chemical cleaning by liquid or dry method (e.g. plasma). This is the case for example with the cleaning of reactors depositing Si, SiO 2 or Si 3 N 4 in reactors of the capacitive RF type (radio frequency discharge between two parallel electrodes). In this case, the equipment manufacturers have different strategies such as:
i) cleaning of the reactors in a liquid bath (wet, chemical method), but the time taken for dismantling and treating the reactor is prohibitive and requires two sets of treatment parts;
ii) plasma etching using gentle processes, that is to say by purely reactive dry chemical method.
For this reason, the majority of equipment manufacturers have developed reactor cleaning methods using auxiliary gas plasmas that are as reactive as possible vis-à-vis the deposits to be removed by reactive chemical method, and at relatively high pressure in order to produce the greatest possible concentrations of reactive species (for example atomic fluorine F for chemical etching of Si, SiO 2 , Si 3 N 4 or W, atomic oxygen O for the etching of carbon or polymers) and heating the walls in order to thermally activate the chemical etching reactions.
Thus it is possible to clean SiO 2 or Si 3 N 4 on walls of reactors covered with these deposits by raising them to 300° to 400° C. in the presence of an NF 3 plasma generated by inductive RF coupling or by surface wave). However, in general, this type of cleaning is possible only if stable volatile reaction products can be formed from the various elements of the deposit to be removed.
The dry cleaning techniques proposed above often have either often high cleaning times by purely chemical method, or high chemical aggressiveness on certain components of the reactor at high temperature (fluorine with nickel, oxygen with the dielectric insulators, and hence high cleaning cost.
They usually require the use of an auxiliary plasma source operating at a higher pressure than the plasma used for the process, and the choice of exotic gases or gases difficult to use, which also poses the problem of the cost of the gases (high flow rates), the retreatment of high gas volumes discharged from the reactor, and safety through the manipulation of dangerous gases (toxic, corrosive, flammable or explosive). An example of this is given in the document US 2005/0224458.
The investment and operating costs incurred by current techniques are therefore extremely high.
One objective of the invention is therefore to propose a cleaning device requiring only minor modifications to the reactor.
An objective of the invention is to propose a simplified cleaning method relying on plasma-assisted dry chemical etching methods, in particular using ion bombardment.
It is this ion bombardment that it is proposed to control in the invention.
SUMMARY OF THE INVENTION
To achieve these objectives, there is provided in the context of the present invention a method for the plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit on its walls and on at least one other biasable surface, characterised in that at least one sequence, referred to as a positive sequence, of cleaning the walls of the reactor was implemented by positive biasing of the or each biasable surface, with respect to the walls of the reactor, the walls being at a referenced potential.
The method according to the invention can also have at least one of the following characteristics:
at least one other sequence is implemented, referred to as a negative sequence, for cleaning the or each biasable surface by negative biasing thereof, with respect to the walls of the reactor; a negative sequence followed by a positive sequence is implemented; at least one alternating succession of a positive sequence and a negative sequence is implemented; a plurality of periodic alternating successions of a positive sequence and a negative sequence are implemented; a biasing to referenced voltage of the or each biasable surface is implemented during the positive sequence; a biasing to referenced voltage of the or each biasable surface is implemented during the negative sequence; an auto-biasing of the or each biasable surface is implemented during the negative sequence.
To achieve these objectives, there is also provided in the context of the present invention a device for the plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit on its walls and on at least one other biasable surface, characterised in that it comprises means for positively biasing, with respect to the walls of the reactor maintained at a referenced potential, the or each biasable surface.
The device according to the invention can also have at least one of the following characteristics:
it comprises means for negatively biasing, with respect to the walls of the reactor, the or each biasable surface; it comprises means for successively alternating the sign of the biasing, with respect to the walls of the reactor, of the or each biasable surface; it comprises a DC voltage generator, electrically connected to the or each biasable surface, and means of controlling the generator for successively delivering positive and negative voltages, with reference to the walls of the reactor; it comprises means for successively and periodically alternating the sign of the biasing, with respect to the walls of the reactor, of the or each biasable surface; it comprises a periodic voltage generator, connected electrically to the or each biasable surface by means of a circuit comprising a low-impedance capacitor and means for short-circuiting the capacitor; it comprises a periodic voltage generator, in direct electrical connection with the or each biasable surface and referenced with respect to the walls of the which are preferably earthed.
BRIEF DESCRIPTION OF THE DRAWINGS
Other characteristics, aims, advantages and objectives of the present invention will emerge from a reading of the following detailed description, and with regard to the accompanying drawings, given by way of non-limitative examples and on which:
FIG. 1 depicts by or example DC voltages applied to at least one biasable surface of a reactor, according to the two types of sequence, with respect to the referenced wall potential V w ;
FIG. 2 depicts, by way of example, a periodic voltage signal V(t) supplied to at least one biasable surface, during a sequence referred to as sequence 1 or negative sequence, in which the biasable surface auto-biases negatively with respect to the referenced potential of the walls V w ;
FIGS. 3 a and 3 b depict, by way of examples, periodic voltage signals supplied and applied to at least one biasable surface, during a sequence referred to as sequence 2 or positive sequence, in which the biasable surface periodically has a positive potential with respect to the referenced potential of the walls V w ;
FIG. 4 depicts, by way of example, a period voltage signal supplied and applied to at least one biasable surface, in which the biasable surface periodically has a positive and negative potential respect to the referenced potential of the walls V w ;
FIGS. 5, 6, 7 and 8 depict schematically different variant embodiments of a device according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
The method according to the invention is a plasma-assisted chemical etching cleaning method.
This can use plasma etching methods conventional in microelectronics and microtechnologies, such as for example:
i) etching of carbon C or carbon compounds (DLC, polymers, etc) by plasmas containing oxygen,
ii) etching of silicon Si or tungsten W by plasmas based on fluorine (SF 6 , CF 4 , NF 3 , etc),
iii) etching of SiO 2 or Si 3 N 4 by plasmas based on fluorine (SF 6 , CF 4 , NF 3 , etc),
iv) etching of Al, B or other compounds by plasmas based on bromine or chorine (Br 2 , Cl 2 , HBr, etc).
So that the cleaning method according to the invention can be implemented, it is necessary for the plasma to be produced in a reactor with walls at referenced potentials (for example earthed).
The cleaning operation comprises at least one cleaning sequence (by plasma etching) in which the walls of the reactor are cleaned by positive biasing, with respect to the walls of the reactor, of the or each biasable surface (for example substrate carrier or electrode). This sequence or sequences are called sequence 2 or positive sequence in the remainder of the description.
The operation comprises, according to the application, at least one other sequence of cleaning the or each biasable surface (for example substrate carrier and/or electrode) by negative biasing of the biasable surface with respect to the walls of the reactor. This sequence or sequences are called sequence 1 or negative sequence in the remainder of the description.
Cleaning of a Conductive Deposit
If the deposit to be cleaned is conductive (C, W, Si etc) and the biasable surface does not need to be cleaned (because its disposition within the reactor for example, or because it carries a substrate during the deposition operations, or because the deposit is considered to be negligible), a sequence 2 may suffice: there is then complete cleaning of the walls of the reactor (chamber) by application to the biasable surface (substrate carrier or electrode) of a positive DC voltage with respect to the walls.
If the deposit to be cleaned is conductive (C, W, Si etc) and the biasable surface is also to be cleaned, two successive sequences only may suffice, namely a sequence 1 and a sequence 2 : there is then complete cleaning of the biasable surface by application to this surface (substrate carrier or electrode) of a negative DC voltage with respect to the walls (for example earthed) and the complete cleaning of the walls of the chamber by application to the surface (substrate carrier or electrode) of a positive DC voltage with respect to the walls.
Reference can be made to FIG. 1 , where the voltage V(t) supplied to the biasable surface and to which it is raised changes from a sequence 1 , referenced 1 , to a sequence 2 , referenced 2 , and where V w is the potential of the walls of the reactor.
Note that, in the context of the invention, it is of little importance whether sequence 1 is carried out followed by sequence 2 or vice versa. However, in practice, it is more suitable to commence with sequence 1 , that is to say to carry out the cleaning of the biasable surface.
The biasable surface (substrate carrier or electrode) can be small compared with the surface of the calls to be cleaned but must have a sufficiently large size to disturb the plasma, so that the potential of the plasma V p is positioned, at each moment t, at a value that is always more positive than the most positive surface (wall or electrode).
The condition to be fulfilled for constituting a substrate carrier or a large-size electrode is that the ratio of the surface S s of the substrate carrier or large-size electrode to the surface S w of the walls is at least greater than approximately 1.5 times the square root of the ratio of the mass m e of the electrons to that of the ions m i , that is to say:
S s /S w >1.5( m e /m i ) 1/2 (1)
For argon, it is therefore necessary for the ratio to be greater than 1/180 (1/30 for hydrogen and 1/500 for xenon), which is generally the case with substrate carriers or electrodes used in microelectronics or in surface treatments by furnace.
Below the ratio given by equation (1), the surface S s does not disturb the plasma, which corresponds to the case of electrostatic probes or Langmuir probes. In this case, the plasma potential V p remains practically unchanged compared with the potential of the walls (generally earthed) if the biasable surface of the surface S s is positively biased with respect to the potential V w of the walls. The ion bombardment energy W w of the walls of the reactor is then close to:
W w ≈e ( V p −V f )=( kT e /2)[1+In( m i /2 πm e )] (2)
where k is Boltzmann's constant, e the charge on the electron, T e is the electron temperature and V f the potential of the biasable surface which is floating, then equal as a first approximation to the potential of the walls (V f ≈V w ).
On the other hand, in the general case that interests us here, that of a ratio S s /S w higher than the value given by equation (1), the biasable surface S s profoundly disturbs the equilibrium of the plasma if it is raised to a positive potential V 0 with respect to the potential of the walls V w (sequence 2 ). In this case, the plasma potential V p is offset by the value V 0 −V w and the ion bombardment energy V w of the walls is, as a first approximation, for a DC voltage V 0 , equal to:
W w ≈e ( V p −V w )= e ( V p −V f +V 0 −V w ) (3)
In other words, by positively biasing the biasable surface S s so the DC potential V 0 with respect to the potential of the walls V w (sequence 2 ), it is possible to adjust to the required value the ion bombardment energy on the walls during sequence 2 . During this sequence, the ion bombardment energy W s of the electrode is equal to:
W s ≈e ( V p −V f ) (4)
If now the surface S s is negatively biased to the DC potential −V 0 with respect to the potential of the walls V w (sequence 1 ), the ion bombardment energy W s of the surface S s is equal to:
W s =e ( V p −V s )= e ( V p −V f +V w −V 0 ) (5)
while the ion bombardment energy W w of the walls during this same sequence is equal to:
W w =e ( V p −V f ) (6)
It can be seen therefore that the bombardment energies of the walls and large-size electrode are reversed when changing from sequence 1 to sequence 2 .
In the case of the cleaning of a conductive deposit, on the walls of the reactor and on at least one other biasable surface of the reactor, it is therefore possible to clean the reactor in two stages:
cleaning of the large-sized biasable surface (substrate carrier or electrode) during sequence 1 by adjusting the energy of the ion bombardment W s by means of the value −V 0 of the DC voltage applied to the large-sized biasable surface ( FIG. 1 ), and cleaning of the walls of the reactor during sequence 2 by adjusting the energy of the ion bombardment W w by means of the value +V 0 at the DC voltage applied to the large-sized electrode ( FIG. 1 ).
This is because, since the rate of chemical etching caused by the ion bombardment increases rapidly with the energy, a method of rapid cleaning of the reactor requires a more energetic con bombardment than that due solely to the difference between plasma potential and floating potential of the biasable surface.
In equations (3) and (5) and in FIG. 1 , +V 0 and −V 0 are opposite values, but nothing makes it necessary to take symmetrical biasing values V 0 . However, as it is preferable to remain below or close to the values of the sputtering thresholds of the reactor, it is more convenient to choose symmetrical values as in the previous example, with typically V 0 =30 to 100 V.
As mentioned above, a sequence 2 or a succession of a sequence 1 and a sequence 2 may suffice according to circumstances. However, if the cleaning of the walls contaminates the large-sized biasable surface, or vice versa, it is preferable to provide is certain number of alternating sequences until there is complete cleaning of the reactor (walls and large-sized biasable surface).
It should be noted that, in the case where the substrate carrier is used as a large-sized electrode, some parts concealed by the substrate may prove to be free of deposit. In fact the deposit may affect solely the edges of the substrate carrier but in this case it is preferable to clean the whole of the substrate carrier (sequence 1 ).
Cleaning of an Electrically Insulating Deposit
If the deposit to be cleaned is insulating (SiO 2 , Si 3 H 4 , etc) and the biasable surface does not need to be cleaned (no insulating deposit), a sequence 2 may suffice.
In the general case, it is however essential to apply a succession of periodic alternating sequences comprising the two sequences described previously:
partial cleaning of the biasable surface (substrate carrier or electrode) during the negative half wave with respect to the walls (generally earthed) of a periodic voltage applied to the biasable surface, and partial cleaning of the walls during the positive half wave (with respect to the walls) of a periodic voltage applied to the biasable surface.
These sequences are applied until there is complete cleaning of the reactor.
Here also, it should be noted that, in the context of the invention, it is of little importance whether sequence 1 is carried out followed by sequence 2 or vice versa. However, in practice, it is more suitable to commence with sequence 1 , that is to say to carry out the cleaning of the biasable surface.
Here also, the ratio of the surface areas of the biasable surface and the walls of the reactor must comply with equation (1).
The periodic voltage of frequency f 0 , supplied for example by a periodic voltage generator, is referenced with respect to the potential of the walls of the reactor (generally earthed), which is not in principle the case with the biasable surface (auto-biasing mode is thought of).
This is because, in the case of the cleaning of an insulating deposit, it is no longer possible to clean the reactor with alternating DC biasing voltages ( FIG. 1 ), and it is therefore necessary to have recourse to periodic biasing to a higher frequency by capacitive effect.
Thus, during a first sequence (sequence 1 or negative sequence) of the periodic biasing, it is usual to carry out negative auto-biasing of the biasable surface (substrate carrier or large-sized electrode) by applying a periodic voltage to the biasable surface through a low-impedance capacitor (the current case of RF auto-biasing) and therefore to clean the large-sized biasable surface by chemical etching assisted by ion bombardment (plasma).
During this sequence 1 , an adapted means therefore supplies a periodic voltage signal V(t) (such as the one illustrated in FIG. 2 ) to the biasable surface which, for its part, biases itself (auto-biasing) so that it receives, during a period, as many positive charges (ions) as negative charges (electrons) having regard to the voltage values taken by this signal and that of the plasma potential.
This auto-biasing results from the non-linearity of the current/voltage characteristic of the plasma.
Once the biasable surface (substrate carrier or electrode) is clean, the invention consists of applying to it, during a second sequence (sequence 2 or positive sequence), a periodic voltage referenced (for example to the potential of the walls, generally earthed) so that the voltage applied to the biasable surface during the positive half wave takes a positive value +V 0 with respect to the potential of the walls.
Examples of periodic voltage signals supplied by a means adapted to the biasable surface are illustrated on FIG. 3 a and FIG. 3 b . On FIG. 3 a , the signal supplied by the adapted means is that carried by the biasable surface. On the other hand, on FIG. 3 b , the signal supplied by the adapted means is carried to the biasable surface solely when V>V w (sequence 2 ), the biasable as therefore “sees” the same signal as at FIG. 3 a.
In other words, it is thus possible to clean the biasable surface during sequence 1 by plasma assisted chemical etching and to clean the walls of the reactor in the same way during sequence 2 .
According to a variant of the invention, a periodic voltage referenced (for example to the potential of the walls, generally earthed) is applied to the biasable surface so that the voltage applied to the biasable surface during the negative half waves (sequences 1 ) takes a negative value −V 0 with respect to the potential of the walls, and so that the voltage applied during the positive half waves (sequences 2 ) takes a positive value +V 0 with respect to the potential of the walls ( FIG. 4 ).
In this variant, it will be understood that there is no longer any negative auto-biasing of the biasable surface (except as long as there remains an insulating deposit). To do this, the low-impedance capacitor is short-circuited ( FIG. 6 ) so that the voltage supplied by adapted means corresponds to the voltage carried to the biasable surface.
Compared with the case of cleaning by successive applications of DC voltages, the auto-biasing values calculated in the case of the application of periodic voltages are more complex than in equations (2) to (6) presented above and depend more or less greatly on the angular velocity ω 0 =2π f 0 (with respect to the ion plasma angular velocity), the shape of the periodic signal or the ratio of the surfaces S s and S w .
It should be noted however that the angular velocity ω 0 of the cleaning sequences is not a limitative given of the method. In particular, this angular velocity may be smaller or greater than the ion plasma angular velocity ω pi defined by ω pi 2 =n e 2 /∈ 0 m 1 where n is the density of the plasma, −e the charge on the electron, m i the mass of the ions of the plasma and ∈ 0 the permittivity of the vacuum.
It should also be noted that the shape of the periodic signal (the succession of periodic alternating sequences) may be sinusoidal, rectangular or other.
However, the values calculated in equations (2) to (6) are in practice valid in the case of the application of rectangular signals or periodic angular velocity voltages ω 0 <<ω pi and highly asymmetric surfaces S s and S w .
It should also be noted that the method of cleaning by the application of periodic voltages as described above make sense only if the ratio of the surfaces S s and S w is small (S s /S w <<1). This is because, if the surfaces S s and S w are close dimensions (S s ≈S w ), a single auto-biasing sequence suffices since the biasing of the two surfaces is then symmetrical with respect to the signal applied, each surface being in turn biased negatively with respect to the plasma potential.
The cleaning by the succession of periodic alternating sequences presented above when the deposit to be cleaned is insulating may also be applied to the cleaning of conductive deposits. However, the cleaning of conductive deposits in two or more sequences under DC voltage procures the advantage of not requiring a periodic voltage generator, much more expensive that a DC supply.
As mentioned above and as far as possible, the voltages applied (whether the deposit be conductive or insulating) must be adjusted so that the ion bombardment energy of the electrode or walls of the reactor remains below or close to the sputtering threshold of the materials that make them up (negligible sputtering of the electrode and walls of the reactor) that is to say typically below 100 eV.
The method according to the invention described above is implemented with means detailed below.
More precisely, the cleaning devices according to the invention comprise, and this in a manner known in the plasma assisted dry chemical cleaning devices, means of producing, in a reactor, a reactive plasma capable of forming volatile reaction products with the deposits to be removed.
These means also comprise a biasable surface (substrate carrier or electrode) of surface area S s sufficient with respect to the surface area S w of the walls [equation (1)] to allow modification of the plasma potential. The biasable surface is then said to be of large size.
These means also comprise means of applying to the large-size biasable surface excessive biasing sequences using DC or periodic voltages according to the method of the invention.
Different devices according to the invention can be described. In particular, the plasma production means can consist of different types of plasma such as microwave plasmas for example distributed electron cyclotron resonance (DECR) plasmas, multi-dipole plasmas (non-limitative examples), such as continuous or radio-frequency capacitive discharges, diodes or triodes, where one of the electrodes is used as a biasable substrate carrier, or such as inductive discharges with inductor internal to the chamber. In all these examples, the substrate holders generally comply with the criterion of surface area ratio of equation (1).
With regard to the application of successive sequences of DC voltages (solely for conductive deposits), a controlled supply capable of successively delivering positive and negative continuous voltages, is necessary.
For application of a periodic negative auto-biasing voltage (sequence 1 , insulating deposit), a conventional means consists of a generator capable of delivering a periodic voltage through a low-impedance capacitor.
On the other hand, obtaining a positive biasing voltage during the positive half wave (sequence 2 , insulating deposit) requires a generator capable of delivering a periodic voltage referenced with respect to a defined potential.
In other words, the invention requires, in very many cases, a generator capable of successively delivering either a periodic voltage through a low-impedance capacitor (biasing of the substrate during the method preceding the cleaning and/or during sequence 1 ), or a referenced periodic voltage having during the positive half wave (sequence 2 ) a positive voltage with respect to the potential of the wall.
According to the variant embodiment mentioned above in the context of the method (sequence 1 , insulating deposit), a device according to the invention will then have to require a generator capable of delivering a periodic voltage referenced with respect to the wall, that is to say having a periodically negative and then positive voltage, symmetrical for example with respect to the potential of the wall.
Thus a first device comprises means of applying DC voltages that are negative and positive, with reference to the walls of the reactor, to a biasable surface (a substrate carrier for example), and this independently or not of the production of the plasma.
This first device is illustrated in FIG. 5 . It has a reactor 10 referenced to earth 11 , a biasable surface 12 electrically connected by a means 13 to a DC voltage generator 14 , comprising means of controlling the generator in order to successively deliver positive and negative voltages, with reference to the walls of the reactor.
A second device ( FIG. 6 ) comprises a periodic voltage generator 140 , electrically connected to the or each biasable surface 12 by means of a circuit 15 comprising a low-impedance capacitor 151 and means 152 for short-circuiting the capacitor. With this device, the biasing of the biasable surface takes place independently or not of the production of the plasma.
The short-circuiting means 152 may for example, but non-limitatively, be formed by a switch, disposed in parallel to the low-impedance capacitor. In this case, the switch is open during a sequence 1 ( FIG. 6 and FIG. 2 ), so that the voltage generated by the generator passes through the capacitor before arriving at the or each biasable surface. On the other hand, the switch is closed for a sequence 2 , so that the voltage generated by the generator is the voltage of the or each biasable surface ( FIG. 3 a and FIG. 3 b ).
A third device comprises means of applying a periodic voltage, for example by a periodic voltage generator 141 , to the or each biasable surface 12 , by means of a direct electrical connection 13 ( FIG. 7 ). This voltage is referenced to the potential of the walls of the reactor (generally earthed), and this independently or not of the production of the plasma.
It should be noted that, in the case of capacitive discharges between electrodes, the biasing is not independent of the production of the plasma, whereas it is generally so in inductive plasmas and microwave plasmas.
One of the main advantages of the invention is its simplicity in terms of the method and device compared with current techniques.
This is because the sequence 1 or negative sequence mentioned in the description above uses known plasma-assisted etching methods in so far as the or each biasable surface is negatively biased with respect to the plasma potential (which is slightly greater than the potential of the walls).
The sequence 2 or positive sequence, for its part, therefore modifies the nominal functioning of the reactor in order to achieve an objective of cleaning the walls of the reactor, which are for this purpose put to a referenced potential.
For certain types of applications known to persons skilled in the art, use is made, in addition to a cathode (which constitutes a biasable surface) negatively biased with respect to the plasma potential, at least one anode intended to collect the electrons, which is, in nominal functioning, biased positively with respect to the plasma potential.
However, in this type of application and in order to avoid insulating deposits on this anode or these anodes, means are provided for negatively biasing the anode or anodes with respect to the plasma potential (the walls are not referenced in this type of application). This method, which can be likened to a sequence 1 as described above from the point of view of the anode or anodes, is implemented for the purpose of ensuring continuity of nominal functioning of the reactor, by ensuring that the anode fulfills its role of electron collector. This is the case for example with the document EP 1 458 006.
Among the advantages that the invention procures, it can in particular be mentioned that it:
1) implements conventional etching methods, tried and tested and well mastered;
2) does not require any modification to the reactor architecture;
3) requires only minor modifications to the biasing supplies for the biasable surface (substrate carrier or electrode);
4) does not cause any sputtering of the biasable surface if the biasing thereof is independent of the production of the plasma (for example plasmas produced by microwaves), and is maintained at a value less than that corresponding to the sputtering of the surfaces of the reactor;
5) offers a method that is scarcely damaging for the reactor or the environment.
To give a clear idea, the applicant supplies below an example of a typical application of its invention, given by way of non-limitative example.
A capacitive discharge is considered in a reactor 10 connected to earth 11 created between a biasable surface 12 (a substrate carrier) to which a voltage is applied and an earthed electrode 15 ( FIG. 8 ) or also a reactor of the same dimensions in which the plasma is produced by microwaves and where the same substrate carrier can be biased by a voltage. The element 16 corresponds, according to the type of voltage generated, to the generator 14 in FIG. 5 , to the assembly formed by the generator 140 and the circuit 15 in FIG. 6 , or to the generator 141 in FIG. 7 .
The ratio of the earthed surfaces and those biasable continuously or periodically (RF) is 700 cm 2 /7000 cm 2 , that is to say 1/10, which perfectly corresponds to the criterion defined by equation (1) and to the case of a substrate-carrier surface that is small compared with the surface of the walls.
A well known example is the removal of the deposits of SiO 2 on the walls of a deposition reactor. In the context of the invention, this deposit can be removed by means of an SF 6 plasma by the formation of the reaction products SiF 4 and O 2 by chemical etching assisted by ion bombardment. It should be noted that the use of CF 4 , and more generally fluorocarbon gases, may, according to the plasma parameters, lead to a CF x deposit of the Teflon type.
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The invention concerns a device and a process, the device being a cleaning device utilizing a dry chemical means assisted by plasma from a reactor ( 10 ) containing an unwanted deposit on its walls and at least one other polarizable surface ( 12 ), characterized in that it comprises means ( 13, 14 ) for positively polarizing one or each of the polarizable surfaces relative to the reactor walls maintained at a reference potential.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. patent application Ser. No. 13/544,468, filed on Jul. 9, 2012, which claims priority to U.S. Pat. No. 8,218,846 filed May 14, 2009, which claims priority to U.S. Provisional Patent Application No. 61/053,523, filed May 15, 2008, each of which is entitled Automatic Pathway And Waypoint Generation And Navigation Method and is hereby incorporated by reference.
BACKGROUND
[0002] Breakthrough technology has emerged which allows the navigation of a catheter tip through a tortuous channel, such as those found in the pulmonary system, to a predetermined target. This technology compares the real-time movement of a locatable guide (LG) against a three-dimensional digital map of the targeted area of the body (for purposes of explanation, the pulmonary airways of the lungs will be used hereinafter, though one skilled in the art will realize the present invention could be used in any body cavity or system: circulatory, digestive, pulmonary, to name a few).
[0003] Such technology is described in U.S. Pat. Nos. 6,188,355; 6,226,543; 6,558,333; 6,574,498; 6,593,884; 6,615,155; 6,702,780; 6,711,429; 6,833,814; 6,974,788; and 6,996,430, all to Gilboa or Gilboa et al.; U.S. Published Applications Pub. Nos. 2002/0193686; 2003/0074011; 2003/0216639; 2004/0249267 to either Gilboa or Gilboa et al; as well as U.S. patent application Ser. No. 11/939,537 to Averbuch et al. All of these references are incorporated herein in their entireties.
[0004] Using this technology begins with recording a plurality of images of the applicable portion of the patient, for example, the lungs. These images are often recorded using CT technology. CT images are two-dimensional slices of a portion of the patient. After taking several, parallel images, the images may be “assembled” by a computer to form a virtual three-dimensional model of the lungs.
[0005] The physician then takes this virtual model and, using the software supplied with the navigation system, plans a path to the target. Planning the path to the target involves creating a patient file and selecting and saving various waypoints along the path to the target. The physician also selects and saves various registration points used by the software to register the virtual model to the actual patient in the upcoming procedure.
[0006] Typically, there is only one path that leads to the target, unless the target is very large. In the airways and vasculature of the body, the body lumina do not split and then rejoin downstream. The branches of a tree provide a good analogy: for any given leaf on a tree, there is only one combination of branches that lead to that leaf. Hence, the step of pathway planning is a time-consuming step that would be avoided if automated.
[0007] Additionally, the present systems provide guidance to the target, but not necessarily to the waypoints along the way. Instead of focusing on the target, it would be advantageous to provide navigation guidance to each of the intermittent waypoints, thereby treating each successive waypoint as a target, then, after the waypoint is reached, changing the target to the next waypoint.
SUMMARY
[0008] In view of the foregoing, one aspect of the present invention provides a system and method for automatically planning a pathway from an entry point in a patient to a target through a luminal network.
[0009] Another aspect of the present invention automatically generates the various waypoints between a starting point and the target.
[0010] Another aspect of the present invention provides a system and method for providing navigational cues to a target via the plurality of waypoints. The cues are provided in such a manner that the next waypoint in a path is automatically detected and treated as a destination. Navigational cues are provided to that waypoint until it is reached. The system then selects the next waypoint along the path and provides navigational cues to that waypoint. This continues until the actual target is reached.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 is a flowchart describing a general step of a method of the present invention;
[0012] FIG. 2 is a flowchart describing a general step of a method of the present invention;
[0013] FIG. 3 is a flowchart describing a general step of a method of the present invention;
[0014] FIG. 4 is a user interface of an embodiment of the system of the present invention; and
[0015] FIG. 5 is a user interface of an embodiment of the system of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0016] Generally, the present invention includes a system and method for constructing, selecting and presenting pathway(s) to a target location within an anatomical luminal network in a patient. The present invention is particularly, but not exclusively, suited for guiding and navigating a probe through the bronchial airways of the lungs. The present invention includes a preoperative and an operative component. The preoperative component is conducted prior to navigation and can be categorized as “Pathway Planning.” The operative component is conducted during navigation and can be categorized as “Navigation.”
[0017] Pathway Planning
[0018] The pathway planning phase includes three general steps, each of which is described in more detail below. The first step involves using a software graphical interface for generating and viewing a three-dimensional model of the bronchial airway tree (“BT”). The second step involves using the software graphical interface for selection of a pathway on the BT, either automatically, semi-automatically, or manually, if desired. The third step involves an automatic segmentation of the pathway(s) into a set of waypoints along the path that can be visualized on a display. It is to be understood that the airways are being used herein as an example of a branched luminal anatomical network. Hence, the term “BT” is being used in a general sense to represent any such luminal network, and not to be construed to only refer to a bronchial tree, despite that the initials “BT” may not apply to other networks.
[0019] First Step—BT Generation
[0020] Referring now to FIG. 1 , there is shown a flowchart describing the first step—using a software graphical interface for generating and viewing a BT. At 20 , the first step begins with importing CT scan images, preferably in a DICOM format, into the software. The data may be imported into the software using any data transfer media, including but not limited to CDs, memory cards, network connections, etc.
[0021] At 22 the software processes the CT scans and assembles them into a three-dimensional CT volume by arranging the scans in the order they were taken and spacing them apart according to the setting on the CT when they were taken. The software may perform a data fill function to create a seamless three-dimensional model.
[0022] At 24 , the software uses the newly-constructed CT volume to generate a three-dimensional map, or BT, of the airways. The three dimensional map can either be skeletonized, such that each airway is represented as a line, or it may be include airways having dimensions representative of their respective diameters. Preferably, when the BT is being generated, the airways are marked with an airflow direction (inhalation, exhalation, or separate arrows for each) for later use during the pathway generation step. It is envisioned that this step is optional. The CT volume may be used as it is.
[0023] At 26 , the software displays a representation of the three-dimensional map on a user interface, such as a computer monitor.
[0024] Second Step—Pathway Selection
[0025] Referring now to FIG. 2 , there is shown a flowchart describing the second step—using the software graphical interface for selection of a pathway on the BT. At 40 , the second step begins with a determination, by the software, of an appropriate pathway to a selected target.
[0026] In one embodiment, the software includes an algorithm that does this by beginning at the selected target and following lumina back to the entry point. Using the airways as an example, the target is first selected. The software then selects a point in the airways nearest the target. If the point closest to the target is in an airway segment that is between branches, the software has to choose between two directional choices. If the airways of the BT were marked with airflow direction, the software moves in the opposite direction of the arrows, thereby automatically generating a pathway to the entry point.
[0027] Alternatively, the pathway to the target may be determined using airway diameter. Moving toward the entry point (the trachea) results in an increased airway diameter while moving distally results in a decreased airway diameter. Hence, the software could choose to move in the direction of increased airway diameter. If the point closes to the target is in an airway segment that includes one or more branches, the choices are more numerous but the following the path of the greatest increase in airway diameter will still result in the correct path to the entry point.
[0028] Though unlikely, in the event that an incorrect path is taken, the software would eventually detect an inevitable decrease in diameter, if this is the case, the software would automatically abort that path and revert to the last decision-making point. The algorithm will resume, blocking off the incorrect path as an option.
[0029] At 42 , after the pathway has been determined, or concurrently with the pathway determination, the suggested pathway is displayed for user review. Preferably, the entire BT will be displayed with the suggested pathway highlighted in some fashion. The user will have zoom and pan functions for customizing the display.
[0030] At 44 , the user is given the opportunity to edit and confirm the pathway. There may be reasons an alternative pathway is desirable. For example, though the targeted lesion is closest to a particular airway, there may be an artery or a lobe division between the selected airway and the target. Hence, it is important to provide the user with editing ability.
[0031] Third Step—Waypoint Selection
[0032] Referring now to FIG. 3 , there is shown a flowchart describing the third step—using the software to automatically generate waypoints. At 60 , the third step begins by designating each of the decision making points from 40 of step 2 as waypoints. This may happen concurrently with 40 . Each time the software, while navigating backwards toward the trachea, was presented with navigational choices, the user navigating toward the target will necessarily also be presented with choices. Hence, it is logical to designate those decision-making points as waypoints along the path to the target.
[0033] At 62 , the waypoints appear on the suggested pathway, and may be labeled in such a way as to distinguish them from each other. For example, the waypoints may be numbered, beginning at 1, in the order that they appear. Preferably, the waypoints are positioned just downstream of each bifurcation, instead of at the bifurcation. In this way, providing navigation directions to the waypoint results in the probe being positioned in the appropriate airway once the waypoint has been reached. Hence, the physician can begin navigation to the next waypoint by simply advancing the probe without being concerned about advancing down an incorrect airway.
[0034] At 64 , the user is given the opportunity to edit the waypoints. It is understood that the second and third steps may occur concurrently. If the user is editing the pathway to the target, the user will also be selecting alternative waypoints, as one in the art will realize.
[0035] Fly-Through Feature
[0036] In addition to the editing features described above, the software presents a “fly-through” feature that presents the user with the opportunity to view the user interface as it would appear from start to finish if the procedure was performed as planned. A preferred embodiment of one view the user interface is shown in FIG. 4 .
[0037] The interface 80 is divided into four quadrants, 82 , 84 , 86 and 88 . The upper-left quadrant 82 is a lateral view of the CT volume of the lungs, i.e. as though looking parallel to the spine of the patient. The lower-left quadrant 84 is a birds-eye view of the CT volume of the lungs. The upper-right quadrant 86 is a side view of the CT volume of the lungs. The lower-right quadrant 88 is a three-dimensional perspective view inside a virtual airway of the BT. Cross-hairs 90 span over all of the quadrants to show the present location of the LG. The cross-hairs 90 in quadrant 88 are shown in a perspective format.
[0038] Navigation
[0039] The heading “Navigation” refers to the processes occurring during the actual procedure. Referring now to FIG. 5 , there is shown a user interface 100 that assists the user in navigating to the target. This view of the user interface 100 includes four quadrants 102 , 104 , 106 , and 108 . The images shown in each quadrant are preferably customizable. Hence, any of the aforementioned views from interface 80 may be displayed. However, pertinent to the navigation discussion is the view shown in the lower-right quadrant 108 .
[0040] Quadrant 108 is shown as displaying an LG steering indicator. The destination 110 appears as a circle which floats over the quadrant 108 and moves when the LG is turned. The destination 110 represents the next waypoint to which the user is navigating, or the final destination (targeted lesion) in the event that the last waypoint has been passed.
[0041] When the distal tip of the LG is pointing directly at the destination 110 , the destination 110 appears in the center of the circle 112 . If the LG is not pointing directly at the destination 110 , the destination 110 is located in a representative location in or out of the circle 112 . For example, if the LG is pointing down and right of the destination 110 in the body (in other words, the destination 110 is above and left of where the LG is pointing), the destination 110 on the display in quadrant 108 will appear above and left of the center of the circle 112 . If the LG is deflected away from the destination 110 far enough, the destination 110 may not even appear in the quadrant 108 . For this reason, a guide arrow 114 appears somewhere on the circle 112 . The guide arrow 114 tells the user which direction the LG must be deflected to align the tip with the destination 110 .
[0042] Although the invention has been described in terms of particular embodiments and applications, one of ordinary skill in the art, in light of this teaching, can generate additional embodiments and modifications without departing from the spirit of or exceeding the scope of the claimed invention. Accordingly, it is to be understood that the drawings and descriptions herein are proffered by way of example to facilitate comprehension of the invention and should not be construed to limit the scope thereof.
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A navigation system for use in a luminal network of a patient, such as the airways, that is able to analyze a three-dimensional model of the luminal network and automatically determine a pathway from an entry point to a designated target. The system further automatically assigns waypoints along the determined pathway in order to assist a physician in navigating a probe to the designated target.
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BACKGROUND OF THE INVENTION
This invention relates to an exhaust gas control means, and more particularly, to an exhaust gas control means for vehicles such as motorcycles.
It is well known that the design of the exhaust system for an internal combustion engine can significantly affect the engine performance. With multiple cylinder engines, it is a practice to employ individual exhaust pipes that extend from the individual exhaust ports of the engine and which merge into a common expansion or collector chamber for improving top end performance. Although the use of an expansion or collector chamber for this purpose is effective increasing maximum output of the engine, it has been found that the chamber can contribute to poor running under other than maximum speed conditions. This is a result of the reflection of the exhaust gas pulses from one cylinder back to another cylinder during these running conditions. These pulsations transferred back into the exhaust parts of another cylinder tend to reduce the breathing ability of the engine at lower running speeds and, as noted, adversely affects the output of the engine.
In order to improve the efficiency of the engine and its output at all running conditions, it has been proposed to incorporate a reflective valve means in the individual exhaust pipes upstream of the expansion or collector chamber. Such an arrangement is shown in the co-pending applications entitled "High Performance Exhaust System for Internal Combustion Engine", by Hideaki Ueda, Ser. No. 935,340, filed Nov. 26, 1986, and "High Performance Exhaust System For Internal Combustion Engine", by Hideaki Ueda, Ser. No. 935,342, filed Nov. 26, 1986, and assigned to the assignee of this application.
Although the systems disclosed in those applications are particularly effective in improving the performance throughout the entire engine and loads ranges, the positioning of the valves in the exhaust pipe is important to the effectiveness of the system and frequently the valves must be positioned directly underneath the engine. In such an arrangement, this can cause difficulty with certain types of vehicles, particularly compact vehicles such as motorcycles. Specifically, where the engine exhaust pipes pass beneath the crankcase transmission of the vehicle, they can seriously reduce the ground clearance and/or may be positioned so that they interfere with leaning of the machine when cornering.
It is, therefore, a principal object of this invention to provide an improved and compact exhaust gas control arrangement for vehicles.
It is a further object of this invention to provide an improved and compact motorcycle arrangement having an exhaust gas control arrangement.
In connection with the use of such exhaust control valves, it is obvious that heat can be a significant problem. In order to provide a valve that is effective, it is desirable to minimize the amount of heat which is exerted on the valve so as to ensure long life and good operation.
It is, therefore, a further object of this invention to provide an improved arrangement for exhaust gas control wherein the control means is effectively cooled.
It is a further object of the invention to provide an exhaust gas control arrangement for a motorcycle wherein the control valve will be adequately cooled.
In connection with the use of control valves for multiple cylinder engines, it is desirable to maintain the valve shafts as short as possible so as to minimize the effect of thermal expansion. One way this can be done is by having the exhaust pipes and the individual valves positioned vertically above each other. However, such a configuration can further aggravate the ground clearance problems already noted.
It is, therefore, a still further object of this invention to provide an exhaust gas control valve arrangement which will permit a compact configuration and, at the same time, minimize the effects of thermal expansion.
It is another object of the invention to provide a compact multiple valve element control valve for an engine exhaust system.
In connection with vehicles wherein the control valve is positioned at a low point in the vehicle, it is essential to ensure that the valve will not be struck by obstacles when the vehicle is in motion. If the valve becomes struck, there is a danger that it may be damaged and/or locked in a position which will not result in good performance under all running conditions.
It is, therefore, still a further object of this invention to provide an improved and protected exhaust gas control means for a vehicle.
SUMMARY OF THE INVENTION
A first feature of the invention is adapted to be embodied in an internal combustion engine that is comprised of a crankcase defined by a crankcase housing. The engine has a plurality of exhaust ports that are formed in a side of the engine and a plurality of exhaust pipes extend from the exhaust ports downwardly and pass beneath the crankcase housing. Valve means are provided in the exhaust pipes for controlling the flow therethrough. This valve means lies beneath the crankcase housing and in accordance with this feature of the invention, a recess is formed in the crankcase housing through which at least a portion of the valve means and exhaust pipes pass.
Another feature of this invention is adapted to be embodied in a control valve arrangement for an exhaust system of an internal combustion engine of the type described in the preceding paragraph. In accordance with this feature of the invention, the valve means is comprised of an outer housing having at least an upper and a lower vertically spaced exhaust passage in which a valve element is positioned. The valve elements are supported upon respective rotatably supported valve shafts. In accordance with this feature of the invention, a control device rotatably positions the lowermost valve shaft and a motion transmitting means transmits motion from the lowermost shaft to the uppermost shaft so that the valves will be operated in unison.
Yet a further feature of the invention is adapted to be embodied in a vehicle having an internal combustion engine with a plurality of exhaust ports from which exhaust pipes extend downwardly and pass beneath the engine. Valve means are provided in the exhaust pipes for controlling the flow therethrough and a skid plate is positioned beneath the valve means for protecting the valve means.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side-elevational view of a motorcycle having an exhaust system constructed in accordance with an embodiment of the invention. The exhaust system is shown in solid lines whereas the remainder of the motorcycle is shown in phantom.
FIG. 2 is an enlarged front elevational view showing the engine and the exhaust system.
FIG. 3 is an enlarged side-elevational view showing the engine, exhaust system and a portion of the motorcycle, which is partially broken away.
FIG. 4 is a top plan view showing the exhaust system and its relationship to the crankcase transmission assembly of the engine.
FIG. 5 is an enlarged longitudinal cross-sectional view showing the control valve.
FIG. 6 is a cross-sectional view taken along the line 6--6 of FIG. 5.
FIG. 7 is an enlarged cross-sectional view, in part, similar to FIG. 5, showing a control valve constructed in accordance with another embodiment of the invention.
FIG. 8 is a cross-sectional view taken along the line 8--8 of FIG. 7.
FIG. 9 is a cross-sectional view, in part, similar to FIGS. 5 and 7, showing a control valve constructed in accordance with yet another embodiment of the invention.
FIG. 10 is a cross-sectional view taken along the line 10--10 of FIG. 9.
FIG. 11 is a side-elevational view of a motorcycle constructed in accordance with another embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring first to FIG. 1, a motorcycle constructed in accordance with a first embodiment of the invention is identified generally by the reference numeral 21 and is shown primarily in phantom. Although the invention has utility with other types of vehicles or other applications for internal combustion engines, it has particular utility in connection with a motorcycle.
The motorcycle 21 is comprised of a frame assembly 22 that journals a front fork assembly 23 for steering movement. A front wheel 24 is supported by the fork assembly 23 and may be steered by means of a handle bar 25. The motorcycle frame 22 further mounts a driven rear wheel 26, which is driven in a manner to be described. A fuel tank 27 is carried by the frame assembly 22 rearwardly of the handle bar 25 and front fork 23. A seat 28 is supported on the frame 22 rearwardly of the fuel tank 27 so as to accommodate a rider. A cowling assembly, or body, 29 is also carried over the frame assembly 22 for affording streamlining and wind protection.
The motorcycle 21 is powered by an internal combustion engine, indicated generally by the reference numeral 31. The engine 31 is suspended in the frame assembly 22 in a known manner and is provided with a cylinder block 32 which is disposed so that the cylinder bores are transversely disposed relative to the longitudinal axis of the motorcycle 21. The engine 31 further includes a combined crankcase transmission assembly 33 which is formed at least in part by a lower crankcase housing 34. The transmission crankcase assembly 33 includes a change speed transmission that drives the rear wheel 26 via a chain 35 in a known manner.
The engine 31 is further provided with an exhaust system, indicated generally by the reference numeral 36 and constructed in accordance with an embodiment of the invention. The exhaust system 36 is best understood by reference to FIGS. 2 through 4. As has been noted, the cylinder block 32 is disposed so that the cylinder bores extend transversely across the motorcycle 21. The cylinder block, or cylinder head, are formed with exhaust ports that pen forwardly and downwardly. In the illustrated embodiment, there are four such exhaust ports and individual exhaust pipes 37, 38, 39 and 41 have respective flanged end portions 42, 43, 44 and 45 that are matingly engaged with and affixed to the exhaust ports in a known manner. The exhaust pipes 37, 38, 39 and 41 extend downwardly and then turn rearwardly and run in a generally horizontal plane beneath the engine 31. Specifically, the exhaust pipes 37, 38, 39 and 41 extend under the crankcase housing 34. For a reason to be described, the exhaust pipes are paired so that the pipes 37 and 41 lie above the pipes 38 and 39 respectively.
In the area under the crankcase member 34, there is provided a control valve assembly indicated generally by the reference numeral 46. The control valve assembly 46 includes a collector, expansion section 47 from which a tail pipe 48 extends. A muffler 49 is positioned at the end of the tail pipe 48 and discharges the silenced gases to the atmosphere in the area adjacent the rear wheel 26 at one side thereof.
Referring now primarily to FIGS. 5 and 6, the construction of the valve assembly 46 will be described. The valve assembly 46 includes a main housing assembly 51 that is formed with four cylindrical inlet sections 52, 53, 54 and 55, that receive the rearward ends of the exhaust pipes 37, 38, 39 and 41, respectively. Cylindrical sections 52 through 55, therefore, form the exhaust gas inlets to the valve body 51. Downstream of the inlet portions, there are provided pairs of upper and lower enlarged openings through which an upper valve shaft 56 and a lower valve shaft 57 extend. Valve plates 58 and 59 are affixed to the valve shaft 56 within the openings that are aligned with the inlet openings 52 and 53. In a like manner, valve plates 61 and 62 are fixed to the valve shaft 57 in the openings which are aligned with the inlet openings 53 and 54. The valve plates 58, 59, 61 and 62 are disposed so that when they are in their fully closed position, as shown in the phantom line view of FIGS. 5 and 6, they will obstruct approximately one-half of the flow area through the respective passages. When in their fully opened position, the valve plates 58, 59, 61 and 62 will offer substantially no restriction to flow.
Downstream of the valve plates 58, 59, 61 and 62, the expansion section 47 forms a collector volume 63 that functions as an expansion chamber. A cylindrical opening 64 is formed at the trailing end of the valve housing 51 and receives the inlet end of the tail pipe 48.
It should be noted that the valve assembly 46 lies under the engine 31 and specifically beneath the crankcase housing 34. In order to minimize the loss of ground clearance, the lower wall of the crankcase housing 34 is provided with a longitudinally extending recess 65 through which a part of the valve body 51 extends and also through which a part of the exhaust pipes 37 and 41 extend. As a result, the loss of ground clearance is substantially minimized. In addition, the longitudinal direction of the recess 45 permits air to flow to cool the exhaust system and, specifically, the control valve assembly 46. To aid in this cooling, the body, or cowling, 29 is provided with an air inlet opening 66 that faces forwardly and through which air may flow so as to cool the exhaust system. The heated air exits through an outlet opening 67 formed in the rear portion of the cowling 29 (FIG. 3).
The valve shafts 56 and 57 and, accordingly, the valve elements 58, 59, 61 and 62 are operated so as to be moved between their open and closed position in response to an engine running condition such as load or speed. To this end there is provided an engine condition sensor 68 which outputs a signal corresponding to the engine running condition to a computer control circuit 69. The computer control circuit 69 operates a control motor 71 which, in turn, drives a pulley 72. The pulley 72 has affixed to it a pair of flexible transmitters 73 which have their sheathes maintained in a bracket 74 positioned in proximity to the valve 46. In this embodiment of the invention, a pulley 75 is affixed to the valve shaft 57 and the flexible transmitters 73 are connected to this pulley for rotating the valve shaft 57.
The control circuit also includes an angle sensor 76 that senses the angle of the pulley 72 and, accordingly, the angle of the pulley 75 and feeds back this signal to the computer 69. Generally, the computer 69 functions to maintain the valve plates 58, 59, 61 and 62 in their fully closed position (wherein they obstruct approximately one-half of the flow area in the exhaust system) at mid-range loads and the valve elements are opened at other loads. Of course, the actual running conditions under which the valves are closed and open will vary from engine to engine and those skilled in the art can readily arrive at an arrangement for appropriately controlling a given engine.
The rotation of the valve shaft 57 is transmitted to rotation of the valve shaft 56 so that all of the valve elements, 58, 59, 61 and 62 will be operated in unison. To this end, there is provided a turnbuckle mechanism 77 that interconnects to a pair of levers 78 affixed to the valve shafts 56 and 57 for ensuring their simultaneous rotation. The turnbuckle 77 permits adjustment of the relative angular positions of the valve shafts 56 and 57.
The fact that the shaft 57 is directly operated by the pulley 75 while the shaft 56 is indirectly operated, permits the valve assembly 46 to be raised higher into the recess 65 of the crankcase casing 34 and thus permits a more compact assembly. In other applications, it may be possible to provide pulleys like the pulley 75 on both the shafts 56 and 57 although some of the advantages of the compactness will, obviously, be lost with such an arrangement.
It should also be noted that the fact that the body has a portion which underlies the valve assembly 46. The valve assembly 46 will be protected from foreign objects which may be thrown up during movement of the motorcycle. However, the air flow passage defined by the openings 66 and 67 will ensure good cooling.
Cooling is further assisted and lightning is possible by means of a plurality of lightning holes 79 that extend through the valve body 51. These lightning holes also reduce the effects of thermal expansion.
FIGS. 7 and 8 show another embodiment of the invention. This embodiment is generally similar to the embodiment of FIGS. 1 through 6. However, in this embodiment the control valve assembly, which is indicated generally by the reference numeral 201 has a slightly different configuration and is formed as a fabrication. The valve element 201 includes a main body portion 202 in which four rectangularly configured openings 203, 204, 205 and 206 are formed. The openings 203 and 206 lie next to each other and above the respective openings 204 and 205. Inlet sections, which may be formed as fabrications 207, 208, are aligned with the openings 203 and 206 and receive the exhaust pipes 37 and 41, respectively. In a like manner, inlet sections 209, 211, extend from the openings 204 and 205 and receive the exhaust pipes 38, 39, respectively.
A fabricated collector section 212 extends from the downstream portion from the main valve body 202 and defines an expansion chamber 213. The tail pipe 48 is received on the end of this collector section.
As with the previously described embodiment, valve shaft 214 and 215 are journaled in the main body portion 202 and extend one above the other. Generally rectangular valve plates 216, 217, 218 and 219 are affixed to the valve shaft 214 and 215 within the openings 203, 204, 205 and 206, respectively, for controlling the flow. In this embodiment, the valve plates 216, 217, 218 and 219 are adapted to fully extend across the openings 203, 204, 205 and 206 when the valves are in their closed position. As may be seen from FIG. 8, however, the cross-sectional area of the valve plates 216, 217, 218 and 219 is substantially less than the area of the openings 203, 204, 205 and 206. The difference in cross-sectional area is approximately one-half so that approximately one-half of the flow area will be obstructed, as with the previously described embodiment, when the valve shafts 214 and 215 are in their fully closed positions.
Like the previously described embodiment, a pulley 75 is affixed to the shaft 215 for operating it. The shaft 214 and 215 are interconnected for simultaneous movement by means of links 221 and 222 that are fixed to the shafts 215 and 214, respectively. The links 221 and 222 are interconnected by means of a pivotal link 223 so that the shafts 215 and 214 will rotate in unison.
A control valve arrangement constructed in accordance with yet another embodiment of the invention is illustrated in FIGS. 9 and 10 and is indicated generally by the reference numeral 251. This control valve differs from the previous control valves in that it only requires one valve shaft. In accordance with this embodiment, a main valve body 252 is provided with a pair of generally oval-shaped sections 253 and 254. The section 253 is aligned with inlet openings 255 and 256, which are generally cylindrical in shape. In a like manner, the opening 254 is aligned with inlet openings 257 and 258 which are cylindrical in configuration. The openings 255, 256, 257 and 258 receive exhaust pipes as in the previously described embodiment.
In this embodiment, a single valve shaft 259 is journaled in the body 252 and extends generally transversely across it. A pair of oval-shaped valve elements 261 and 262 are affixed to the valve shaft 259 and extend into the passages 253 and 254. Rotation of the valve elements 261 and 262 will selectively open and close the flow areas so as to achieve the results as aforedescribed.
In all of the embodiments thus far described, the motorcycle 21 was provided with a cowling, or body portion, 29 that had a portion that extended beneath and protected the valve assembly. FIG. 11 shows an embodiment of a motorcycle, indicted generally by the reference numeral 301, that has a construction the same as the previously described embodiment except that it lacks the cowling 29. For that reason, components of this embodiment which are the same as the previously described embodiment have been identified by the same reference numerals and will not be described again. In this embodiment, however, a shield or skid plate 302 is affixed to the frame 22 beneath the valve element 46 so as to protect it. The skid plate 302 is, however, configured so as to provide an open and front end so as to define a longitudinally extending air passage 303 for cooling. In all other regards, this embodiment is the same as the previously described embodiments and for that reason further description of it is believed to be unnecessary.
It should be readily apparent from the foregoing description, that a number of embodiments of the invention have been illustrated and described. Each of these embodiments incorporates a control valve for controlling the reflective area of the exhaust system so as to improve performance at mid-range conditions. In addition, the arrangements are all designed so that the control valve will not seriously and adversely affect the ground clearance and also so that it will be cooled by a path of cooling air flowing across it. In addition, the control valve is protected by a skid plate or a body portion so as to avoid its damage. In addition to the illustrated and described embodiments, variously changes and modifications may be made without departing from the spirit and scope of the invention, as defined by the appended claims.
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A number of embodiments of motorcycle exhaust systems including control valves for controlling the effective area of the exhaust pipes and for improving performance by preventing reflections from one exhaust pipe back into the cylinder served by another exhaust pipe. The valve means lies under the engine crankcase and the crankcase is formed with a recess for clearing the valve means and permitting air flow across it for cooling purposes. Various valving arrangements are disclosed as is a skid plate arrangement for protecting the valve means.
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RELATED APPLICATION
Ser. No. 07/064,760, filed June 22, 1987, now abandoned.
BACKGROUND OF THE INVENTION
The invention relates generally to a new design of a vase which will relieve stress and is a source of beautification and gratification in improving one's self image.
SUMMARY OF THE INVENTION
The invention relates to a vase that can be filled with a round like pebble or other symbolic object.
The pebble represents an image of a "good deed"performed by the person who owns the vase.
It is an object of the invention to provide a gift to oneself by placing a pebble into the vase each time you have done a good deed or act for someone or yourself. To make it effective, whenever the owner of the vase becomes down on oneself because they have made a mistake or did not do something right or something has happened in their lIfe that they do not feel good about, they can turn to their vase and meditate. It mentally will give a relief of stress when they can take a short moment to remind themselves of all of the good they have done by seeing all of the pebbles that have accumulated inside the vase.
It is another object of the present invention to find extraordinary in oneself through a unique vase filled with small pebbles. By filling the vase in this manner, it will change an ordinary to bad day into a more peaceful and meaningful day for yourself and all that are around you.
It is a further object of the invention to provide means to watch ourselves honestly so that we can see that often we are own worst enemy in almost every situation. To remind ourselves that one of the worst things in life is to try and please but please not, especially, ourselves. The unique vase and pebble concept will remind us that we are full of self good and by reminding ourselves of this we can find inner peace to give to ourselves and people who are around us.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a side elevational view of a round like pebble and
FIG. 2 is a perspective view of a precious pebbles vase in accordance with my invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to Figure, a preferred embodiment of the precious pebbles vase is shown. In this embodiment, the precious pebble vase is comprised of a square crystal base 1 and an attached pair of vertically disposed crystal hands 3 which securely hold a transparent, hollow, crystal vessel 2. The hollow vessel 2 has an opening 4 at the top center as a means for the user to place the round pebble 5 shown in FIG. 1 inside of the ball-shaped vessel 2 each time a good deed is performed.
In the preferred embodiment of my invention, the support base, hands, hollow vessel and pebble are made of crystal glass. The base, hands and pebble are preferably solid; however, one or all components can be hollow. A lower grade of glass can be used for any of the components 1, 2, 3 and 5. In order to achieve the functions of my invention which includes enabling the user to view the accumulation of the pebbles inside the vessel, it is important that the walls of the vessel be sufficiently transparent to permit the user to see the pebbles. The vessel is preferably clear and colorless; however, it can be various gradations of color such as a rose-hued, yellow-hued or the like that does not prevent seeing the pebbles. In lieu of opening 4 positioned at the top center of the vessel, the opening can be positioned at about mid-point or higher of the vessel side wall. Also, the size of the opening 4 can be increased so as to enable the user to reach her or his hand into the vessel. The vessel can be made of colored or clear and transparent glass or plastic.
The base 1 in the preferred embodiment is solid and square in order to provide good stability for the vase. Stability can be achieved using numerous other shapes, solid or hollow, such as rectangular, triangular, oval, circular, diamond, or the like. Suitable materials for the base include glass, plastic, wood, stone and various ceramic materials. The support base component can be clear and transparent, semi-transparent or opaque of various colors.
The hands 3 of the vase which support and hold the transparent, hollow vessel 2 in the preferred embodiment are vertically aligned(longitudinal) and the wrist portion resting on and secured to the top surface of the base support 1. The hands can be connected to the base as by gluing, screw or bolt, or making, such as by molding, the hands and support base as a single, integral piece. The hands can be made of the same materials as described for the base or different materials. Similarly, the hands can be clear and transparent, semi-transparent or opaque of various colors. In another embodiment of the vase of the present invention, not shown, the hands are laterally aligned and substantially parallel to the top surface of the base. The outer edge of the hand in this embodiment rest on and is connected to the top surface of the base with the fingers extending and holding the hollow vessel latitudinally.
The term "hollow vessel", as used herein and the appended claims, means vessels of various shapes such as ball(oval or round), cylindrical, square, rectangular shape, or the like.
The term "transparent", as used herein and the appended claims, means clear and transparent, as well as, semi-transparent.
The term "pebble", as used herein and the appended claims, means a spheroid shaped pebble as shown in FIG. 1 and includes polygonal shapes such as cubes, hexagonal, octagonal, or the like.
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A precious pebbles vase comprising a base which supports a pair of hands for holding a transparent, hollow vessel adapted to receive and hold a plurality of pebbles. A small pebble is placed in the vessel each time a good deed or act is performed by the owner of the vase.
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This application is a division of application Ser. No. 32,444, filed Apr. 23, 1979, now U.S. Pat. No. 4,294,923, issued 10/13/81.
BACKGROUND OF THE INVENTION
The present invention relates to substrates and methods for determining enzymes. More particularly, the invention relates to qualitative and quantitative methods for determining proteolytic enzymes.
The determination of specific enzymes in biological fluids, such as blood, tissue homogenates, and cytoplasm can be very useful for the diagnosis of certain diseases. The discovery of synthetic substrates for such determinations has resulted in clinical assay procedures having a high degree of specificity, reliability, and sensitivity. Such substrates have been employed for the determination of amylase (Driscoll, R. C., et al., U.S. Pat. No. 4,102,747) and various proteinases.
Synthetic proteinase substrates have generally been amino acid derivatives of aromatic amines. The number and arrangement of amino acids in the peptide moiety determine the enzyme specificity of the substrate and the enzyme activity is measured by the amount of aromatic amine moiety liberated upon hydrolysis of the substrate. Amino acid derivatives of p-nitroaniline have been widely used as synthetic substrates. Erlanger, B. F., U.S. Pat. No. 3,412,150. Other aromatic amines which have been reacted with amino acids or peptides include 2-naphthylamine, 4-methoxy-2-naphthylamine, and 7-amino-4-methylcoumarin. The use of 2-naphthylamine and 4-methoxy-2-naphthylamine for the preparation of synthetic substrates and prior art relating thereto are discussed by Smith, R. E., U.S. Pat. No. 3,862,011. Peptide derivatives of 7-amino-4-methylcoumarin have recently been reported as fluorogenic substrates for a number of proteinases. Zimmerman, M., Yurewicz, E., Patel, G., Anal. Biochem. 70, 258-262 (1976) and Zimmerman, M., Quigley, J. P., Ashe, B., Dorn, C., Goldfarb, R., Troll, W., Proc. Natl. Acad. Sci., 75, 750-753 (1978).
Because the chromophore, p-nitroaniline, is yellow, enzyme assays employing that chromophore are colorimetric. Fluorescence assays are sometimes preferred over colorimetric assays, because of greater sensitivity and less background interference. The aromatic amine chromophores heretofore used to prepare synthetic substrates are fluorescent, but their fluorescence generally occurs in the blue region of the spectrum. Such fluorescence is disadvantageous, because it is difficult to measure with inexpensive instruments, and it is similar to fluorescense of other materials present in the analyte, including, in some instances, the intact substrate. These assays are useful for cytological studies for the detection of an enzyme within a single cell. When such cells are viewed under a fluorescence microscope, a blue color is difficult to see or distinguish from the background, but cells emitting light in the yellow region of the spectrum are easily visualized.
To overcome these problems, investigators have focused on reactions involving the enzyme-liberated chromophore to enhance color or fluorescence at a desired wavelength. For instance, aromatic amine chromophores may be reacted with diazonium salts to form azo dyes which are determined spectrophotometrically. In U.S. patent application Ser. No. 828,394, R. E. Smith, et al. disclose a reaction of the aromatic amine chromophore with certain aromatic aldehydes to form Shiff base compounds which fluoresce in the yellow-green region of the spectrum.
Although such methods have each constituted significant advances over the prior art, there is a need for synthetic substrates for proteinase enzymes which do not fluoresce in the yellow region, but which upon enzyme hydrolysis, release a chromophore which fluoresces strongly in that region of the spectrum. Such substrates would, thus, obviate the need for further reactions involving the liberated chromophore, and the concentration of such chromophore could be readily determined by a fluorometric technique.
SUMMARY OF THE INVENTION
In accordance with the present invention, there is disclosed a method for determining the presence of an enzyme in an enzyme-containing analyte, comprising:
(a) contacting the analyte with a substrate which can be hydrolyzed by said enzyme to liberate 7-amino-4-trifluoromethylcoumarin, said substrate having the formula ##STR1## wherein R is an amino acid, a peptide, or a derivative thereof, therby forming an analyte-substrate mixture;
(b) incubating the analyte-substrate mixture under enzyme hydrolyzing conditions to form an enzyme hydrolyzate; and
(c) fluorometrically or spectrophotometrically determining the presence of 7-amino-4-trifluoromethylcoumarin in the enzyme hydrolyzate.
DETAILED DESCRIPTION OF THE INVENTION
The substrates of the present invention are represented by the formula ##STR2## wherein R may be a single amino acid or a peptide, consisting of two or more amino acids. The terminal amino acid may be reacted with any suitable blocking groups as is well known in the art, such as carbobenzoxy, benzoyl, glutaryl, t-butyloxycarbonyl, and certain d-amino acids, e.g. d-proline, d-valine, or d-alanine.
Thus, upon enzymatic hydrolysis, the chromophore, 7-amino-4-trifluoromethylcoumarin is released. This chromophore fluoresces strongly in the yellow region of the spectrum when irradiated with ultraviolet light, but the intact substrates fluoresce very weakly, if at all, in that region. The fluorescent properties of the substrates and the chromophore render these compounds particularly useful for the enzyme assays. The presence of the liberated substrate can be qualitatively or quantitatively determined fluorometrically without employing dye-forming or wavelength-shifting reactions.
In contrast with prior art substrates which are used either in colorimetric or fluorometric assays, but not both, the present substrates may be used in both direct colorimetric and fluorometric assays. The 7-amino-4-trifluoromethylcoumarin chromophore has a yellow color, but the intact substrates are substantially colorless. Thus, the substrates can be employed in spectrophotometric as well as fluorometric assays. This property of the substrates makes them particularly valuable for use in enzyme kinetic studies.
The number and arrangement of amino acids attached to the chromophore determine the enzyme specificity for the substrate. Any combination of amino acids can be employed to obtain the desired specificity. Preferably, the amino acid chain consists of from 1 to about 12 amino acids and, most preferably from 1 to about 6 amino acids. The amino acids are bound together through peptide bonds.
Advantageously, the amino acid chain may be terminated with a blocking group. Such a blocking group may be employed during the synthesis of the substrate to prevent reactions with the terminal amino acid, and the blocking group is sometimes employed in substrates to improve enzyme specificity. Such blocking groups are well known in the art as described above.
Preferred substrates of the present invention are compounds represented by the above formula wherein R is Cbz-Gly-Gly-Arg-; D-Ala-Leu-Lys-; Cbz-Val-Lys-Lys-Arg- and Leu- (Cbz represents carbobenzoxy and the amino acid abbreviations are generally recognized and accepted in the art). The first substrate is useful for assays for trypsin and urokinase, the second is useful for plasmin assays, the third is useful for the determination of cathepsin B, and the fourth is useful for the determination of aminopeptidase M.
The substrates may be prepared by acylating 7-amino-4-trifluromethylcoumarin with an appropriate amino acid or peptide. Such acylation may be accomplished by a conventional mixed anhydride reaction. Similarly, amino acids or peptides can be added to substrates having one or more unblocked amino acids. For instance, a urokinase substrate can be prepared by the following reaction scheme: ##STR3## Any desired number and arrangement of amino acids may thus be added onto the chromophore. Blocking groups may be removed, e.g. by hydrogenolysis or treatment with anhydrous hydrogen bromide in acetic acid, trifluoroacetic acid or other conventional deblocking agents as are known in the art.
In the practice of the method of the present invention, an analyte containing, or suspected of containing, an enzyme is contacted with a substrate which can be hydrolyzed by that enzyme. Such analyte is usually a natural biological fluid such as blood, serum, urine, tissue homogenate, etc., but may also be a synthetic solution used for quality control or as a reference standard. The substrate is generally employed in excess of the amount which can be completely hydrolyzed by the quantity of enzyme present. For instance, the substrate is preferably employed in an amount of from 1 to about 10 times, most preferably from about 1 to about 4 times that amount which can be completely hydrolyzed by the enzyme.
The analyte-substrate mixture is incubated under enzyme-hydrolyzing conditions to form an enzyme hydrolyzate. Such enzyme-hydrolyzing conditions include conditions of pH and temperature which are conducive to the enzymatic hydrolysis of the substrate. The pH of the analyte-substrate mixture will generally be in the range of the normal physiological environment of the enzyme, and thus may vary from one enzyme to another. Such pH is usually in a range of from about 4 to about 10, and preferably in a range of from about 5 to about 8.5. A pH of about 8 has been employed for urokinase, plasmin, and trypsin assays and a pH of about 7.2 has been used for aminopeptidase M assays. The pH of the mixture is conveniently controlled by dissolving the analyte and substrate in an appropriate buffer, as is well known in the art. A suitable buffer is N-tris (hydroxymethyl) methyl-2-aminoethanesulfonic acid (TES).
The temperature at which the enzyme hydrolysis is effected is not critical, and may fall within a broad range, provided that the temperature is high enough to insure enzyme activity, but not too high to cause degradation or other deleterious reactions involving the substrate, the enzyme, or other components of the mixture. The temperature advantageously is from about 15° C. to about 50° C., preferably from about 20° C. to about 40° C.
The fluorometric determination of the liberated chromophore may be either a rate determination or an endpoint determination. Rate determinations are preferred, because they are generally more sensitive and precise. In a rate determination, the fluorescence of the substrate-analyte mixture may be determined promptly after the analyte is contacted with the substrate. In an endpoint determination, the enzyme hydrolysis reaction is allowed to proceed for a predetermined length of time, e.g. from about 5 to about 60 minutes, preferably from about 15 to about 30 minutes. Such reaction time is selected so that a sufficiently quantity of chromophore has been released to provide an acceptable degree of accuracy for the assay.
For fluorometric assays, excitation and emission wavelengths may be selected to conform to existing equipment commonly available in clinical laboratories. Maximum excitation and emission wavelengths for the 7-amino-4-trifluoromethylcoumarin chromophore are 365 nm and 495 nm, respectively. Wavelengths of 400 nm and 505 nm have been employed; and at these wavelengths, the fluorescence of the liberated chromophore is about 700 times greater than an equimolar solution of the substrate, while retaining about 57% of the maximum fluorescence.
The absorbance maximum wavelength for the liberated chromophore is about 370 nm. In spectrophotometric assays, the absorbance measurements are usually made at about 380 nm to minimize interference by the intact substrate.
Those skilled in the art will recognize that the substrates of this invention may be useful in a variety of analytical techniques. For instance, the substrates can be utilized in cytological studies to indicate the presence of certain enzymes in single cells. Other uses of the substrates include their utilization as indicators for various chromatographic or electrophoretic techniques. Enzymes may be isolate by chromatography, e.g. paper chromatography, thin-layer chromatography or column chromatography, or by electrophoresis and the appropriate substrate may be applied to the chromatographic or electrophoretic medium to indicate the location or intensity of the enzyme spot, band, or zone.
Thus, there has been discovered a sensitive and reliable method and novel substrates for the determination of proteinase enzymes. The invention is further illustrated by the following examples which are not intended to be limiting.
EXAMPLE I
This example describes a procedure for preparing a substrate of the formula ##STR4## wherein Cbz is carbobenzoxy, and is applicable to the preparation of any of the substrates of the present invention by selection of the proper reactants.
Cbz-arginine, 1.7 g, was dissolved in 10 ml of dry demethylformamide, the solution was cooled in an ice-acetone bath, and 0.75 ml of isoamylchloroformate was added. The mixture was stirred for three hours at -15° C. 7-amino-4-trifluoromethylcoumarin, 1.15 g, was added and stirring was continued for another 20 hours while the bath was allowed to warm to room temperature. The solvents were removed by vacuum distillation at 5 mm Hg pressure at room temperature, and the residue was dried overnight under 10μ of Hg pressure at room temperature. The crude reaction mixture was purified by high performance liquid chromatography using a silica gel column and 10% methanol in methylenedichloride as the eluant, thus yielding a product of the formula: ##STR5##
That product, 555 mg, was dissolved in 5 ml of 32% HBr in acetic acid. After 30 minutes at room temperature, the orange solution was poured into 80 ml of ether. The mixture was centrifuged and the precipitate was washed twice with ether and dried overnight. This procedure is effective for removing the carbobenzoxy blocking group. The resulting product, 0.98 g, was dissolved in 5.0 ml of dry dimethylformamide, and this solution was combined with the mixed anhydride prepared from 660 mg of Cbz-Gly-Gly in 5.0 ml of dried dimethylformamide at -15° C. (mixed anhydride prepared by reacting Cbz-Gly-Gly with isobutylchloroformate in the presence of N-methylmorpholine in DMF solvent). The mixture was stirred overnight as the temperature was allowed to reach room temperature. The solvents were removed by vacuum distillation at 5 mm Hg pressure at room temperature, and the residue was dried overnight at room temperature at 30μ Hg pressure. The product was purified by twice subjecting it to high pressure liquid chromatography on a silica gel column using 20% methanol in methylenedichloride. The nuclear magnetic resonance spectrum of the product was consistent with the assigned structure. The optical rotation of the product (195 mg /10 ml methanol) [α] D 23 -6.4°. The elemental analysis for carbon, hydrogen, and nitrogen was also consistent with the assigned structure.
EXAMPLE II
A series of experiments was conducted to demonstrate the method of the present invention. Solutions of each of the enzymes, urokinase, plasmin, aminopeptidase M, and trypsin were prepared at various concentrations within the ranges indicated in Table I. For trypsin and urokinase assays, the substrate cbz-gly-gly-arg-7-amino-4-trifluoromethylcoumarin was used as the substrate. For plasmin assays, d-ala-leu-lys-7-amino-4-trifluoromethylcoumarin was used, and for aminopeptidase M assays, leu-7-amino-4-trifluoromethylcoumarin was used. Dimethylformamide solutions of the substrates (10 2 millimolar for aminopeptidase M assays and 20 millimolar for trypsin, urokinase, and plasmin assays) were prepared. To conduct an assay, 50 μl of substrate solution was added to 900 μl of buffer (0.05 M TES, pH 8, for urokinase and plasmin; 0.05 M TES, pH 7.2, for aminopeptidase M; 0.5 M TES, pH 8.0 for trypsin) in a cuvette. To this solution, 50 μl of enzyme solution was added and the temperature was controlled at 25° C. Fluorescence was recorded for five minutes or more on a recording spectrofluorometer using an excitation wavelength of 400 nm and an emission wavelength of 505 nm. The rate of increase of fluorescence was linear over the enzyme concentration ranges indicated in Table I, and the rate of increase of fluorescence was found to be directly proportional to enzyme concentration.
TABLE I__________________________________________________________________________ Substrate C═7-amino-4-trifluoro- Linear DetectionEnzyme methylcoumarin Range Limit__________________________________________________________________________Trypsin Cbz--Gly--Gly--Arg--C 0.08-25 ng/ml 0.08 ng/mlUrokinase Cbz--Gly--Gly--Arg--C 0.75-50 I.U./ml 0.75 I.U./mlPlasmin d-Ala--Leu--Lys--C 0.0006-0.06 CTA/ml 0.0006 CTA/mlAminopeptidase M Leu--C 6.0-600 ng/ml 6.0 ng/ml__________________________________________________________________________
EXAMPLE III
A patient serum may be assayed for the enzyme cathepsin B by the following procedure. A 2 millimolar solution of the substrate Cbz-Val-Lys-Lys-Arg-7-amino-4-trifluoromethylcoumarin in dry dimethylformamide was prepared. This substrate solution, 0.50 μl, was added to 900 μl of 0.05 M sodium cacodylate buffer (pH 5.6-6.2) in a cuvette. To this solution, 50 μl of 1:10 diluted patient serum was added and the temperature was controlled at 25° C. Fluorescence was measured as described in Example II and the rate of increase of fluorescence was compared to a standard calibration curve to determine enzyme concentration.
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A method is disclosed for determining the presence of an enzyme in a biological fluid, which includes the steps of contacting the fluid with a synthetic chromogenic substrate, which is an amino acid derivative of 7-amino-4-trifluoromethylcoumarin; incubating the substrate-containing fluid to effect enzymatic hydrolysis; and fluorometrically determining the presence of the free 7-amino-4-trifluoromethylcoumarin chromophore in the hydrolyzate.
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BACKGROUND OF THE INVENTION
This invention relates to an improved, self-lighting cigarette or cigar which helps prevent the inhalation of the irritating and noxious fumes produced by the self-lighting ignition element.
Self-lighting cigarettes have been known for quite some time. Most of these cigarettes are based on the incorporation of combustible substances at one end of the cigarette which ignite when that end is struck on a rough surface. The primary advantage of these cigarettes is the avoidance of any need for matches or an external heat source such as a cigarette lighter.
One of the drawbacks of self-lighting cigarettes is that irritating and noxious fumes are generated by the ignition since the combustible substances used are generally based upon sulfur, phosphorous, or similar compounds. These fumes are frequently drawn into the mouth of the smoker and inhaled, producing an unpleasant sensation and a distaste for self-lighting cigarettes. Many attempts have been made to overcome this problem. Some of them are described in U.S. Pat. No. 2,874,700 to Kahler; U.S. Pat. No. 3,136,318 to Nakamura; and U.S. Pat. No. 3,692,030 to Whang.
SUMMARY OF THE INVENTION
My invention relates to an improved self-lighting cigarette which has an ignition means located at one end of the cigarette and has a means located at the opposite end, the lip end, to prevent the inhalation of the irritating fumes produced by the ignition means. Advantageously, the preventive means is a cap or cover which encloses the lip end of the cigarette and keeps the smoker from inhaling any smoke or fumes through the cigarette until the cap has been removed. Preferably, the cap or cover is made from plastic film.
In a preferred embodiment of my invention, the ignition means or cap is not directly attached to the cigarette paper or the tobacco, but is held on the cigarette by connection or attachment to the preventive cap. This serves two functions. First, it precludes the ignition of the cigarette via the self-lighting means if the preventive cap has been removed from the lip end. Second, if the connecting means is properly designed, it permits the removal of the ignition cap with the preventive cap after the completion of the ignition process. This reduces the possibility that the hot ignition cap will fall on the floor or clothing or burn the smoker when he attempts to remove the ignition cap from the cigarette.
Advantageously, the ignition cap and the preventive cap are attached to each other by one or more straps which may also be made of plastic. Preferably, at least two straps are involved. One of these straps may be designed to burn through during the ignition process while the other may be located in such a way, or of such a thickness, that it will not normally burn through. This later strap will permit the ignition cap to be removed from the cigarette at the same time the preventive cap is removed.
A primary advantage of my invention is that the preventive means will keep the smoker from inhaling the noxious fumes generated by the ignition cap at the other end of a self-lighting cigarette. This will reduce one of the major obstacles to the acceptance of self-lighting cigarettes.
Another advantage of my invention is that the attachment of the ignition cap to the preventive means precludes premature removal of the preventive cap and also promotes easy removal and disposal of the ignition cap without burning the smoker, his clothes, or the carpeting.
Additional features and advantages of my invention are described in, and will appear from, the description of the preferred embodiments which follow and from the drawing to which reference is now made.
DESCRIPTION OF THE DRAWING
FIG. 1 is a perspective view of the self-lighting cigarette of this invention;
FIG. 2 is a sectional view of the self-lighting cigarette of FIG. 1 taken along line 2--2 in FIG. 1.
FIG. 3 is another sectional view of the self-lighting cigarette of FIG. 1 taken along line 3--3 in FIG. 1.
FIG. 4 is a view of the preventive cap, ignition head, and connecting straps of this invention after they have been removed from the cigarette.
DESCRIPTION OF PREFERRED EMBODIMENTS
Referring now to the drawing, reference numeral 10 designates a typical cigarette comprised of a tobacco filler 12 surrounded by a paper wrapper 14. In the particular embodiment shown, cigarette 10 also has a filter 16. While the present invention is primarily intended to be used in conjunction with a cigarette, it can also be used in conjunction with a cigar, a cigarillo or the like.
Located at one end of cigarette 10 is an ignition cap 20 which comprises a combustible ignition head 22 surrounded by collar 24. Ignition head 22 is designed so that it ignites when struck on a surface. It may be designed to function as a "strike-anywhere" ignition head or may be designed to be ignited only when struck on a specially prepared friction surface in a manner similar to a safety match. In the latter case, the specially prepared striking surface may be directly incorporated onto the side of the cigarette package as is shown by FIG. 4 of U.S. Pat. No. 3,692,030. The particular formulations which may be used for the ignition head are generally well known in the art and generally based on one or more phosphorous compounds. However, in addition to the normal igniting agents, the ignition head to be used in conjunction with my invention will preferably contain post-combustion binders such as ground glass or similar materials for the purpose of fusing and holding the ignition head ash together after the cigarette has been ignited. Inert materials such as diatomaceous earth may also be used to provide bulk to the ignition head and to regulate the speed of the combustion reaction.
Ignition head 22 will normally have about the same diameter as that of the cigarette itself. The thickness of ignition head 22 will preferably be on the order of a sixteenth of an inch in order to prevent ignition cap 20 from sliding off the end of the cigarette when striking it on a friction surface, but yet allow easy removal of ignition cap 20 from the end of the cigarette after ignition is complete.
While the ignition head 22 may be attached directly to the cigarette itself by means well known in the art, it is preferably secured not to the cigarette but, as shown in FIG. 1, to collar 24 which is connected via straps 36 to preventive cap 30 located at the lip end of the cigarette. The advantages of this means of attachment will be described below.
As referred to above and as shown in FIGS. 1 and 3, the lip end of the cigarette is enclosed by a protective or preventive cap 30. The primary purpose of this preventive cap is to keep the smoker from inhaling the irritating fumes produced by the ignition cap which would normally be inhaled by the smoker through the cigarette. This preventive cap advantageously comprises an end portion 32 which covers the end of the cigarette and a side portion 34 which extends along side of the cigarette. The length of side portion 34 is preferably on the order of about one-fourth of an inch or more to discourage the smoker from holding the cigarette in his mouth while the cigarette is being ignited and to prevent the inhalation of noxious fumes through the cigarette if it is actually held in the mouth while the ignition cap is still on the other end of the cigarette. For this reason, side portion 34 should normally fit rather snuggly around cigarette 10 or filter 16 if the cigarette is so equipped. A snug fit will also keep the preventive cap from falling off the end of the cigarette before it is intended to be removed. While preventive cap 30 can be made from almost any material, it is advantageously made of paper, plastic, or plastic film.
In a preferred aspect of my invention, the ignition head is not directly attached to the cigarette itself, but to collar 24. The straps and possibly the collar are designed so that one strap becomes severed as a result of ignition. This severing of less than all of the straps may be accomplished by proper shaping of the collar and the straps, by varying the thickness of the collar and straps, using different materials or adhesives, etc.
In the preferred embodiment illustrated, straps 36 connect preventive cap 30 with ignition cap 20. One of the straps is attached to collar 24 while the other passes over the collar and has a tab portion 26 which is attached to the ignition head 22. Preferably these straps are made of paper, plastic or plastic film.
A primary function of straps 36 is to keep the smoker from removing the preventive cap 30 without removing the ignition means 20. If the straps are broken, as would be required if the smoker attempted to remove the preventive cap prior to ignition, the ignition cap 20 will fall from the cigarette, thus precluding ignition via the ignition cap. Accordingly, the smoker will not be tempted to remove the preventive cap prior to ignition and will be kept from inhaling the irritating fumes that would otherwise be drawn through the cigarette from the ignition head 20.
The end result of this aspect of the invention is shown in FIG. 4. In that Figure, broken strap 38 is shown, as is the residual, non-consumed portion of ignition cap 20. As can be seen from FIG. 4, the result of the breaking strap 38 is that ignition cap 20 is still connected to preventive cap 30 and can be easily removed from the cigarette along with the preventive cap. This is accomplished merely by pulling the preventive cap from the lip end of the cigarette. The advantage of this aspect of the invention is that the ignition cap can easily be removed from the cigarette without burning the smoker, his clothes, or the carpeting.
The embodiments described above are intended to be exemplary of the types of ignition, preventive and connecting means which fall within the scope of my invention. However, one skilled in the art would certainly be expected to be able to make modifications and variations of these preferred embodiments without departing from the spirit and scope of the invention as it is defined in the following claims.
I claim:
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A self-lighting cigarette is disclosed having a protective or preventive cap enclosing the lip end of the cigarette to prevent the inhalation of the irritating fumes produced by the ignition means. Also disclosed is a means for attaching the self-lighting device to the preventive cap to prevent premature removal of the preventive cap.
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CROSS-REFERENCE TO RELATED PATENT APPLICATIONS
The present Application is a National Phase Application of PCT/EP2005/002124 entitled, “Device for Locking and/or Unlocking a Component, in particular in/or on a Vehicle and Method” filed on Mar. 1, 2005 which published under PCT Article 21(2) on Oct. 20, 2005 as WO 2005/097544 A1 in the German language, which claims priority to German Patent Application DE 10 2004 017 592.6 filed Apr. 7, 2004, the entire disclosure of which, including the specification and drawings, is expressly incorporated herein by reference.
BACKGROUND
The present invention relates to a locking device for locking and/or unlocking a component in relation to a mating element. More specifically, the present invention relates to a locking device for use in or on a vehicle wherein the locking device has a locking element and a blocking element, the locking element being able to be set into a locking position and into an unlocking position, the blocking element being able to be set into a blocking position and into an actuating position, and the setting of the blocking position bringing about the setting of the locking position.
Locking devices of this type are known. Such locking devices are sometimes used in vehicles (e.g., motor vehicles, etc.) when components are: (1) moveable to different positions; and (2) have to be retained in at least one of these positions counter to a relatively large force (e.g., a force occurring in an accident situation, etc.). For example, in the case of removable vehicle seats, the vehicle seats have to first be retained fixedly in their normal position (i.e. their use position) in which they provide a seat for the vehicle occupants and then they have to be folded over, for example to make it easier for vehicle occupants to get to a rear seat bench or else to enlarge the volume of the loading space. To secure a vehicle seat in such positions, it is known in general to use reversible falling-latch-type locks, in which a hook can either retain or lock a bolt situated on the opposite side or else can unlock it. In such locks, the hook conventionally has two different setting positions, with a hook of this type conventionally “snapping” actively at least into its locking position. This is the case when the bolt on the opposite side enters the region of engagement of the hook, with the result that, by the hook being locked or by it adopting its locking position, a fixed retention or locking is possible. However, it may be possible that the hook will also spring or snap erroneously into the locking position which may be difficult to detect by a user.
Furthermore, in known blocking closures, it is generally the case that a blocking pawl or a blocking cam has to be brought into an open position before the hook is opened or unlocked, but, for correct functioning, it has to be ensured that the bolt on the opposite side of the blocking closure is also actually unlocked (i.e. moves out of the engagement region of the hook). It is possible that again the hook will snap or drop into its locking position without the bolt being locked.
Accordingly, there is a need for a locking device (e.g., a locking device suitable for use with a vehicle seat, etc.) that is simple to manufacture, is compact in terms of construction space (e.g., owing to a vertical arrangement of a hook and blocking element, etc.), can be produced cost-effectively, and which avoids the disadvantages of the prior art.
SUMMARY
One exemplary embodiment relates to a device for locking and/or unlocking a component (e.g., in or on a vehicle seat, etc.) in relation to a mating element. The device includes a locking element and a blocking element. The locking element is configured to be set into a locking position and into an unlocking position. The blocking element is configured to be set into a blocking position and into an actuating position. The setting of the blocking position brings about the setting of the locking position and the setting of the actuating position favors the adoption of the unlocking position.
Another exemplary embodiment relates to a device for locking and/or unlocking a component (e.g., in or on a vehicle, etc.) in relation to a mating element. The device having a locking element and a blocking element. The locking element is configured to be set into a locking position and into an unlocking position. The blocking element is configured to be set into a blocking position and into an actuating position. The setting of the blocking position brings about the setting of the locking position. The device further comprises an ejection element. The ejection element is configured to be set into an ejection position and into a clamping position. The setting of the ejection position brings about an unlocking of the mating element by the locking element. The setting of the clamping position onto the mating element to be locked causes a force which acts in the direction of the unlocking position and opposes a locking. Such a configuration may advantageously reduce the probability of a misuse of the device by a user.
According to an exemplary embodiment, the setting of the ejection position causes the setting of the actuating position. This has the advantageous effect that there is no reduction in the locking security and on the contrary an opening or unlocking of the mating element is possible only after the blocking element is actuated.
According to another exemplary embodiment, the locking element is a hook and, in particular, that the locking element and the blocking element are connected by means of a first spring means. Such a configuration may allow the device to be produced cost-effectively in a simple manner and with particularly simple means.
According to another exemplary embodiment, the locking element is arranged rotatably about a first axis of rotation, and that the blocking element is arranged rotatably about a second axis of rotation. By this means, the elements can be realized with comparatively little friction, thus providing reliable operation of the device.
According to another exemplary embodiment, the device has a guide element, the guide element defining the arrangement of the locking element and of the blocking element relative to each other, in particular defining the first and second axes of rotation. In a particularly advantageous manner, the guide element has the effect that the mating element can only be locked in a single position by the hook or by the locking element. As a result, the reliability of use of the device is increased.
According to another exemplary embodiment, the ejection element is a sliding plate which can be displaced in relation to the locking element and/or the blocking element and is prestressed toward the ejection position by means of a second spring means. Such a configuration may provide a reliable unlocking of the device that can be brought about with extremely simple means.
Another exemplary embodiment relates to a method for locking and/or unlocking a component (e.g., in or on a vehicle, etc.) in relation to a mating element. The component comprises a locking element and an ejection element. The locking element is configured to be set into a locking position and into an unlocking position. The ejection element is configured to be set into an ejection position and into a clamping position. The setting of the ejection position favors the adoption of the unlocking position, and, in order to set the locking position, a force being exerted on the ejection element or on the component by the mating element. Such a configuration may prevent random influences from closing the clamping hook or the blocking hook. Before any locking, a comparatively large force is to be applied in order to set the clamping position of the ejection element or at least in order to move the ejection element out of its ejection position, with the desired locking reliably being ensured following this. Due to the comparatively large application of force in order to set the clamping position, it is unlikely that a user of the component will set the ejection element inadvertently into the clamping position and thereby impair the functionality of the component.
According to an exemplary embodiment, a stop or a first control component of the ejection element blocks the locking element and/or a blocking element if the ejection element is in its ejection position. This enables the effect of the first spring means, which has a tendency to act in the direction of setting the locking position, to be blocked in the ejection position of the ejection element. When carrying out the entire locking of the mating element, the ejection element is brought into its clamping position, with the stop or the first control component of the ejection element first of all releasing the blocking element or the locking element, as a result of which the locking element moves out of the static unlocking position and, in the process, is followed by the blocking element, for example owing to the stressing of the first spring means, until the locking element is set in its locking position.
According to another exemplary embodiment, during the unlocking of the component, the ejection element has, owing to the prestressing of a second spring means, at least an effect assisting the removal of the component from the mating element. In particular, it is advantageously possible as a result that the component can be raised in relation to the mating element, but at least the separation of the two can be assisted.
According to another exemplary element, the locking element is arranged rotatably about a first axis of rotation and the blocking element is arranged rotatably about a second axis of rotation. The ejection element is guided in a manner such that it can move freely parallel to the section connecting the axes of rotation. This can take place in a particularly advantageous and particularly simple manner by means of guide elements.
According to another exemplary embodiment, the component has a blocking element, the blocking element being able to be set into a blocking position and into an actuating position, and in particular the setting of the blocking position causing the setting of the locking position. By this means, the functionality of the component or of the device can be further increased.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of a locking device according to an exemplary embodiment and shown in a locked position.
FIG. 2 is a perspective view of the locking device of FIG. 1 shown in the locked position.
FIG. 3 is another perspective view of the locking device of FIG. 1 shown in an unlocked position.
FIG. 4 is a side view of the locking device of FIG. 1 shown in the unlocked position.
FIG. 5 is a side view of a locking device according to another exemplary embodiment and shown in an unlocked position.
FIG. 6 is a perspective view of the locking device of FIG. 5 shown in the unlocked position.
FIG. 7 is a perspective view of the locking device of FIG. 5 shown in a locked position.
FIG. 8 is a side view of the locking device of FIG. 5 shown in the locked position.
FIG. 9 is a side view of a locking device according to another exemplary embodiment and shown in an unlocked position.
FIG. 10 is a front view of the locking device of FIG. 9 shown in the unlocked position.
DETAILED DESCRIPTION
FIGS. 1 through 10 illustrate a device 2 according to various exemplary embodiments. FIGS. 1 , 2 , 7 and 8 illustrate the device 2 in a locked position, while FIGS. 3 , 4 , 5 , 6 , 9 and 10 illustrate the device 2 in an unlocked position. Further, FIGS. 1 , 4 , 5 , 8 and 9 each illustrate a side view of the device 2 , FIGS. 2 , 3 , 6 and 7 each illustrate a perspective view of the device 2 , while FIG. 10 illustrates a front view of the device 2 .
Referring generally to all of the FIGURES, the device 2 is suitable for use within a vehicle (e.g., a motor vehicle, etc.) and is configured to selectively latch or otherwise lock a component 20 relative to the vehicle. For example, in certain situations, the device 2 may be configured to temporarily lock the component 20 to a mating component (not specially designated). In other situations, the locking is to be cancelled and an unlocked state is to be brought about. It should be noted that in the FIGURES, only a mating element 30 of the mating component is illustrated. Otherwise, the device 2 is essentially completely accommodated on the component 20 or is fastened thereto. In FIG. 1 , the component 20 is indicated by means of a dashed line. The component 20 may be, for example, a seat or another moveable component in or on a motor vehicle.
The device 2 comprises a locking element, shown as a hook 3 , which is configured to rotate, at least within limits, about a first rotational axis 33 . According to various alternative embodiments, the locking element may take a form other than a hook. For example, a slide or the like are also possible for the locking element. However, by way of example, only the embodiment of the locking element as a hook 3 will be described below. The hook 3 can be set in a locking position 31 and in an unlocking position 32 . The locking position 31 of the hook 3 is illustrated in the figures which illustrate the device 2 in its locked position (i.e. FIGS. 1 , 2 , 7 and 8 ). The other FIGURES show the hook 3 in its unlocking position 32 .
The device 2 further comprises a blocking element 4 which, according to the embodiment illustrated, is also rotatably arranged on the device 2 . The blocking element 4 is rotatable, at least within limits, about a second axis of rotation 43 . The blocking element 4 is also referred to as a blocking cam 4 . The blocking element 4 can be set in a blocking position 41 and in an actuating position 42 . The blocking position 41 of the blocking element 4 corresponds to the locking position 31 of the locking element 3 . The blocking position 41 is illustrated in FIGS. 1 , 2 , 7 and 8 . Correspondingly, the actuating position 42 of the blocking element 4 is illustrated in FIGS. 3 , 4 , 5 , 6 , 9 and 10 .
The first axis of rotation 33 and the second axis of rotation 43 are defined by means of a guide element 6 , which is shown in FIGS. 5 , 6 , 8 and 10 (i.e. the guide element 6 defines the positions of the locking element 3 and of the blocking element 4 ), in particular their axes of rotation 33 , 43 , relative to each other. At a distance from the respective axes of rotation 33 and 43 , the locking element 3 includes a first engagement point 34 and the blocking element 4 includes a second engagement point 44 .
A first spring means 35 is arranged between the first engagement point 34 and the second engagement point 44 . The first spring means 35 has a tendency to bring the first engagement point 34 and the second engagement point 44 closer to each other (i.e. biases the first engagement point 34 and the second engagement point 44 toward each other). According to the embodiment illustrated, the lever arm is larger in the direction of force of the first spring element 35 on the blocking element 4 than on the locking element 3 . As such, without other influences, as the locking element 3 and the blocking element 4 rotate about their respective axes of rotation 33 , 43 , the locking element 3 has the tendency, due to the first spring means 35 , to latch into its locking position 31 in which the locking element 3 is held by the blocking element 4 (which is in its blocking position 41 ).
According to an exemplary embodiment, the device 2 further comprises an ejection element 5 which, by means of elongated holes 59 , is arranged displaceably relative to the axes of rotation 33 , 43 and also displaceably relative to the locking element 3 or the blocking element 4 . The ejection element is arranged in a manner such that it is guided by means of guide elements (shown in FIG. 2 ), namely a second guide element 49 connected, in particular, integrally to the blocking element 4 , and a first guide element 39 connected, in particular, integrally to the locking element 3 .
In its lower region 50 , it is possible for the ejection element 5 to be displaced into a region of the mating element 30 locked by the hook 3 when the device 2 is in its unlocked position. This is immediately apparent by a comparison of FIGS. 1 and 4 . The ejection element 5 can likewise be set into two positions, namely into a clamping position 51 and into an ejection position 52 . In FIGS. 1 , 2 , 7 and 8 , the ejection element 5 is set in the clamping position 51 and in the other FIGURES the ejection element 5 is set in the ejection position 52 .
As already indicated, the lower region 50 of the ejection element 5 is in a gripping region of the hook 3 , in which the hook 3 would hold the mating element 30 in the locked position of the device. According to the embodiment illustrated, the ejection element 5 is prestressed in the direction of its ejection position 52 by means of a second spring means 55 . Therefore, if the locking element 3 were moved straight into its unlocking position 32 , the prestressing of the second spring element 55 would cause the mating element 30 to be pushed out of or ejected from the locking region of the hook 3 . For this purpose, the second spring means 55 is connected to the ejection element 5 by means of a third engagement point 54 , and the second spring means 55 is furthermore fastened by means of a fourth engagement point 64 which is situated on the guide element 6 .
Assuming that no mating element 30 is locked in the device 2 , the ejection element 5 is set into its ejection position 52 , which has the effect that a first control component 58 on the ejection element 5 in interaction with a second control component 48 , which is arranged on the blocking element 4 , in particular in the form of a recess, and that the blocking element 4 cannot be moved counterclockwise from its actuating position 42 into its blocking position 41 . This has the consequence that, owing to the effect of the first spring means 35 , the hook 3 likewise remains set in its unlocking position 32 . This is a stable state which is unlikely to be changed even by random influences, such as small dynamic forces, on the hook or on the locking element 3 . If the mating element 30 then comes into the vicinity of the locking region of the locking element 3 , the mating element 30 moves the ejection element 5 from its ejection position into its clamping position or at least in the direction of its clamping position 51 . For this purpose, a force which cannot be disregarded is required, as is illustrated in FIG. 9 by means of the designation F and an arrow. The force required depends on the strength of the second spring means 55 . According to an exemplary embodiment, the force required may approximately 150 N. It is improbable that such a force would act on the specified place by chance. Therefore, a closing of the device arises essentially only on the basis of a movement of the mating element 30 . Such a configuration may reduce malfunctioning of the device 2 .
If the mating element 30 presses with the required force F in the direction indicated in FIG. 9 , the ejection element 5 is moved somewhat in the direction of its clamping position 51 . It is possible, after a certain distance, for the first control means 58 , which is designed in particular as a lug or as a projection of the ejection element 5 projecting into the plane of rotation of the blocking element 4 , for the blocking element 4 to now rotate in the counterclockwise direction ( FIGS. 4 , 5 , 9 ), as a result of which, owing to the action of the first spring means 35 in the above-described manner, a locking both of the blocking element 4 and of the locking element 3 taking place (i.e. the locking element 3 is set into its locking position 31 and the blocking element 4 is set into its blocking position 41 ). This permits a reliable latching or locking of the mating element 30 on the component 20 by means of the device 2 .
If the locking is now released, an actuating device (not illustrated) may be used, for example at the second engagement point 44 of the blocking element 4 , to exert a movement in the clockwise direction of the blocking element 4 (cf. FIGS. 1 , 8 ), i.e. from the blocking position 41 of the blocking element 4 into the actuating position 42 of the blocking element 4 . Movement of the locking element 3 from its locking position 31 into its unlocking position 32 is made possible on account of the shaping both of the locking element 3 and of the blocking element 4 and is also brought about owing to the action of the first spring means 35 , with the setting of the locking element 3 into the unlocking position 32 merely being favored. This in turn has the effect that, by means of the action of the second spring means 55 , the ejection element 5 ejects the mating element 30 out of the locking means of the locking element 3 .
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A device for locking and/or unlocking a component (e.g., in or on a vehicle, etc.) in relation to a mating element is provided. The device comprises a locking element and a blocking element. The locking element is configured to be set into a locking position and into an unlocking position. The blocking element is configured to be set into a blocking position and into an actuating position. The setting of the blocking position brings about the setting of the locking position and the setting of the actuating position favors the adoption of the unlocking position.
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BACKGROUND
Counterflow vortex tubes and their method of operation are well known, such tubes being described, for example, in Fulton U.S. Pat. Nos. 3,173,273 and 3,208,229, and Ranque U.S. Pat. No. 1,952,281. Compressed air (or other gas) from any suitable source enters such a tube and is throttled through nozzles to produce the special temperature change effects which are the unique characteristics of a vortex tube. The result is that the compressed air entering the tube is divided into hot and cold fractions from outlets at opposite ends of the tube. Usually a vortex tube is used for the cold air produced with typical temperatures at the cold air outlet ranging from minus 40° F. to plus 30° F. The air fraction discharged from the hot end is commonly exhausted to atmosphere.
In some applications, such as where a vortex tube is used for cooling the wearer of a protective suit, or a suit (or helmet) worn in a sandblasting operation or in some other industrial operation, some control over the extent of cooling is required to meet the needs or preferences of the wearer. Quite commonly, such control is achieved by providing a valve at the tube's hot end which may be manually adjusted to regulate the proportion of air discharged from the respective ends. Since the temperature reduction of the air discharged from the cold end of the vortex tube varies indirectly with the amount of air flowing therefrom, an adjustment which causes a greater proportion of the compressed air to escape from the cold end (and a lesser proportion from the hot end) would also result in an elevation of the temperature of air from the cold end. However, the reduction in the cooling effect resulting from an increase in the air temperature discharged from the tube's cold end may be offset at least partly by the increased volume of air flowing from the cold end. A user desiring to reduce the cooling effect and adjusting the vortex tube in order to increase the temperature of the air discharged from the tube's cold end might, because of such increased flow, sense that even further adjustment is necessary. Because manual adjustments produce changes in flow as well as temperature, a user may encounter considerable difficulty in selecting a condition of adjustment which provides just the right amount of cooling.
SUMMARY
One aspect of this invention lies in recognizing the aforementioned disadvantage or defect of prior constructions, and, in particular, in recognizing the need for a vortex tube assembly equipped with a control which may be shifted into any selected position along its range of movement to produce corresponding or "sensible" changes in the temperature of the air discharged from the primary outlet of the assembly.
Another object is to provide a vortex tube assembly having an operating handle which may be shifted in any selected position of adjustment to control the temperature of the air discharged from the primary outlet without at the same time substantially altering the rate of flow from that outlet. A still further object is to provide a compact and highly effective assembly equipped with a single operating handle which may be readily adjusted to vary the temperature of the air discharged from the primary outlet over a temperature range extending from maximum hot to maximum cold.
A still further object is to provide a "sensible" control for regulating the temperature of air discharged from a vortex tube; that is, a control which may be shifted into settings anywhere from one extreme position to the other to produce corresponding changes in discharge temperature bearing a generally linear relation with respect to the settings of the control handle.
Briefly, the assembly comprises a basic vortex tube mounted within a housing having a primary outlet and a secondary outlet. A pair of flow-dividing members are disposed within the chamber of the housing, one of the members being movable with respect to the other to regulate the proportions of cold and hot air passing into the respective outlets.
More specifically, a first flow-dividing member is disposed within the chamber of the housing and is provided with a hot air passage receiving air from the hot end of the vortex tube and a cold air passage receiving air from the tube's cold end. A second flow-dividing member is disposed immediately adjacent the first and is provided with a pair of flow passages extending therethrough. One of such flow passages of the second flow-dividing member is in continuous communication with the primary outlet of the housing whereas the other flow passage remains in communication with the secondary outlet. The members are positioned and arranged so that the two flow passages of the second member receive substantially all of the air passing from the hot and cold air passages of the first member, the relative positions of the two members determining the proportions of hot and cold air which each flow passage of the second member receives from the passages of the first member.
In the embodiment illustrated and described, the two members are generally cylindrical and are coaxial with respect to each other and to the vortex tube itself. The first flow-dividing member is provided with an axial recess which rotatably receives an end portion of one outlet tube, preferably the hot air tube, of the vortex tube. The second flow-dividing member is fixed within the housing with opposing end surfaces of the two members in slidable sealing engagement with each other. By rotating the first member relative to the second member so that the flow passage of the latter which communicates with the primary outlet of the assembly receives varying amounts of air from the hot and cold passages of the first member, the temperature of the air discharged from the primary outlet may be varied without significantly altering the volume of air flowing through that outlet.
Other features, objects, and advantages of the invention will become apparent from the drawings and specification.
DRAWINGS
FIG. 1 is a perspective view of a vortex tube assembly embodying the invention, the assembly being equipped with a holder to facilitate the wearing of the device by a user.
FIG. 2 is a broken and somewhat schematic longitudinal sectional view of the assembly.
FIG. 3 is an exploded perspective view of the flow-dividing members of the assembly.
FIG. 4 is similar to FIG. 3 but illustrates other portions of the flow-dividing members.
FIG. 5 is an exploded perspective view schematically illustrating the flow-dividing members in one extreme position of adjustment.
FIG. 6 is a view similar to FIG. 5 but illustrating the members in an intermediate position of adjustment.
FIG. 7 is similar to FIGS. 5 and 6 but illustrates the members in a second extreme position of adjustment.
FIG. 8 is a graph indicating certain performance characteristics of one assembly embodying this invention.
DETAILED DESCRIPTION
Referring to the drawings, FIG. 1 illustrates a vortex tube assembly 10 mounted upon a suitable holder 11 which, in the embodiment illustrated, takes the form of a rectangular piece of leather 12 or other flexible material to which a belt or carrying strap 13 is suitably mounted. Fasteners provided by the belt, one of which is indicated at 14, permit the device to be worn by a user. Flaps or tabs 15 may be partially cut from the leather piece and riveted or otherwise secured to the casing 16 of the vortex tube assembly.
The casing or housing 16 is generally cylindrical in shape and defines a chamber 17 therein (FIG. 2). One end of the casing is closed by end wall 18; the opposite end is provided with an apertured end wall 19 having a neck portion 20 which defines the primary outlet 21 for the assembly. The neck portion may be externally threaded, or may be provided with any other suitable projections or formations, for facilitating the attachment and detachment of a hose adapted to carry air to a wearer's suit or helmet, or to any other article or device requiring cooling. In the illustrated embodiment, end wall 19 is removably mounted within the tubular shell of the casing, being secured therein by screw 22. Leakage of pressurized air is prevented by resilient sealing ring 23.
A conventional vortex tube 24 is mounted within casing 16. Vortex tube 24 is similar to the vortex tubes disclosed in the aforementioned patents, having a cylindrical generator body 25, a tubular hot air outlet 26 coaxial with the body and projecting from one end thereof, and a tubular cold air outlet 27 also coaxial with the body and projecting from the opposite end thereof. As shown in FIG. 2, the vortex tube is coaxial with the cylindrical casing 16 with the tubular hot air outlet facing towards the primary outlet 21 and the tubular cold air outlet facing towards, but spaced from, end wall 18. If desired, however, the position of the vortex tube may be reversed with the hot air outlet tube 26 facing end wall 18.
A laterally-projecting inlet fitting 28 communicates with the generator body 25 of the vortex tube 24, the fitting being threadedly secured to both the casing and the generator body as indicated in FIG. 2. Fitting 28 is adapted to be connected to a source of pressurized gas and, more particularly, to a line or hose extending to a compressor or other source of pressurized air. For most applications, the pressure of the air supplied to the vortex tube through fitting 28 will fall within the range of about 80 to 120 psig.
Reference may be had to the aforementioned patents for details concerning the structure and operation of vortex tube 24. For purposes of fully disclosing the present invention, it is believed sufficient to state that the vortex tube 24 operates to divide a stream of compressed air (or other gas) entering the body of the tube through inlet 28 into hot and cold fractions, the hot fraction being discharged axially from the free end of outlet tube 26 and the cold fraction being discharged from the free end of outlet tube 27. By controlling the relative dimensions of the parts, the proportions of the respective fractions, and the maximum/minimum temperatures of those fractions, may be established as desired. Preferably, vortex tube 24 should be constructed so that the rate of discharge from the hot and cold ends is approximately equal.
The casing contains a pair of flow-dividing members 30 and 31 for controlling the temperature of the air discharged from primary outlet 21. As shown most clearly in FIGS. 3 and 4, each member is generally cylindrical in configuration. Except for certain modifications described hereinafter, the two members are essentially the same in construction and, if desired, may be formed in the same mold with certain distinctive changes or additions made thereafter in each of them.
Each member 30, 31 has a planar end face 32 which extends along a plane normal to the axis of the member and which is adapted to make sealing contact with the same end face of the other member when the members are reversely oriented as indicated in FIGS. 2 and 3. In the illustration given, each of the flow-dividing members has a pair of passages 33 and 34 extending axially inwardly from end face 32 and divided by a generally diametrically oriented septum 35. Referring to FIG. 3, it will be seen that the septum 35 radiates outwardly from a central hub portion 36 and merges with an annular outer wall 37, with the result that each of the passages 33 and 34 is of arcuate configuration.
Only one of the arcuate passages 34 extends completely through each member, opening through the opposite end face 38 thereof (FIG. 4). The other arcuate passage 33, in the case of member 31, opens laterally outwardly through opening 39 in side wall 37 and, in the case of member 30, opens laterally inwardly into the recess 40 of hub 36 through opening 41 (FIGS. 2 and 4). As indicated in FIG. 2, the central recess 40 in hub 36 of member 30 snugly but rotatably receives the end portion 26a of outlet tube 26 of the vortex tube 24. Consequently, the arcuate passage 33 of member 30 is in direct flow communication with outlet tube 26 and, since that tube constitutes the hot air outlet for the vortex tube, the arcuate flow passage 33 of member 30 functions as a hot air passage. Conversely, the other arcuate passage 34 of member 30 serves as a cold air passage since it communicates with outlet 27 of the vortex tube through the interior of the casing external to the vortex tube (FIG. 2).
More specifically, referring to FIG. 2, it will be observed that the free end of the cold air outlet 27 of the vortex tube is spaced from end wall 18 of the casing, the end wall serving as a deflector to reverse the direction of flow of cold air discharged from the vortex tube. Since the outside dimensions of generator body 25 are smaller than the inside cross sectional dimensions of the casing, cold air deflected by end wall 18 is directed towards the opposite end of the casing through filter 42 and into the arcuate cold air flow passage 33 of flow-dividing member 30. Such reversed direction of flow is indicated by arrows 43 in FIG. 2.
Hot air from the vortex tube's hot air outlet 26 follows the direction of flow indicated by arrows 44 in FIG. 2. After leaving the outlet of the vortex tube, such hot air flows into axial recess 40 of member 30, then laterally through port or opening 41 and into arcuate hot air flow passage 33 of member 30.
If desired, a suitable noise muffling element, such as fine-mesh folded screening 45, may be mounted within the arcuate passage 33 of member 30. The screening not only provides a noise muffling function but also distributes the hot air more evenly through arcuate passage 33.
Member 42 also performs sound-suppressing functions, and can be formed of open-celled foam, folded screening or open-mesh fabric, or any other suitable porous material. Open-celled foam such as polyurethane foam has been found particularly effective.
As already stated, member 31 is reversely oriented with respect to member 30. Air flowing into passage 34 of member 31 may continue completely through member 31 into the chamber portion 17a of the casing, exiting from that chamber portion through the primary outlet 21. Gas entering the other arcuate passage of the member 31 exits laterally outwardly through aligned openings 39 and 47 in the member 31 and casing 16, respectively. A projection 48 from end 38 of member 31 is received within a recess provided by end wall 19 of the casing, thus keying or locking the two parts together and, since the end wall is fixed by screw 22 against rotation with respect to the casing, member 31 is effectively held against rotation within casing chamber 17. Thus, the opening 39 in the side wall of member 31 is held in alignment with opening 47 of the casing, such lateral opening serving as a secondary outlet for the vortex tube assembly.
A suitable muffling element 49 may be mounted within the arcuate flow passage 33 of flow-dividing member 31, as shown most clearly in FIG. 2. Such element may take the form of folded screening and may be identical to element 45 disposed in flow-dividing member 30.
A helical compression spring 50 is disposed within chamber portion 17a of the casing to maintain the two flow-dividing members 30 and 31 in firm engagement with each other (FIG. 2). It will be observed that member 30 is held against axial movement away from spring 50 by the hot air outlet tube 26 of the vortex tube upon which it is journaled, the vortex tube in turn being secured against axial displacement within the chamber by means of compressed air inlet fitting 28. Consequently, the spring not only holds the flow-dividing members with their end faces 32 in sliding and sealing engagement, but also helps to maintain an effective seal between the recess 40 of member 30 and the outlet tube 26 of vortex tube 24.
Although member 31 is fixed against rotation within chamber 17, member 30 may be rotated approximately 180° by means of a handle or lever 51 which projects radially outwardly through semi-circumferential slot 52 in casing 16 (FIG. 1). It is the rotational movement of flow-dividing member 30 relative to flow-dividing member 31 that results in a full range of adjustment of the air discharge temperatures through primary outlet 21 from maximum cold to maximum hot.
The operation is graphically depicted in FIGS. 5 through 7, with only the flow-dividing members 30 and 31 being shown, such members being illustrated in axially-spaced relation for purposes of illustration although it is to be understood that in actual operation their opposing end faces 32 would be held in mutual sliding sealing engagement. Member 31 is fixed against rotation with its arcuate flow passage 34 in continuous communication with primary outlet 21, and with its other arcuate flow passage 33 (not visible in FIGS. 5-7) in continuous communication with the secondary outlet through lateral opening 39.
Although the other flow-dividing member 30 is rotatable, its two flow passages 33 and 34 remain in constant communication with the hot and cold ends of the vortex tube, respectively. Passage 33 of member 30 is always a hot air passage and, conversely, passage 34 of that member is always a cold air passage. By rotating member 30 over its 180° arc of movement, hot air (represented by shaded arrows in FIGS. 5-7) flowing through the hot air passage 33 of member 30 is either directed entirely into arcuate passage 33 of member 31 (from which it is laterally discharged through opening 39, as shown in FIG. 5), or is directed entirely into arcuate passage 34 of member 31 (FIG. 7), or is divided so that some of it flows through each of the passages of member 31, the proportional amounts depending on the rotational position of member 30 (FIG. 6). Similarly, cold air (represented by dotted arrows in FIGS. 5-7) is directed entirely into passage 34 of member 31 (FIG. 5), or entirely into the other arcuate passage and out through lateral opening 39 (FIG. 7), or is divided between the two arcuate passages of member 31 (FIG. 6).
It is believed apparent that the vortex tube assembly may be easily adjusted by means of the single handle lever 51 to vary the air temperature at the primary outlet 21--the outlet which discharges air to be used by the user--to provide any selected temperature over the full range which the vortex tube is capable of generating. Furthermore, the adjustability is "sensible"; that is, incremental variations in the handle position may be relied upon to produce corresponding incremental variations in discharge temperature without significant changes in air flow volume.
FIG. 8 is a graph showing the performance characteristics of a vortex tube assembly operated with air at 100 psig and showing the results at each of nine settings from maximum cold air discharge to maximum hot air discharge. The handle settings were equally spaced so that setting "4" was the mid point between the two extremes. At each setting, the output temperature (the temperature of air discharged from primary outlet 22) was measured after allowing three minutes of operation for purposes of stabilization. Line 55 shows the output temperature at each of the settings from a minimum temperature of 30° F. to a maximum temperature of 90° F. It will be observed that a state of linearity is closely approached with temperature variations falling within 4° F. from a straight line 56.
The output flow from the primary outlet 21 remained relatively constant over the full range of incremental positions, as indicated by line 57. Specifically, line 57 reveals that the output flow in cubic feet per minute for all nine settings was 13.05 SCFM±9%. While results may vary depending on design variations of the vortex tube assembly, it is believed that the results depicted in FIG. 8 are fairly representative and that even better results are possible. For most purposes, particularly for air conditioning flight suits, work suits, helmets, and the like, the performance characteristics represented in FIG. 8, would be highly acceptable. Since such performance is achievable by a device having only a single operating lever which may be readily manipulated by the user, it is believed apparent that this assembly is especially suitable for industrial use.
While in the foregoing I have disclosed an embodiment of the invention in considerable detail for purposes of illustration, it will be understood by those skilled in the art that many of these details may be varied without departing from the spirit and scope of the invention.
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A vortex tube assembly equipped with a control mechanism for use in selectively adjusting the temperature of air discharged from the primary outlet of the assembly to any temperature within the range from maximum hot to maximum cold, the temperature of the discharged air varying in generally linear relation with adjustments in the position of a temperature control handle. Ideally, the temperature of the discharged air may thus be varied without significantly altering the rate of flow through the primary outlet. The assembly includes a vortex tube disposed within a cylindrical housing having primary and secondary outlets, and a pair of flow-dividing members within the housing, at least one of which is movably mounted, for controlling the temperature of the air discharged from the primary outlet by altering the proportions of hot and cold air flowing through the passages of such members.
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FIELD OF THE INVENTION
The present invention relates to a method and delivery device for delivering a substance, such as a drug or pharmaceutical agent transdermally to a patient. More particularly, the invention is directed to a device containing a diluent for delivering a reconstituted drug transdermally to a patient.
BACKGROUND OF THE INVENTION
Various devices have been proposed for transdermally delivering pharmaceutical agents, drugs and other substances. Although the subcutaneous delivery methods using a standard cannula are effective for many applications, the pain normally induced by the cannula has prompted the development of less painful delivery methods.
The use of prefilled syringes and other delivery devices has increased significantly in recent years due in part to the convenience and reduced risk of contamination. Prefilled syringes are generally suitable for drug solutions that are stable for extended periods of time. The drug solution itself must be stable and the solution must not interact with the syringe barrel or other container during storage. Certain drugs are inherently unstable in solution and are normally stored as a dried or lyophilized powder that must be reconstituted prior to use. These drugs are not suitable for standard prefilled syringes.
A method that has received much attention in recent years is the delivery of drugs through the skin by forming micropores or cuts through the stratum corneum. By penetrating the stratum corneum and delivering the drug to the skin in or below the stratum corneum, many drugs can be effectively administered. The devices for penetrating the stratum corneum generally include a plurality of micron size needles or blades having a length to penetrate the stratum corneum without passing completely through the epidermis. Examples of these devices are disclosed in U.S. Pat. No. 5,879,326 to Godshall et al.; U.S. Pat. No. 5,250,023 to Lee et al., and WO 97/48440.
The skin is made up of several layers with the upper composite layer being the epithelial layer. The outermost layer of the skin is the stratum corneum which has well known barrier properties to prevent molecules and various substances from entering the body and analytes from exiting the body. The stratum corneum is a complex structure of compacted keratinized cell remnants having a thickness of about10-30 microns.
The natural impermeability of the stratum corneum prevents the administration of most pharmaceutical agents and other substances through the skin. Numerous methods and devices have been proposed to enhance the permeability of the skin and to increase the diffusion of various drugs through the skin so that the drugs can be utilized by the body. Typically, the delivery of drugs through the skin is enhanced by either increasing the permeability of the skin or increasing the force or energy used to direct the drug through the skin.
One example of a method for increasing the force for the delivery of drugs through the skin include iontophoresis. Iontophoresis generally applies an external electrical field to ionize the drug, thereby increasing the diffusion of the drug through the skin. However, it can be difficult to control the amount and rate of drug delivery using iontophoresis. Under some circumstances, iontophoresis can cause skin damage depending on the extent of ionization, the energy applied to ionize the drug and duration of the treatment.
Sonic, and particularly ultrasonic energy, has also been used to increase the diffusion of drugs through the skin. The sonic energy is typically generated by passing an electrical current through a piezoelectric crystal or other suitable electromechanical device. Although numerous efforts to enhance drug delivery using sonic energy have been proposed, the results generally show a low rate of drug delivery.
The prior methods and apparatus for the transdermal administration of drugs has exhibited limited success. Accordingly, a continuing need exists in the industry for an improved device for the administration of various drugs and other substances.
SUMMARY OF THE INVENTION
The present invention is directed to a method and device for the transdermal delivery of a substance, such as a drug, vaccine or other pharmaceutical agent, to a patient. In particular, the invention is directed to a method and device for delivering a pharmaceutical agent to the stratum corneum of the skin to a sufficient depth where the pharmaceutical agent can be absorbed and utilized by the body.
Accordingly, a primary object of the invention is to provide a method and device for reconstituting a pharmaceutical agent and administering the pharmaceutical agent transdermally through the skin substantially without pain to the patient.
Another object of the invention is to provide a prefilled delivery device having a reservoir containing a substance and a plurality of microneedles or blades for penetrating the stratum corneum of the skin for delivering the substance to the skin.
A further object of the invention is to provide a device having a dried pharmaceutical agent and a reservoir containing a diluent for reconstituting the dried pharmaceutical agent and delivering the pharmaceutical agent to the patient.
Another object of the invention is to provide a device having a bladder containing a substance and a cannula for piercing the bladder to dispense the substance and deliver the substance to the patient.
A further object of the invention is to provide a device for the transdermal delivery of a substance where the apparatus includes a bladder containing the substance, a cannula to pierce the bladder and a protecting shield to prevent premature piercing of the bladder.
A still further object of the invention is to provide a device for the transdermal delivery of a pharmaceutical agent having a plurality of microneedles for penetrating the stratum corneum and a bladder containing the pharmaceutical agent for delivering the pharmaceutical agent to the microneedles.
Another object of the invention is to provide a device having a plurality of microneedles for penetrating the stratum corneum and an outer adhesive patch for adhesively attaching the apparatus to the skin of a patient.
Still another object of the invention is to provide a transdermal delivery device having an array of microneedles for penetrating the stratum corneum of the skin, a flexible bladder containing a substance and flexible cover that can be deflected toward the bladder to dispense the substance to the microneedles.
A further object of the invention is to provide a device for the transdermal delivery of a substance to a patient where the device has an array of microneedles and a dried substance on the microneedles, where the dried substance is reconstituted by dispensing a diluent from a bladder within the device.
These and other objects of the invention are substantially attained by providing an intradermal delivery device for introducing a substance into the skin of a patient. The device comprises a housing having a central opening and a planar member positioned in the central opening of the housing. The planar member has an inner surface and an outer surface. The outer surface has a plurality of microneedles extending therefrom, at least one opening passing through the planar member from the inner surface to the outer surface, and at least one cannula on the inner surface. A flexible cover is coupled to the housing and overlies the central opening and is spaced from the planar member to define a cavity in the housing. A bladder containing at least one substance is positioned in the cavity of the housing between the planar member and the flexible cover. The bladder is piercable by the cannula and is collapsible by pressing the flexible cover to dispense the substance through the opening to the microneedles.
The objects and advantages of the invention are further attained by providing an intradermal device for administering a pharmaceutical agent through the skin of a patient. The device comprises a housing having a bottom wall and at least one side wall defining a cavity. The bottom wall has a plurality of microneedles and a plurality of passages extending through the bottom wall to the microneedles. A flexible cover is coupled to the housing and encloses the cavity. The flexible cover has a generally arcuate shaped outer surface in a first position and is movable from the first position to a second position toward the bottom wall. A bladder contains a substance and the bladder is positioned in the cavity and is collapsible by applying pressure to the flexible cover to dispense the substance through the passages in the bottom wall to the microneedles.
Another object of the invention is to provide a method of administering a substance such as a pharmaceutical agent through the skin of a patient which comprises providing a delivery device having a housing with a bottom wall and at least one side wall defining a cavity. The bottom wall has an outer surface with a plurality of microneedles extending therefrom and has a plurality of passages extending through the bottom wall from the cavity to the microneedles. A bladder contains at least one substance and is positioned in the cavity, and a flexible cover encloses the cavity. The device contacts the skin of a patient and sufficient pressure is applied to the device to cause the microneedles to penetrate the skin a sufficient depth for delivering a substance to the patient. Sufficient pressure is applied to the flexible cover to rupture the bladder and dispense the substance to the microneedles.
The objects, advantages and other salient features of the invention will become apparent from the following detailed description which, taken in conjunction with the annexed drawings, discloses preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The following is a brief description of the drawings in which:
FIG. 1 is a top view of the transdermal delivery device in accordance with a first embodiment of the invention;
FIG. 2 is a cross-sectional view of the transdermal delivery device of FIG. 1;
FIG. 3 is a perspective view of the transdermal delivery device of FIG. 1;
FIG. 4 is a side view in cross-section of a transdermal delivery device of FIG. 1 showing the outer cover and bladder depressed;
FIG. 5 is a side elevational view in cross-section of a second embodiment of the invention;
FIG. 6 is side elevational view in cross-section of the delivery device in a third embodiment of the invention;
FIG. 7 is a partial side view of the transdermal delivery device in a fourth embodiment of the invention;
FIG. 8 is a partial top view of the embodiment of FIG. 7; and
FIG. 9 is a partial cross-sectional side view of the embodiment of FIG. 7 showing the bladder pierced by the cannula.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is directed to an intraepidermal delivery device for administering a substance to a patient. More particularly, the invention is directed to a prefilled delivery device containing a drug solution or diluent for a dried drug and to a method for administering the drug solution or a reconstituted drug solution into or below the stratum corneum of the skin of a patient. Intradermal refers to one or more layers within the skin and is not limited to the dermis layer of the skin.
The device and method of the present invention are particularly suitable for use in administering various substances, including pharmaceutical agents, to a patient, and particularly to a human patient. As used herein, a pharmaceutical agent includes a substance having biological activity that can be delivered through the body membranes and surfaces, and particularly the skin. Examples include various drugs, such as antibiotics, antiviral agents, analgesics, anesthetics, anorexics, antiarthritics, antidepressants, antihistamines, anti-inflammatory agents, antineoplastic agents, vaccines, including DNA vaccines, adjuvants, biologics, and the like. Other substances which can be delivered intradermally to a patient include proteins, peptides and fragments thereof. The proteins and peptides can be naturally occurring, synthesized or recombinantly produced.
The invention is directed to a delivery device 10 having a housing 12 , a plurality of microneedles 14 and a prefilled bladder 16 as shown in FIGS. 1-4. The invention is further directed to a method of delivering a substance to a patient using the delivery device 10 .
Referring to FIGS. 1-4, the housing 12 of device 10 in this embodiment has a generally circular shape having a central opening 18 defining an inner wall 20 . Housing 12 is preferably made of a flexible plastic or rubber-like material that is non-reactive to the substance being delivered to the patient. In the embodiment illustrated, the microneedles 14 are integrally formed with a planar member 22 that is dimensioned to fit within the central opening 18 . Planar member 22 preferably has a shape corresponding to the shape of central opening 18 and fits securely against inner wall 20 . An outer edge 24 of planar member 22 abuts inner wall 18 to form a fluid tight seal. In one embodiment of the invention, the planar member 22 is attached to the inner wall 20 by a suitable adhesive or other suitable bonding method. As shown in FIG. 2, planar member 22 is positioned in the central opening 18 of housing with the microneedles 14 facing outwardly beyond the housing 12 to ensure complete contact with the skin of the patient as discussed hereinafter in greater detail.
Housing 12 in the embodiment shown in FIGS. 1-4 is sufficiently flexible to conform to the contour of the patient's skin. In other embodiments, the housing can be made of a rigid material. A bottom surface 26 of housing 12 preferably includes a pressure sensitive adhesive 28 for attaching housing 12 to the skin of a patient during use. The pressure sensitive adhesive 28 can be a suitable adhesive as known in the art that is commonly used in adhesive bandages. The adhesive layer 28 preferably encircles the central opening 18 and is able to form a substantially fluid tight seal around the central opening 18 and microneedles 14 .
Planar member 22 forms a bottom wall of housing 12 having the microneedles 14 facing outwardly from the housing 12 . In the embodiment illustrated, microneedles 14 are integrally formed with the planar member 22 . In alternative embodiments, a separate bottom wall can be provided and a second member having microneedles formed thereon can be superimposed.
As shown in FIG. 1, a flexible film 42 of a sheet material is attached to the housing 12 . Film 42 has a dimension to extend beyond the dimension of the housing 12 in opposite directions. Film 42 includes an adhesive coating for attaching delivery device 10 to the skin of a patient in a manner similar to an adhesive bandage strip.
Delivery device 10 is generally made from a plastic material that is non-reactive with the substance being administered. Suitable plastic materials include, for example, polyethylene, polypropylene, polyesters, polyamides and polycarbonates as known in the art. The microneedles can be made from various materials by methods as known in the art. For example, microneedles can be made from silicon, stainless steel, tungsten steel, alloys of nickel, molybdenum, chromium, cobalt, and titanium, ceramics, glass polymers and other non-reactive metals, and alloys thereof.
The length and thickness of the microneedles are selected based on the particular substance being administered and the thickness of the stratum corneum in the location where the device is to be applied. In one embodiment, the microneedles penetrate the stratum corneum substantially without penetrating or passing through the epidermis. The microneedles can have a length for penetrating the skin up to about 250 microns. Suitable microneedles have a length of about 5 to 200 microns. Typically, the microneedles have a length of about 5 to about 100 microns, and generally in the range of about 10 to 40 microns. The microneedles in the illustrated embodiment have a generally conical shape. In alternative embodiments, the microneedles can be triangles, flat blades or pyramids. Typically, the microneedles are perpendicular to the plane of the device. The width of the microneedles can be about 15 to 40 gauge to obtain optimum penetration of the skin.
The microneedles 14 are generally formed in uniformly spaced rows and columns to form an array. The microneedle array generally has a surface area of about 0.5 to about 5.0 cm 2 . The spacing between the rows and columns can be varied depending on the substance being administered and the desired dosage. In one embodiment, the microneedles are spaced apart a distance of about 0.05 mm to about 5.0 mm.
In the embodiment of FIGS. 1-4, microneedles 14 include a hollow passage 30 extending axially through each microneedle 14 and planar member 22 . Passage 30 of each microneedle is dimensioned to allow fluid to pass through the microneedles to the tips 32 of the microneedles for delivery to the skin surface.
A generally domed shaped cover member 34 is attached to a top surface 36 of housing 12 to completely cover central opening 18 and define a cavity 38 within housing 12 . As shown in FIG. 2, cover member 34 has a dimension slightly larger than the dimension of central opening 18 and has a generally convex outer surface 40 . Cover member 34 is preferably made of a plastic sheet material that is sufficiently flexible to be flexed in a generally downward direction. In one embodiment, cover member 34 is made of material that has sufficient memory to return to its domed shape and can be depressed to snap to an inverted concave shape.
Flexible bladder 16 is positioned in cavity 38 of housing 12 . Bladder 16 is preferably a sealed bulbous shaped member made from a flexible material that can conform to the shape of cavity 38 and can be depressed to dispense the contents. Bladder 16 is prefilled with a desired substance before the delivery device is assembled.
A cannula 44 is provided on the top surface 46 of planar member 22 as shown in FIG. 2 . In the embodiment illustrated, three cannulas 44 are positioned to face toward bladder 42 , although the number used can vary as needed. Cannula 44 has a generally flat base 46 and a pointed tip 48 that is capable of piercing the bladder. Cannula 44 can be made of suitable metal or plastic having sufficient strength to pierce bladder 42 . As shown in FIG. 2, cannula 44 is a separate element that is attached to planar member 22 . In alternative embodiments, cannula 44 can be integrally formed with planar member 22 . Typically, cannula 44 has a generally conical shape, although can be any suitable shape capable of piercing bladder 16 .
Bladder 16 can contain a drug solution or other substance to be delivered to the patient. Preferably, bladder 16 is dimensioned to contain a premeasured dosage for the particular drug solution being administered.
In further embodiments, bladder 16 contains a diluent or carrier for reconstituting a substance to be delivered to the patient. The diluent can be, for example, distilled water or saline solution. In a preferred embodiment, a dried drug is provided as a coating on the outer surfaces of the microneedles. In further embodiments, the dried drug can be a coating on the top surface of planar member 22 or in passages 30 . In this embodiment, the dried or lyophilized drug or pharmaceutical agent is dissolved or dispersed in the diluent and delivered to the patient. This embodiment is particularly suitable for unstable drug solutions.
Delivery device 10 is produced as a complete, prefilled unit for delivery of a substance to a patient. The device can include a protective cover (not shown) over microneedles 14 to prevent damaging or contamination of the microneedles during storage and shipping. Similarly, a protective release liner (not shown) can be applied over the adhesive and the device packaged in a suitable packaging material commonly used for medical devices.
The primary barrier properties of the skin including the resistance to drug penetration reside in the outermost layer of the skin, referred to as the stratum corneum. The inner layers of the epidermis generally include three layers, commonly identified as the stratum granulosum, the stratum malpighii, and the stratum germinativum. Once a drug or other substance penetrates below the stratum corneum, there is substantially less resistance to permeation into the subsequent layers of the skin and eventual absorption by the body. Thus, delivery of a substance below the stratum corneum can be an effective system for administering some substances, and particularly some vaccines, to the body. The delivery device of the invention is able to deliver a substance into or below the stratum corneum where it can be utilized by the body. Preferably, the device and method of the invention pierce the stratum corneum substantially without penetrating the dermis to target the tissue layers below the stratum corneum. As used herein, the term penetrate refers to entering a layer of the skin without necessarily passing completely through. Piercing refers to passing completely through a layer of the skin. As used herein, transdermal refers to the delivery of a substance, such as a pharmaceutical, biological agent or vaccine, through one or more layers of skin.
In use, delivery device 10 is removed from its packaging and the release sheet, if provided, is separated to expose the adhesive layer on the bottom face of the device. Delivery device 10 is positioned on the desired location of the skin 48 and pressed in place with a gentle downward pressure until the microneedles penetrate the outermost layer of skin and the adhesive layer contacts the skin and forms a seal around the microneedle array. A gentle rubbing motion also can be applied to delivery device 10 to assist in the penetration of the skin by the microneedles 14 . Cover member 34 is then pushed downwardly in the direction of arrow 50 as shown in FIGS. 3 and 4 with sufficient pressure to cause cannula 44 to pierce bladder 16 . The pressure is applied to cover member 34 and bladder 16 to collapse the bladder and force the contents of the bladder into cavity 38 and through passages 30 to tips 32 of the microneedles 14 . Preferably, adhesive layer 28 on the bottom of housing 12 and film 42 form a seal to contain the drug solution or other substance in the target area of the microneedle array where it can penetrate the stratum corneum and be absorbed by the body.
Generally, the pressure applied to cover 34 is sufficient to enable a drug solution to flow to the tips of the microneedles 14 where the drug solution is available for absorption by the skin. In further embodiments, cover member 34 can be made of stiff plastic material so that when pressed, the dome shaped cover member snaps to an inverted position and retains the inverted position to maintain a constant force on the bladder. In this manner, a constant pressure can be produced to deliver the substance to the microneedles.
Embodiment of FIG. 5
FIG. 5 shows a second embodiment of the delivery device 52 . Delivery device 52 is similar to the embodiment of FIGS. 1-4 and includes a housing 54 having a central opening 56 , a bottom surface 58 and a top surface 60 . Bottom surface 58 is preferably provided with a layer of a pressure sensitive adhesive 62 that encircles central opening 56 . A flexible film 64 having an adhesive 66 is attached to top surface 60 of housing 54 for attaching delivery device 52 to the skin 68 of a patient.
A planar member 70 is formed with an array of microneedles 72 . Microneedles 72 are provided with an axial hollow passage 74 extending through planar member 70 . A bladder 75 contains a drug solution, diluent or other substance as in the previous embodiment. A cannula 76 is provided on the top surface of planar member 70 , and a flexible cover 78 is attached to housing 54 to enclose a cavity 80 .
In the embodiment of FIG. 5, an indicator device 82 is provided in housing 54 for indicating proper contact of the microneedle array with skin 68 of the patient. In the embodiment illustrated, indicator device 82 is an electrical device that contacts the skin when sufficient downward pressure is applied to delivery device 52 . Indicator device 82 includes a pair of electrodes 84 connected by leads extending from the bottom surface 62 of housing 54 to top surface 60 . Electrodes 84 are coupled to a power source 86 having a visual indicator 88 , such as, for example, a liquid crystal display or liquid crystal diode.
Delivery device 54 is applied to skin 68 of a patient with a downward pressure until electrodes 84 contact skin 68 . The conductivity of the patient's skin completes the electrical circuit between electrodes 84 to actuate indicator 88 thereby providing an indication that sufficient pressure is applied for microneedles 72 to penetrate the skin a sufficient depth for delivery of the drug solution. Cover member 78 is then depressed to pierce bladder 75 by cannula 76 and dispense the contents of bladder 75 .
In the embodiment illustrated, the indicator device is an electrical device that relies on the electrical conductivity of the skin of the patient. In further embodiments, the indicator can be a pressure sensor device or other suitable devices capable of providing an indication that sufficient pressure is applied to the microneedle array.
Embodiment of FIG. 6
FIG. 6 shows a delivery device 92 in a further embodiment of the invention. Delivery device 92 is similar to the delivery device 10 of FIGS. 1-4 except for the array of microneedles 94 . Accordingly, identical components are identified by the same reference number with the addition of a prime.
The microneedle array 94 is formed on a bottom surface of a planar member 96 . As in the previous embodiments, the planar member 96 is coupled to housing 12 ′ in the central opening 14 ′ to define a cavity. A plurality of passages 98 extend through the planar member 96 from the cavity to the outer face. In this embodiment, microneedles 94 are solid structures and passages 98 terminate substantially at the base of the microneedles and between adjacent microneedles 94 .
Delivery device 92 is used in substantially the same manner of the previous embodiments. Delivery device 92 is positioned on the skin and rubbed or pressed gently to enable microneedles 94 to penetrate the skin. Cover member 34 ′ is then pressed to cause bladder 16 ′ to be pierced by cannula 44 ′. The substance contained in the bladder 16 ′ is then dispensed and directed to passages 98 to microneedles 94 . As in the previous embodiments, bladder 16 ′ can contain a drug solution or a diluent to dissolve a dried drug in the cavity 38 ′ or on the surface of the microneedles 94 .
Embodiment of FIGS. 7 - 9
A delivery device 100 in a further embodiment is shown in FIGS. 7-9. Delivery device 100 is similar to delivery device 10 of the embodiment of FIGS. 1-4, except for a protecting shield device 102 that cooperates with a cannula 104 . Accordingly, identical components are identified by the same reference number with the addition of a prime.
As in the previous embodiment, delivery device 100 includes a planar member 22 ′ having an array of microneedles 14 ′ on a bottom surface of the planar member 22 ′. Microneedles 14 ′ include an axial passage 30 ′ that extends through planar member 22 ′ to cavity 38 ′.
The protecting member 102 is a supporting or cradle-like device that is positioned in the upper surface of planar member 22 ′ to shield cannula 104 for preventing or resisting premature rupturing and piercing of bladder 16 ′. As shown in FIGS. 6 and 7, protecting member 100 includes a base 106 having an outer edge 108 and has a height greater than a height of cannula 104 . In the embodiment illustrated, base 106 is a flat circular member, although the actual shape of the base can be varied depending on the particular needs of the device.
A cannula 104 is coupled to base 106 and extends in a generally upward direction away from planar member 22 ′ toward bladder 16 ′. Cannula 104 in the embodiment illustrated is a separate member coupled to base 106 by a suitable adhesive, welding or the like. In alternative embodiments, cannula 104 can be integrally formed with the base. Cannula 104 has a generally conical shape converging to a sharp tip 110 suitable for piercing bladder 16 ′.
A resilient arm 112 has a first end 114 coupled to the base 106 and a second end 116 extending away from the base 106 . In the embodiment of FIGS. 7-9, four arms 112 are coupled to the base 106 and extend at an incline toward the tip 110 of cannula 104 . The arms 112 are positioned such that the second free ends 116 of arms 112 assume a normal position above tip 110 of cannula 108 as shown in FIG. 7 . Arms 112 surround tip 110 of cannula 104 and support bladder 16 ′ above cannula 104 to prevent bladder 16 ′ from contacting cannula 104 during shipping and storage. In the embodiment illustrated, arms 112 are integrally formed with base 106 , although in other embodiments, the arms 112 can be separate members that are assembled together.
The delivery device 100 is used in a manner similar to the previous embodiments. Delivery device 100 is positioned on the skin 118 of the patient and gently rubbed and pressed against skin 118 and secured in place by the adhesive. Cover member 34 ′ is then pushed downwardly to push bladder 16 ′ toward cannula 104 . Arms 112 of protecting member 102 are sufficiently flexible that downward pressure on cover member 34 ′ and bladder 16 ′ pivots free end 116 of arms 112 toward base 106 to enable cannula 104 to pierce bladder 16 ′ as shown in FIG. 9 to dispense the contents of the bladder.
The delivery devices of the invention are generally intended for single use and contain a selected dose for the substance being delivered to the patient. The adhesive film is able to hold the delivery device in place with minimal discomfort for extended periods of time. The length of time the delivery device remains in contact with the skin can vary from several minutes to several hours. Various factors that determine the length of time the delivery device remains in contact with the skin include, for example, the depth of penetration, the volume of the substance being delivered, and the absorption rate of the substance.
While several embodiments have been shown to illustrate the present invention, it will be understood by those skilled in the art that various changes and modifications can be made therein without departing from the scope of the invention as defined in the appended claims.
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A device for delivering a substance into the skin of a patient includes a housing and a plurality of microneedles for penetrating the skin. The housing includes a bottom wall with a plurality of apertures for supplying the substance to the microneedles. The housing also includes a flexible top cover member enclosing a bladder containing the substance to be delivered. The bottom wall of the housing has at least one cannula facing the bladder. Pressing on the top cover member causes the cannula to puncture the bladder and deliver the substance to the microneedles for delivery to the patient. In one embodiment, the cannula is surrounded by a flexible member to prevent piercing of the bladder until sufficient pressure is applied to the cover member to depress the flexible member.
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This is a divisional of now abandoned application Ser. No. 08/119,642, filed Sep. 13, 1993, abandoned, which in turn is a divisional of application Ser. No. 07/743,225, filed Aug. 9, 1991, now U.S. Pat. No. 5,274,555.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle such as an automobile or the like by use of an electric motor in correspondence to the running state of the vehicle, i.e., a turning angle of a steering wheel, etc.
2. Description of the Prior Art
Vigorous research and development has been directed to a four-wheel steering system to steer the rear wheels of a vehicle corresponding to the vehicle running state, and some systems have actually been put to practical use.
In a four-wheel steering system now in practical use, for example, as disclosed in Japanese Patent Laid-Open Publication No. 1-22575 (22675/1989), when the vehicle is running at speeds lower than a predetermined vehicle velocity, a turning ratio between the front and rear wheels is set so that a steering angle of the rear wheels becomes the reverse phase to that of the front wheels. On the other hand, when the vehicle is running at higher speeds than the predetermined vehicle velocity, the turning ratio is set so that the steering angle of the rear wheels becomes the same phase as that of the front wheels. FIG. 12 is a concrete example of the turning ratio set in the prior art four-wheel steering system.
A main advantage of the four-wheel steering vehicle is to enforce the cornering force approximately at the same time for the front wheel tires and rear wheel tires. Therefore, the four-wheel steering vehicle is allowed to move in a transverse direction faster than a front-wheel steering vehicle when the operator turns a steering wheel. In other words, if the front and rear wheels are turned in the reverse phase at low speeds and in the same phase at high speeds with an appropriate turning ratio, the vehicle starts turning at an earlier stage, thereby reducing a delay in transverse acceleration after turning of the steering wheel. This realizes, as effects in practical use, a capability of a small turn at low speeds and a capability of an emergency avoidance at high speeds, etc.
As a method to determine a steering angle of the rear wheels, the assignee of the present invention has proposed in Japanese Patent Application No. 2-212861 (212861/1990) to provide detecting means of a yaw rate (angular velocity of rotation around the center of gravity of a vehicle), so that the steering angle of the rear wheels is determined in accordance with the vehicle velocity, steering angle of the front wheels and yaw rate, and a displacement in an advancing direction of the vehicle due to external disturbances such as transverse winds or bad roads, etc. is corrected by turning the rear wheels by the determined steering angle.
However, the characteristic and response of an electric motor are varied with time in the prior art four-wheel steering apparatus of the aforementioned structure, whereby the stability of the rear wheels is undesirably endangered.
If the rotation of the electric motor is unstable, with resultant vibrations (therefore hindering the electric motor from stopping at a fixed position), the rear wheels become unsteady in their movement, resulting in an increase of power consumption in the electric motor.
Considering the yaw rate, if a signal of the yaw rate sensor is to be used for feedback, such delays as a time delay before the yaw rate is generated to the vehicle body after the rear wheels are turned, a response delay of the rear wheels, a time delay of the yaw rate sensor, a time delay for A/D conversion, a phase delay in a low pass filter to reduce noises of the yaw rate sensor, etc. make the movement of the rear wheels unstable, e.g., during the change of a lane at high speeds, thus deteriorating the steering stability.
Furthermore, a response speed to a desired steering angle of the rear wheels, which angle is determined by the angle of the steering wheel, yaw rate and vehicle velocity, namely, a response speed of the electric motor mounted in the rear wheels is set always constant in the prior art four-wheel steering apparatus, and aimed for a high speed region requiring a quick response. Therefore, the response speed is kept high even in a region not requiring a quick response, for example, even when the rear wheels remain unturned. As a result, the electric motor consumes unnecessary power.
SUMMARY OF THE INVENTION
An essential object of the present invention is to provide a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle, which realizes smooth and comfortable running of the vehicle without unstable operation of an electric motor resulting from the unevenness and change with time or vibrations of the characteristic of the electric motor.
A further object of the present invention is to provide a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle, whereby a desired steering angle of the rear wheels is obtained stably and a displacement in an advancing direction of the vehicle due to external disturbances such as transverse winds or bad roads, etc. is stably corrected, and which is further characterized in that the steering angle of the rear wheels is properly controlled even when the unstable movement of the rear wheels is detected.
A still further object of the present invention is to provide a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle, designed to change a response speed of an electric motor for a desired steering angle of the rear wheels thereby suppressing power consumption in the electric motor.
In accomplishing the above-described objects, according to the present invention, a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle is provided with at least one of an angle sensor of a steering wheel, a vehicle speed sensor and a yaw rate sensor, so that the rear wheels are steered directly by an electric motor via a reduction gear in correspondence to the running state of the vehicle detected by the sensor. The controlling apparatus includes a position detector for detecting the position of the electric motor, a first interface circuit for detecting the current position of the electric motor from the position detector, an operating unit for operating a desired steering angle or the like of the rear wheels from an input value of each sensor, and a second interface circuit for impressing a current instructing value to a motor driver from the operating unit. In the controlling apparatus, a desired position of the electric motor is changed step by step by intermittently connecting the electric motor with the rear wheels, and the response waveform of the electric motor at this time is calculated by the operating unit from the current position of the electric motor detected by the position detector. Then, a deviation between the desired position and current position of the electric motor is operated in the operating unit, and a weighting constant is determined for proportional, integral and differential operations. The obtained results of operations are added and output as a current instructing value to the motor driver via the second interface circuit.
Moreover, the operation of the deviation between the desired position and current position of the electric motor is repeated and the weighting constant is changed until the response waveform of the electric motor when the desired position is changed step by step is comprehended within a desired response.
In the case where the deviation between the desired position and current position of the electric motor repeats positive and negative values for a predetermined number of times or more within a preset term, and, if an absolute value of the deviation during the term is not smaller than a fixed value, it is determined that the electric motor is vibrating and zero is output as a current instructing value to the motor driver.
The above-discussed constitution enables constant response of the controlling apparatus without influences of the variation and change with time of the characteristic of the electric motor. If the deviation between the desired position and current position of the electric motor repeats positive and negative values with a fast cycle, in other words, when the electric motor is judged to be vibrating, zero is output as a current instructing value to the motor driver, thereby stopping the vibration and unstable movement of the rear wheels.
In a further aspect of the present invention, a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle is provided with an angle sensor of a steering wheel, a vehicle speed sensor, a rear wheel steering angle sensor for detecting a steering angle of rear wheels and a yaw rate sensor, wherein the rear wheels are directly steered by an electric motor via a reduction gear in correspondence to the running state of the vehicle detected by the above sensors. The controlling apparatus includes a controlling device which outputs a rear wheel steering angle instructing signal in response to the sensor signals of the above sensors and a rear wheel steering device which steers the rear wheels based on the rear wheel steering angle instructing signal from the controlling device, so that a response time before a yaw rate is generated to the vehicle body after the rear wheels are turned by use of the sensor signals, and the size of the yaw rate are predicted within the controlling device, and a signal of the yaw rate sensor is corrected by using the predicting value to be an actual yaw rate.
In the case where a deviation between a desired steering angle and the current steering angle of the rear wheels operated within the controlling device repeats positive and negative values for a predetermined number of times or more within a preset term, and, if an absolute value of the deviation is not smaller than a fixed value in the term, the rear wheels are judged to be vibrating, and a gain to the detecting value of the yaw rate sensor is reduced so that the absolute value becomes the fixed value or lower.
The controlling apparatus further features a plurality of yaw rate sensors to detect the yaw rate of the vehicle.
In the above-described constitution, a delay of the yaw rate sensor is corrected through prediction of the response time and size of the yaw rate. Therefore, when the rear wheels are detected to be unstable, a gain of a yaw rate feedback loop is reduced to stabilize the feedback loop. In other words, when the absolute value of the deviation exceeds the fixed value, the rear wheels are judged to be vibrating and a gain to an average value of the detecting values of the yaw rate sensors is reduced so that the absolute value becomes the fixed value or lower. Moreover, the rear wheels are steered in accordance with a value obtained by adding an average value of the detecting values of the plurality of yaw rate sensors and an average value of the differential values for every sampling cycle.
In a still further aspect of a controlling apparatus of the present invention, a position detector is installed in an electric motor. A controlling device of the controlling apparatus is provided with a first interface circuit for detecting the current position of the electric motor from the position detector, an operating unit for operating a desired steering angle of the rear wheels from input values of an angle sensor of a steering wheel, a yaw rate sensor and a vehicle speed sensor, and a second interface circuit for impressing a current instructing value to a motor driver from the operating unit.
According to one way of approach to the above-described objects by the controlling apparatus of the present invention, a deviation between the desired position and current position of the electric motor is operated within the operating unit. Then, a value obtained through differential operation of the current position of the electric motor is subtracted from a value obtained by multiplying an adding value of a value through proportional operation of the deviation and a value through integral operation of the deviation with a value proportional to the size of the vehicle velocity, which is output as a current instructing value to the motor driver via the second interface circuit.
In another way of approach made by the controlling apparatus, a deviation between the desired position and current position of the electric motor is operated within the operating unit. Then, a value obtained through differential operation of the current position of the electric motor is subtracted from a value obtained by multiplying an adding value of a value through proportional operation of the deviation and a value through integral operation of the deviation with a proportionating constant which is made different between for the same phase time and for the reverse phase time, and then output as a current instructing value to the motor driver via the second interface circuit.
In the above-described constitution, a response speed of the electric motor, namely, rear wheels is raised as the vehicle velocity is increased. Therefore, power consumption during the low speed running time not requiring a quick response of the rear wheels is reduced.
Furthermore, a response speed of the electric motor is made different to the steering wheel angle sensor from that to the yaw rate sensor and the speed in steering the rear wheels in the reverse phase is decreased to the steering wheel angle sensor, thereby reducing power consumption and ensuring smooth generation of the yaw rate. Since the response of the electric motor to the yaw rate sensor in steering the rear wheels in the same phase is maintained high, a feedback loop of a steering system of the rear wheels is stabilized. Errors in an advancing direction or course of the vehicle due to the external disturbances can be corrected stably by steering the rear wheels.
These and other objects and features of the present invention will become apparent from the following detailed description taken in conjunction with preferred embodiments thereof with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle according to a first embodiment of the present invention;
FIG. 2 is a flow chart of the operation of the controlling apparatus of FIG. 1;
FIG. 3 is a graph explanatory of the vibration of an electric motor;
FIG. 4 is a flow chart of the operation of a controlling apparatus according to a modified embodiment of FIG. 1;
FIG. 4(a) is a graph showing a motor response to the step input of FIG. 4;
FIG. 4(b) shows constants to the overshoot and rise time of FIG. 4;
FIGS. 4(c) and 4(d) are graphs each showing one example of the step response of FIG. 4;
FIG. 5 is a block diagram of a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle according to a second embodiment of the present invention;
FIG. 6 is a flow chart of the operation of the controlling apparatus of FIG. 5;
FIG. 7 is a block diagram of a controlling apparatus according to a modified embodiment of FIG. 5;
FIG. 8 is a flow chart of the operation of a controlling apparatus according to a further modified embodiment of FIG. 5;
FIG. 9 is a graph explanatory of the vibration of rear wheels;
FIG. 10 is a block diagram of a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle according to a third embodiment of the present invention;
FIG. 10(a) is a graph showing the relation between speed and f(V) of FIG. 10;
FIG. 11 is a block diagram of a controlling apparatus according to a modified embodiment of FIG. 10; and
FIG. 12 is a graph of the ratio of steering angles between the front and rear wheels in a conventional four-wheel steering vehicle.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Before the description of the present invention proceeds, it is to be noted here that like parts are designated by like reference numerals throughout the accompanying drawings.
First Embodiment
Referring to a block diagram of FIG. 1 showing a controlling apparatus in a first embodiment of the present invention, right and left rear wheels 1 are turned by an electric motor 4 according to a rear wheel steering angle instructing signal 6-a output to a motor driver 3 from a controlling device 2 which controls a steering angle of rear wheels of a four-wheel steering vehicle. A reduction gear 5 is present between the electric motor 4 and rear wheels 1 to amplify a torque. The controlling device 2 is constituted by an operating device 16 which determines a target steering angle of rear wheels according to an input value from each of a speed sensor 7, a steering wheel angle sensor 8 and a rear wheel position detector 10 and, also determines the above-referred rear wheel steering angle instructing signal 6-a and, interface circuits 11, 12, 14, 15 of the respective sensors. The operating device 16 is comprised of a desired steering angle setting device 22 for setting a desired steering angle of the rear wheels, a comparator 26 and a current instructing value setting device 23 which consists of a comparator 23a and couplers 23b, 23c. Values of the above sensors, i.e., speed sensor 7, steering wheel angle sensor 8 and rear wheel position detector 10 are input into the operating device 16 via the interface circuits 11, 12, 14.
FIG. 2 is a flow chart of the controlling apparatus of FIG. 1.
A sub routine shown in the flow chart of FIG. 2 is a "vibration preventing routine" processed for every sampling cycle T. A deviation of the electric motor is operated in step S1 first. If it is found in step S2 that the deviation continues-for a predetermined time (T2) or more with the same symbol, the electric motor is judged not to have vibrations, and the flow returns to a main routine S6.
In the event the vibration with the same symbol does not continue for a predetermined time in step S2, the change of the symbol of the deviation is monitored in step S3. If the symbol of the deviation is changed for a predetermined number of times K1 or more, the flow goes to step S4. In the other cases, the flow returns to the main routine S6. A peak value of the deviation is checked in step S4, and if an absolute value of the peak value is larger than K2, the electric motor is judged to be vibrating. The flow then moves to step S5. If the absolute value of the peak value is smaller than K2, the flow returns to the main routine S6. A current instructing value for the motor driver is changed to 0 in step S5. Kp, Kd, Ki are determined by an initializing routine when an ignition switch is turned ON (initialized).
FIG. 3 is a graph diagrammatically representing the vibrating phenomenon of the electric motor. When it continues that the current position of the motor is not focused to a desired position, the motor is judged to be vibrating, when the supply of electric current to the motor driver is cut.
According to the first embodiment as described hereinabove, vibrations are removed when the electric motor is in the state approximately agreeing with a desired value, so that power consumption by the electric motor is reduced.
A modification of the above first embodiment will be discussed hereinbelow.
In FIG. 4, "an initializing routine of the electric motor" is started immediately after an ignition switch is turned ON. The electric motor and rear wheels are intermittently connected with each other in step S11, that is, the motion of the electric motor is arranged not to be transmitted to the rear wheels. In the succeeding step S12, the electric motor is driven step by step. The current position of the electric motor is obtained in step S13 from the position detector 10 and corresponding interface circuit 14. If an overshoot of the electric motor is not smaller than a predetermined value in step S14, each constant for the proportional operation, differential operation and integral operation is set in step S16 so as to make the overshoot smaller. Then, the flow returns to step S12 to drive the electric motor step by step.
Meanwhile, if the overshoot of the electric motor is not larger than a predetermined value in step S14, it is checked in step S15 whether a rise time of the electric motor is equal to or lower than a predetermined value. If the rise time is not smaller than a predetermined value, a constant for each of the proportional, differential and integral operations is set in step S16 so that the rise time is reduced. Thereafter, the flow returns again to step S12.
To respond step by step is repeated until each of an overshoot and a rise time is turned not larger than a predetermined value.
FIG. 4(a) is a graph showing a motor response including a motor position c relating to the motor angle and time in response to the step input. In FIG. 4(a) there is shown a position demand a, overshoot amount b for the motor angle, and a raising-up time d for the target time. FIG. 4(b) is a graph showing the change in each constant according to overshoot and rise time, wherein Ki is decreased when the overshoot is large, while Kp, Ki are increased when the rise time is large. However, actual initial value of Ki is 64/16 4 (reduced every 2/16 4 ), actual initial value of Kp is 128/16 4 (increased every /16 4 ), and actual initial value of Kd is 12800/16 4 (increased every 256/16 4 ). FIGS. 4(c) and 4(d) are graphs each showing one sample of the step response including the motor position c, motor position command d, and motor current command l in the event of having a target of overshoot amount being within 50 deg and raising-up time being 50 msec.
The above sequence is repeated to determine the constant for the proportional, differential and integral operations so that the electric motor shows a suitable transient response.
Although the foregoing modification is related to the initializing routine in general use to determine the constant for the proportional, differential and integral operations, the present invention is applicable to determining of a weighting constant for adaptive control or the like.
In the manner as above, the unstable movement of the rear wheels and electric motor resulting from the variation or unevenness of the characteristic and response or vibrations of the electric motor can be solved, and the power consumption of the electric motor is effectively reduced.
Second Embodiment
FIG. 5 is a block diagram of a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle according to a second embodiment of the present invention. In the controlling apparatus of FIG. 5, the right and left rear wheels 1 are turned by the electric motor 4 according to the rear wheel steering angle instructing signal 6-a output from the controlling device 2 to the motor driver 3. The reduction gear 5 between the electric motor 4 and rear wheels 1 is provided so as to amplify a torque. The controlling device 2 is constituted by the operating device 16 which determines a desired steering angle of the rear wheels according to input values of the speed sensor 7, steering wheel angle sensor 8 and rear wheel position detector 10, and interface circuits 11-15 for the corresponding sensors. The operating device 16 is comprised of a yaw rate predicting/operating device 20, an actual yaw rate setting device 21, the desired steering angle setting device 22 and the current instructing value setting device 23.
A predicting value of the yaw rate and a detecting value of the yaw rate detected by the yaw rate sensor are compared in the yaw rate comparator.
As a result of the comparison in the yaw rate comarator, the detecting value K1* (K1>1) is set as an actual yaw rate value in the actual yaw rate setting device if the predicting value is larger.
The detecting value K2 (k2<1) is set as an actual yaw rate value if the detecting value is larger.
Actual value of K1=1.1
Actual value of K2=0.9
The operation of the controlling apparatus in the above-described structure will be explained with reference to a flow chart of FIG. 6.
Values of the speed sensor 7, steering wheel angle sensor 8 and rear wheel position detector 10 are input to the operating device 16 via the interface circuits 11-14 (S21). A time before a yaw rate of the vehicle body is generated after the rear wheels are turned and, the size of the yaw rate are predicted in the yaw rate predicting/operating device 20 from the output values of the sensors (S22). Then, a desired steering angle of the rear wheels and a current instructing value are set by the desired steering angle setting device 22 from the predicted yaw rate, vehicle velocity and steering wheel angle (S23). At this time, the actual yaw rate setting device 21 is not driven at all without outputs from the yaw rate sensor 9, but transmits the output from the predicting/operating device 20 as it is to the desired steering angle setting device 22. The rear wheel steering angle instructing signal 6-a is output from the current instructing value setting device 23 to the motor driver 3 through the interface circuit 15 (S24). Subsequently, a yaw rate generated in the vehicle body after the rear wheels are turned is detected by the yaw rate sensor 9 via the interface circuit 13 (S25). The actual yaw rate detected in step S25 and the predicted yaw rate obtained in step S22 are compared with each other (S26). If the predicted yaw rate is found larger than the actual yaw rate, the actual yaw rate *K1 (K1>1) is corrected to an actual yaw rate value (S27). On the other hand, if the actual yaw rate is larger than the predicting value, the actual yaw rate *K2 (K2<1) is corrected to an actual yaw rate value (628). These values K1, K2 are constants determined by the responding capability of the yaw rate sensor 9.
The procedure in steps S26-S28 is conducted by the actual yaw rate value setting device 21.
Back in step S23, a desired steering angle of the rear wheels and a current instructing value are set from the actual yaw rate value, vehicle velocity and steering wheel angle, which are output as the rear wheel steering angle instructing signal 6-a through the interface circuit 15 to the motor driver 3 in a similar manner as in step S24 described earlier. Subsequently, the above process is repeated until the rotary movement of the vehicle is finished.
According to the second embodiment of the present invention, information of the yaw rate is used in addition to the vehicle velocity and steering wheel angle so as to determine the desired steering angle of the rear wheels. Moreover, a time delay in outputting the yaw rate is predicted beforehand by the yaw rate predicting/operating device 20. Therefore, it becomes possible to suppress the unstable movement of the rear wheels during running at high speeds.
A modified embodiment of the controlling apparatus of FIG. 5 will now be described below.
FIG. 7 is a block diagram of a modified controlling apparatus. Although the fundamental structure is the same as that of the second embodiment, this modification employs two yaw rate sensors.
The operation of the modified controlling apparatus will be depicted hereinafter.
Signals from a first and a second yaw rate sensors 9a, 9b are input to the operating device 16 through respective interface circuits 13a, 13b. Thereafter, each detecting value of the yaw rate sensors is multiplied with a constant Kp1, Kp2 and averaged. Moreover, a difference between each detecting value and a detecting value one cycle before is multiplied with a constant Kd1, Kd2 and averaged. The obtained averaged values are added to be an actual yaw rate value. The constants Kp1, Kp2, Kd1, Kd2 are determined by the inertia of the vehicle or the like in order to keep a yaw rate feedback loop stable. Then, a desired steering angle of the rear wheels and a current instructing value are set from the actual yaw rate value, vehicle velocity and steering wheel angle, similar to the second embodiment, and output as the rear wheel steering angle instructing signal 6-a to the motor driver 3 via the interface circuit 15. If the vibration of the rear wheels as a result of the instability of the yaw rate feedback loop is detected in the operating device 16, the constants Kp1, Kp2 are reset and a fresh current instructing value is set. At the next sampling time, an actual yaw rate value is set with use of these reset constants.
When a vibration is detected, a current instructing value is set after Kp1-ΔKp1 and Kp2-ΔKp2 are reset to Kp1 and Kp2, respectively. A yaw rate value is set by using the reset constants at the next sampling time.
Actual initial value of Kp1=256/16 2 (=1) (reduced every 2/16 2 )
Actual initial value of Kp2=256/16 2 (=1) (reduced every 2/16 2 )
FIG. 8 is a flow chart of an algorithm used to detect the vibration and to reset the constants in the modified embodiment of FIG. 7. A sub routine called a "vibration preventing routine" is processed for every sampling cycle. A deviation between the position of the rear wheels and a desired steering angle thereof is operated in step S30. If it is found in step S31 that the deviation continues for a predetermined time (T2) or more with the same symbol, the flow returns to a main routine S35.
In the event the vibration with the same symbol does not continue for a predetermined time in step S31, the change of the symbol of the deviation is monitored in step S32. If the symbol of the deviation is changed for a predetermined number of times K1 or more, the flow goes to step S33. In the other cases, the flow returns to the main routine S35. A peak value of the deviation is checked in step S33, and if an absolute value of the peak value is larger than K2, the rear wheels are judged to be vibrating. The flow then moves to step S34. If the absolute value of the peak value is smaller than K2, the flow returns to the main routine S35. In step S34, gain constants Kp1, Kp2 are reset to the detecting values of the yaw rate sensors to stabilize the yaw rate feedback loop.
FIG. 9 is a graph diagrammatically representing the vibrating phenomenon of the rear wheels. When it continues that the current position of the rear wheels is not focused to a desired position, the rear wheels are judged to be vibrating.
As described hereinabove, in the modified embodiment, the rear wheels are turned according to the value obtained by adding the average value of the detecting values of the two yaw rate sensors and the average value of the differential values for every sampling cycle, thus eliminating errors proper to the sensors. In the case where the rear wheels are detected to be vibrating from the outputs of the position detector and the feedback system starts vibrating, the input gains Kp1, Kp2 of the feedback system are reset to settle the vibration. Therefore, the unstable movement of the rear wheels or waste of power due to the vibration of the-rear wheels can be reduced. Although two yaw rate sensors are used in the modified embodiment, three, four or more yaw rate sensors may be employed. Increasing the number of the yaw rate sensors makes it possible to further reduce errors proper to the sensors.
It is so arranged in the second embodiment of the present invention that the yaw rate of the vehicle is fed back to steer the rear wheels, namely, to correct the moving direction of the vehicle, without a time lag between outputs of the yaw rate sensor and the other sensors. Accordingly, the rear wheels can be turned stably. Even if an unstable movement of the rear wheels is detected, a spin or the like danger can be avoided by adjusting the gain of the yaw rate.
Third Embodiment
FIG. 10 is a block diagram of a controlling apparatus for controlling a steering angle of rear wheels of a four-wheel steering vehicle according to a third embodiment of the present invention. As indicated in FIG. 10, the right and left rear wheels 1 are driven directly by the motor driver 3 and electric motor 4. Within the controlling device 2 are provided the first interface circuit 14 mounted to the electric motor 4 which converts a value of the position detector 10 to a digital value to thereby obtain the current position of the electric motor 4, steering wheel angle sensor 8, interface circuits 12, 13 for converting a detecting signal of the yaw rate sensor 9 to a digital value, second interface circuit 15 which feeds a current instructing value 6 to the motor driver 3 and operating device 16 which operates a desired steering angle of the rear wheels, the current instructing value 6 and detects a cycle of the speed sensor 7.
An algorithm within the operating device 16 will be discussed now. A deviation between a target steering angle of the rear wheels determined by the steering wheel angle, yaw rate and vehicle velocity, i.e., a target steering angle of the electric motor 4 mounted in the rear wheels 1 and, the current position of the electric motor 4 is operated for every sampling cycle. The deviation is integrated for every sampling cycle.
In the first place, a value obtained by multiplying the deviation with Kp is added to a value obtained by multiplying an integrating value of the deviation with a coefficient Ki. Then, a value obtained by multiplying a velocity of the electric motor 4 obtained through reduction of the current position and a current position one cycle before with Kd is subtracted from a value obtained by multiplying the above adding value with a function f(V) of the vehicle velocity, which is output as the current instructing value 6 to the motor driver 3 via the second interface circuit 15. The function f(V) is a constant proportional to the vehicle velocity. In other words, as the vehicle velocity is increased while the deviation is the same, the current instructing value 6 to the motor driver 3 is increased, thereby enhancing the controlling property of the electric motor 4.
FIG. 10(a) is a graph showing the relation between vehicle velocity and function f(V), wherein f(V) is increased in proportion to the vehicle velocity.
FIG. 11 is a block diagram of a controlling apparatus according to a modification of the third embodiment. The modified controlling apparatus is fundamentally equal to the apparatus of FIG. 10 in its structure, but is provided with a K1 (same phase) and a K2 (reverse phase) circuits in the f(V) circuit within the operating device 16.
Whether the rear wheels are turned in the same phase or reverse phase to the front wheels is detected by a phase detector from a steering wheel angle and a motor (rear wheel) angle. A gain K1 or K2 is multiplied for the same phase time or for the reverse phase time.
An algorithm within the operating device 16 will be depicted hereinbelow. A deviation between a target steering angle of the rear wheels determined by the steering wheel angle, yaw rate and vehicle velocity, i.e., a target steering angle of the electric motor 4 mounted in the rear wheels 1 and the current position of the electric motor 4 is operated for every sampling cycle. The deviation is integrated for every sampling cycle.
A value obtained by multiplying the deviation with Kp is added to a value obtained by multiplying an integrating value with the coefficient Ki. Thereafter, in the case where the front (not shown) and rear wheels are turned in the same phase, a value obtained by multiplying the velocity of the electric motor obtained through reduction of the current position and a current position one cycle before of the electric motor with Kd is subtracted from a value obtained by multiplying the adding value with K1. On the other hand, if the front and rear wheels are turned in the reverse phase, the value is subtracted from a value obtained by multiplying the adding value with K2. The resultant value is output as the current instructing value 6 to the motor driver 3 via the second interface circuit 15.
K1 is set larger than K2. That is, when the rear wheels are turned in the reverse phase to the front wheels in proportion to the size of the steering wheel angle, the electric motor gets delayed in response. If the rear wheels are turned in the same phase as the front wheels in proportion to the size of the yaw rate, the responding capability of the rear wheels is improved.
Although the above embodiment effects control according to a proportional integrating method, the fundamental concept of the third embodiment is made effective in the other controlling methods as well even when the responding capability of the electric motor is changed depending on the vehicle velocity or when the rear wheels are turned in the reverse or same phase to the front wheels.
In the above third embodiment, since the current instructing value fed to the motor driver is made smaller at a low speed region not requiring a quick response of the rear wheels, the responding speed of the electric motor is decreased to suppress the power consumption. Moreover, since the responding capability of the rear wheels is changed between when the rear wheels are turned in the reverse phase to the front wheels in proportion to the steering wheel angle and when the rear wheels are turned in the same phase as the front wheels in proportion to the yaw rate, the feedback loop for the rear wheel steering system to feed back the yaw rate is retained stable, whereby the advancing direction or course of the rear wheels can be corrected stably.
Although the present invention has been fully described in connection with the preferred embodiments thereof with reference to the accompanying drawings, it is to be noted that various changes and modifications are apparent to those skilled in the art. Such changes and modifications are to be understood as included within the scope of the present invention as defined by the appended claims unless they depart therefrom.
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A steering angle of rear wheels of a four-wheel steering vehicle is controlled so that a quick response of an electric motor mounted in the rear wheels is achieved only when it is necessary, thereby avoiding wasteful consumption of power. In addition, a yaw rate feedback system is kept stable. When unstable vibration of the electric motor is detected, a gain to the yaw rate is adjusted.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to the field of laundry and other article-drying equipment and, more particularly, to an improved combustion chamber used to advantageously provide large volumes of very hot air to high-production commercial dryers.
2. Description of the Prior Art
An overall view of typical prior art in industrial laundry dryer-conditioners, generally referred to in the industry as merely "dryers", may be found by referring to U.S. Pat. Nos. 2,604,313, 2,643,463, 3,443,323, 3,861,865 and 4,015,930. Dryers such as those discussed in these patents and, for that matter, industrial dryers in general, require large volumes of air having a temperature, in the tumbler of the dryer, in the range of 300° to 350° F., which elevated temperature air flow combines with the tumbling action of the dryer to achieve rapid, yet safe, drying.
The high temperature of the air flowing through the dryer is achieved by the burning of fuel such as natural gas, propane, butane, or fuel oil in a combustion chamber from which hot air is supplied to the dryer housing, generally with the aid of an air pump or blower. The fuel is mixed with appropriate portions of air to obtain clean burning of the fuel, and is introduced into the combustion chamber under pressure. Internal temperatures in the combustion chamber may typically range from 400° to 700° F., and it may therefore be apprecited that the high temperature of operation is a factor in the design of the combustion chamber.
The present state-of-the-art of the combustion chamber is illustrated in U.S. Pat. No. 3,861,865, and utilizes double wall construction with between-wall cooling by intake (make-up) air as well as an air barrier to eliminate the need for a refractory endpiece. While this design offers significant advantages over previous such combustion chambers, it has, as do other previous designs, several disadvantages which are discussed at length below. The solution to these disadvantages in a combustion chamber offering at least as economic and dependable operation as presently existing devices will present to its manufacturer a significant competitive advantage in the industry.
The first of these problems is related to the placement of the burner in the front wall of the combustion chamber. At best it is inconvenient to have the burner in the front of the dryer, since the fuel line must be routed around to the front of the machine. Since the portion of exhaust from the dryer which is to be recirculated back into the dryer with the hot air flow in present devices enters the combustion chamber at the end opposite the burner, it is apparent that the flow of hot gas generated by the burner will move in a direction opposite to the flow of exhaust gas which is being recirculated. This counterflow problem results in a loss in efficiency due to swirl occurring in the combustion chamber, as well as making the regulation of the amount of exhaust gas recirculated relatively difficult to control.
A closely related problem is caused by the differing locations at which fresh air is supplied to the dryer and exhaust air is purged from the dryer. In the arrangement shown in U.S. Pat. No. 3,861,865, fresh air enters the combustion chamber from both ends of the dryer, and exhaust air leaves through an exhaust stack at the back of the dryer. It has been found desirable to have a more hermetically sealed combustion chamber, where both fresh air and exhaust air flows are supplied through ducting at the same end of the chamber. This simplifies the construction of the chamber and permits better control of the air flow.
In addition, the preferred method of supplying fresh air and removing exhaust air is to use a coaxial tube arrangement, with the fresh air being ducted in a tube contained within the stack carrying out the exhaust air. This technique offers the advantage fo preheating the fresh air without expending any further energy, thereby reducing the amount of fuel which must be burned to heat the fresh air prior to supplying it to the dryer. This type of ducting arrangement is difficult to use with a combustion chamber having the air intake on one end of the combustion chamber and the exhaust on the other end, and bulky and expensive manifolds and added ducting work only with diminished efficiency. It is therefore apparent that it is highly desirable to have the fresh air intake as close to the exhaust as possible, and it is further desirable to have the system hermetically sealed.
A further problem in existing combustion chambers for dryers relates to the problems of temperature control and air mixture. Clothing in the dryer can tolerate a fairly high temperature when wet, in the neighborhood of 300°-350° F., as stated above. However, when the clothes are about 25% through the drying cycle, although still damp, they can no longer tolerate higher temperatures without scorching. Accordingly, the temperature should be reduced at this point in the drying cycle. One way to do this is by reducing the level of the burner. It is desirable to effect this reduction in temperature by the introduction of a greater amount of cooler fresh air, rather than to lower the temperature exclusively by lowering the level of the burner.
It may therefore be seen that a number of areas for improvement exist with respect to combustion chambers for dryers. It is of course also apparent that while the combustion chamber should be as inexpensive to purchase as possible, the efficiency of operation is most important, since even small gains in efficiency translate over a long period into relatively large savings. Finally, it is desirable that an improved combustion chamber may be retrofitted onto older dryers so the operators of such dryers may also obtain the attendant advantages of the improved combustion chamber.
SUMMARY OF THE INVENTION
The present invention utilizes a radical redesign of the combustion chamber of a dryer to solve the above problems and to achieve the above advantages. The combustion chamber of the present invention is a hermetically sealed unit, and it features a design having the burner mounted in back. The burner fires into a first or burner cylinder which is open at the end away from the burner. A second or heating cylinder of a larger diameter than the burner cylinder overlaps the burner cylinder, and the flame from the burner extends through the heating cylinder.
Fresh air enters through the end of the heating cylinder overlapping the burner cylinder, with the fresh air passing through the clearance between the heating cylinder and the burner cylinder. Exhaust gas passes around the heating cylinder, and a portion of the exhaust gas may be recirculated through the dryer by selectively opening or closing an exhaust gate. The exhaust air is separated from the fresh air only by a single wall, and the coaxial ducting arrangement discussed above may be utilized with a minimum of difficulty. The direction recirculated exhaust gas takes is no longer opposed to the direction of hot gases from the burner, and swirl losses are thereby minimized.
A slide gate is utilized to selectively provide cooler air to the air mix supplied to the dryer to prevent scorching of clothes after the first 25% of the cycle. A deflector shield is provided to accomplish mixing of the cooler air with the heated air. A heat shield with a perforated portion is supplied at the front of the combustion chamber, with a glass window provided in the housing to allow observation for adjustment of the flame provided by the burner.
Since most of the heating is done inside the two cylinders, double wall construction is unnecessary, resulting in a more economical construction. Another added feature afforded by the particular arrangement of the combustion chamber, with the burner mounted on the opposite side of the exhaust passage from the dryer inlet opening, is the length of the flame extending from the burner, which is longer than the flame in other types of combustion chambers. The added flame length allows better mixing with the air, for cleaner and more efficient operation. It may therefore be appreciated that the present invention is a substantial improvement over the art, and provides a hermetically sealed combustion chamber for a commercial dryer which is more efficient than those previously known.
The burner, located in the back of the combustion chamber, no longer fires into the exhaust stream but through the exhaust stream, which travels around the flame. The exhaust and fresh air paths are adjacent, allowing coaxial ducting to be used. Both exhaust recirculation and cool air mixing are easily accomplished with a high degree of control. The combustion chamber of the present invention is adaptable to being retrofitted onto older dryers, making its commercial potential high for both manufacturers and end users. These significant advantages are all provided by the present invention without substantial disadvantage, making the present invention a highly desirable improvement in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
A better understanding of the present invention may be had from a consideration of the following detailed description, taken in conjunction with the accompanying drawings in which:
FIG. 1 is a perspective view, in elevation, of a dryer system incorporating the present invention;
FIG. 2 is a side view of the combustion chamber and blower of FIG. 1 with the air-fuel mixing and introduction means simplified;
FIG. 3 is a perspective view, in elevation, of the combustion chamber of FIG. 1 with the first side wall and the top wall partially cut away;
FIG. 4 is a sectional view of the combustion chamber of FIG. 3, with both the exhaust gate and the slide gate partially open;
FIG. 5 is a sectional view of the combustion chamber of FIGS. 3 and 4; and
FIG. 6 is a further sectional view of the combustion chamber of FIGS. 3 and 4.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
In FIG. 1 a commercial dryer system 10 is shown which includes a housing 12 which rotatably supports a basket 14 within said housing 12. A cover 16, shown in FIG. 1 in its removed position, is supported by an arm 20. A control center 22 contains the controls for the dryer system 10 and operates the various cycles and positions of the dryer system 10. A combustion chamber 24, mounted on top of the control center 22, heats the air used in the drying process. The housing 12 is tiltably supported by a base 26.
The housing 12 is shown in FIG. 1 in its loading position, in which it is tilted back by mechanical means (not shown) operated by the control center 22. The axis of rotation of the housing 12 is about journal 28 and a corresponding journal (not shown) on the opposite side of the housing 12. In this loading position the cover 16 is in the removed position shown, away from a front opening 30 in the housing 12 through which laundry may be loaded into the basket 14. The front opening is surrounded by a gasket 32 for sealing the opening whenever the cover 16 is in place over the front opening 30.
This control center 22 includes various switches, lights, relays, timers, sensor controls and similar elements of conventional construction. For purposes of describing the present invention, the control console includes a cycle timer 85 and a division timer 87. The timer 85 is set to determine the length of the drying cycle and the timer 87 picks off a selected portion of that time period (say 25%) to perform a particular operation of the present invention, to be explained bwlow. The console 22 may also include a sensor control stage 49 to develop a desired response to the sensing of particular operating conditions, such as the humidity of the recirculating air, for example.
A cover positioner 34 is used which may be a pneumatic or hydraulic actuator which cooperates through a chain member 36 with teeth 38 on a gear member 40 to which the arm 20 is secured, the gear member 40 being rotatably mounted on the housing 12. When the positioner 34 receives a signal from the control center 22, the positioner 34 pulls downwardly on the chain member 36, causing the gear member 40 to rotate and raising the cover 16 away from its position in cooperation with the gasket 32 surrounding the front opening 30 in the housing 12. A similar mechanism may be provided on the opposite side of the housing 12, particularly if the cover 30 is of heavy construction.
While the combustion chamber is stationary, since it is connected to ducting (not shown) to supply fresh air and to remove exhaust air, a coupling 42 allows the housing 12 to move relative to the combustion chamber 24. It is through this coupling 42 that the heated air passes as it is supplied to the housing 12 of the dryer system 10 from the combustion chamber 24. The details of construction fo the dryer system 10 illustrated in FIG. 1 are used as an example to illustrate the novel combustion chamber 24 which is the heart of the subject invention. It is important to note that the combustion chamber disclosed herein may be used with many different dryers other than the type illustrated, both of the single load type shown in FIG. 1 and the continuous operation type described in U.S. Pat. No. 4,015,930.
Referring now to FIG. 2, the right side of the dryer system 10 is illustrated, showing the air circulation apparatus. As mentioned above, the hot air is supplied from the combustion chamber 24 to the housing 12 through the coupling 42. Hot air is used in the housing 12 to aid in the rapid drying of laundry contained in the dryer 10 and tumbling in the basket 14. Exhaust air is drawn out of the housing 12 by a blower 44 through an aperture (not shown) in the housing 12. The blower 44 pulls the exhaust air out of the housing 12, and forces it through a duct 46 into the bottom of the combustion chamber 24. This creates a negative pressure in the housing 12 and acts to draw heated air into the housing 12 from the combustion chamber 24. With the exception of the connection of the duct 46 to the combustion chamber 24 and the coupling 42, the dryer system as described to this point is as known in the art. It is the particular construction of the combustion chamber 24 and its interfaces with the duct 46 and the housing 12 through the coupling 42 that departs from the art and is discussed below. A sensor 47 is mounted to extend into the duct 46 for sensing air conditions, such as humidity for example. This is used to control particular elements included in the combustion chamber, explained below.
Referring now to FIGS. 3 and 4, the combustion chamber which is the heart of the present invention is illustrated in considerable detail. It will immediately be noted that a burner assembly 50 is mounted on the back of the combustion chamber 24, rather than on the front as is conventional. The burner assembly 50 is shown in rather simplified form and comprises a fuel-gas mixing chamber 52 which receives fuel through a pipe 54, as well as air, which is usually under pressure and supplied from the blower 44. The chamber 52 may also have an automatic flap valve (not shown) which adjusts the air input to the mixture as the fuel flow changes. A pilot 56 is typically provided to light the air-fuel mixture issuing from a jet 58 when the system 10 is operating to dry clothes.
There are a number of conventional safety features, such as automatic shut-off of the fuel valve if the pilot is inadvertently extinguished and interlocking features which automatically shut down the system 10 if any of the normal conditions for operation of the system 1 are departed from, which are not specifically explained herein since they are well known in the art. A pilotless ignition of the electronic variety may also be used, which variety is well known in the art. Note that the burner assembly 50 is not shown in FIG. 3, for purposes of clarity, but that it extends through a back wall 60 of the combustion chamber 24.
Referring now to FIGS. 3-5, the combustion chamber 24 is enveloped by walls on all sides, making it a hermetically sealed chamber. In addition to the aforementioned back wall 60 on which the burner assembly 50 is mounted, there is a front wall 62 opposite the back wall 60, a first side wall 64 which is adjacent the housing 12 (FIG. 1) and between the front wall 62 and the back wall 60, and a second side wall 66 opposite the first side wall 64 and between the front wall 62 and the back wall 60. There are also a top wall 68 and a bottom wall 70, both of which have apertures therein which will be described below. In one particular embodiment, all of the walls of the combustion chamber 24 are made of 14 gauge metal, preferably steel, and it should be noted that the combustion chamber is of single wall construction. In the preferred embodiment, the front and back walls 60, 62 are approximately 36 inches square.
The burner assembly 50 is mounted approximately in the middle of the back wall 60, with the jet 58 and the pilot 56 extending through the back wall 60 into the interior of the combustion chamber 24. A burner cylinder 72 is mounted on the interior side of the back wall 60, and extends around the jet 58 and the pilot 56 and into the interior of the combustion chamber toward the front wall 62. The end of the burner cylinder 72 extending toward the front wall 62 is open, and the burner cylinder 72 extends approximately 7 inches from the end wall 60.
A heating cylinder 74, which is open on both ends and which is of larger diameter than the burner cylinder 72, is mounted coaxially with and slightly overlapping the burner cylinder 72. The heating cylinder 72 extends through two walls supporting it at its ends, with both of these walls being parallel to and intermediate the back wall 60 and the front wall 62, and extending between the first and second side walls 64, 66 and the top and bottom walls 68, 70. A separation wall 76 supports the heating cylinder 74 at the end nearer the back wall 60, and a gate wall 78 supports the heating cylinder at the end nearer the front wall 62. The heating cylinder 74 is approximately 22 inches long. The specific configuration utilizing the coaxial, slightly overlapping cylinders as the location of the burner flame obviates the need for double wall construction, thereby reducing the cost of manufacture.
The separation wall 76 has a U-shaped aperture therein, with the aperture extending to the top of the separation wall 76 and the rounded portion of the aperture corresponding to the bottom of the U holding the heating cylinder 74 therein. The gate wall 78 has a similar U-shaped aperture in the same orientation. In addition, the gate wall 78 has a rectangular aperture on the bottom adjacent the bottom wall 70.
There is an additional wall which is a U-shaped wall 80. The rounded portion of the U-shaped wall 80 surrounds the lower half of the heating cylinder 74, with the legs of the U-shaped wall 80 extending upward from the sides of the heating cylinder to the top wall 68. The U-shaped wall 80 extends between the separation and gate walls 76, 78. The intersections between the walls themselves, and the walls and the cylinders are sealed, as by welding.
Note that the bottom wall 70 has an aperture therethrough, which aperture is located between the separation wall 76 and the gate wall 78. This aperture is for exhaust air returned under pressure from the housing 12 through the duct 46 by the blower 44 (FIG. 2). The exhaust air passes into the combustion chamber 24 through the aperture in the bottom wall 70, and leaves the combustion chamber through two apertures in the top wall 68, which two apertures correspond to the legs of a U and are between the separation and gate walls 76, 78 and the first and second side walls 64, 66 and the U-shaped wall 80. Note that the exhaust air thus passes around the heating cylinder 74, through which the flame from the burner assembly 50 extends. Thus, the burner assembly 50 fires through the exhaust. This also helps improve the economy of the device slightly, since the hot exhaust air will act to heat the air passing through the heating cylinder 74 and any fresh air passing within the chamber formed by the U-shaped wall 80.
Fresh air is supplied to the combustion chamber 24 through an aperture in the top wall 68. This aperture is between the back and separation walls 60, 76 and the first and second side walls 64, 66. The primary path of fresh air is through this aperture and into the clearance between the heating cylinder 74 and the burner cylinder 72, and then into the heating cylinder 74. It may thereby be appreciated that fresh air enters the combustion chamber 24 on one side of the separation wall 76, and exhaust air exits the combustion chamber 24 on the other side of the separation wall 76. This proximity makes possible the expeditious connection of the combustion chamber 24 to a coaxial duct arrangement at the base of an exhaust/intake stack through a simple manifold 82 (FIG. 2). Note that this achieves the significant advantage of using the heat of exhaust air to preheat the incoming fresh air.
In addition to the primary path for fresh air mentioned above, fresh air may also move in a secondary path through the same aperture into the area between the legs of the U-shaped wall 80 and the top wall 68 and the heating cylinder 74. Slidably mounted over the portion of the U-shaped aperture in the gate wall 78 above the heating cylinder 74 is a slide gate 84, which may be used to selectively open or close the secondary path of fresh air. The slide gate 84 would typically be closed when beginning the drying cycle, and would be opened about 25% into the cycle to cool the temperature of the air supplied to the dryer, as will be more apparent below. The slide gate 84 is shown coupled to an actuator 83 to control the movement and position of the gate. The actuator 83 is controlled from the control center 22 by either or both of the division timer 87 and the sensor control stage 49.
Also located near the gate wall 78 is an exhaust gate 86, which is used to recirculate a portion of the exhaust air entering the combustion chamber 24 through the aperture in the bottom wall 70. The exhaust gate 78, shown best in FIGS. 4 and 5, is mounted on a rod 88 which may be turned by a gate control lever 90. When opened, the exhaust gate 86 allows some exhaust air to flow through the rectangular aperture in the gate wall 78, to be recirculated back to the dryer.
Approximately half of the combustion chamber is located between the gate wall 78 and the front wall 62. It is in this portion that the air to be supplied to the dryer will be made up, and the components of that air are heated air entering through the heating cylinder 74, cooler air passing through the slide gate 80, and recirculated exhaust air passing through the exhaust gate 86. There is a deflector shield 92 mounted on the top wall 68 and extending downward at an angle to help mix cooler air coming through the slide gate 80 with the hotter air coming from the heating cylinder and through the exhaust gate 86.
Located at the end of the combustion chamber near the front wall 62, and offset from the front wall 62 by spacers 94, is a heat shield 96. Located in a portion of the heat shield having an aperture is a perforated shield 98. The front wall 62 has an aperture therein, with a frame 100 disposed around the aperture, and a piece of heat-resistant glass 102 such as Pyrex disposed in the frame 100. An observer can look through the glass 102 and the perforated shield 98 to observe and adjust the flame coming from the burner 50.
Referring now to FIG. 3, the aperture in the first side wall 64 through which hot air is supplied to the housing 12 (FIG. 1) has the coupling 42 mounted therein. The coupling 42 includes an angled portion 104 having two 90° bends in the cross section thereof and arranged in a rectangular configuration in the aperture in the first side wall 64. The angled portion 104 is basically U-shaped in cross section, with the U fitting around the edges of the aperture in the first side wall 64. A flat plate 106 having a rectangular aperture therein is mounted around the angled portion outside of the first side wall 64. A bolt 108 extends through the flat plate 106, the first side wall 64, and the angled portion 104 inside the first side wall 64, and slots in the parts allow the coupling 42 to move considerably toward the front and back of the combustion chamber 24, with a lesser degree of movement being allowed around the axis of the bolt 108. This movement in the coupling allows adjustment of any space between the coupling 42 and the facing opening in the dryer housing 12, thereby facilitating final adjustments during mounting of the combustion chamber 24 in the dryer system 10.
The operation of the combustion chamber 24 will now be discussed briefly, with particular reference to FIGS. 3 and 4. The blower 44 (FIG. 2) is started to circulate air through the housing 12 (FIG. 1), with heated air being drawn into the housing 12 from the combustion chamber 24 as a result of exhaust air being pulled out of the housing 12 by the blower 44. The burner assembly 50 produces a flame that extends through the heating cylinder 74 toward the front end 62 of the combustion chamber 24, with the flame produced by the combustion chamber of the present invention extending substantially the full length of the chamber (approximately six feet for the embodiment described) for better mixing with the air being supplied to the dryer.
Fresh air enters the heating cylinder 74 in the area between the heating cylinder 74 and the burner cylinder 72, and is heated by the flame as it passes through the heating 74. At the start of the cycle, both the slide gate 80 and the exhaust gate 86 are closed. Hot air is supplied through the aperture 42 in the first side wall 64 to the dryer housing 12. As the exhaust air heats up, the exhaust gate 86 may be opened to recycle a portion of the exhaust air.
When the cycle is about 25% through, the slide gate 80 is opened to cool the air supplied to the housing 12 slightly, to avoid scorching the clothes in the dryer 10. Note that the gate 80 may be controlled manually or by the control center 22, which may also control the opening of the exhaust gate 86. Automatic control of the gate 80 may be effected by the division timer 87, coupled to cycle timer 85, or it may be responsive to humidity of the dryer exhaust air as sensed by the sensor 47 (FIG. 2) which provides an output signal to the sensor control 49 for driving the actuator 83.
When the opening of the gate 80 is controlled manually or by automatic control from the division timer 87, it is preferable to open the gate gradually or by stages, beginning with the time that the gate starts opening at about 25% through the dryer cycle. The actuator 83 is then controlled to continue the opening of the gate 80, either continuously or by stages, over the remaining 75% of the dryer cycle in response to the division timer 87.
When the control of the opening of the gate 80 is effected by the actuator 83 responding to an output signal from the humidity sensor control element 49, it is arranged to begin opening the gate 80 when the humidity of the dryer exhaust air (which begins at a maximum level) reduces to a predetermined threshold value. Thereafter, the opening of the gate continues gradually in proportion to the reduction of exhaust air humidity until a minimum level is reached corresponding to the drying of the laundry being completed, at which point the gate 80 is fully opened.
It is apparent that the present invention presents substantial advantages over the art, the most important being that it is a more efficient combustion chamber than those previously known. It is therefore a desirable unit both to produce and to utilize. It has the burner at the back of the unit, a more desirable location, and the burner fires through the exhaust, rather than opposing the exhaust and resulting in diminished efficiency.
The combustion chamber of the present invention allows better control of both exhaust air recirculation and introduction of cooler air at a particular point in the cycle. The combustion chamber is also hermetically sealed, and susceptible to easily utilizing coaxial fresh air intake and exhaust air ducts, thereby further increasing efficiency. Finally, it is also able to retrofit onto a wide variety of existing dryers, making its appeal broad from an economic standpoint due to the increased efficiency and lower operating cost of the improved combustion chamber.
Although there have been described above specific arrangements of a combustion chamber for a commercial laundry dryer in accordance with the invention for the purpose of illustrating the manner in which the invention may be used to advantage, it will be appreciated that the invention is not limited thereto. Accordingly, any and all modifications, variations or equivalent arrangements which may occur to those skilled in the art should be considered to be within the scope of the invention as defined in the annexed claims.
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A combustion chamber for supplying heated air to a commercial dryer utilizes a back-mounted burner firing through coaxial cylinders of different diameters contained in the combustion chamber to heat air drawn through the larger cylinder. Additional fresh air in a secondary passage alongside the larger cylinder is selectively controlled to reduce the temperature of air flowing through the cylinder for the protection of the laundry articles in the dryer.
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BACKGROUND OF THE INVENTION
1. Field
Embodiments of the invention relate to updating of objects in persistent storage. More specifically, embodiments of the invention relate to insuring data consistency during the parallel update of objects requiring time sensitive response.
2. Background
Integrated information technology (IT) solutions attempt, to the extent possible, to provide real time information for a given business process instance integrated across several business objects and IT components. Business processes are often modeled as objects within the computer system. These objects control the fulfillment of the business process or some part thereof. These objects are used for both visibility and as active process control. In the context of warehouse management, a warehouse request business object (BO) triggers the warehouse execution and controls its fulfillment. For example, warehouse request BO may be a customer order expected to be shipped in the near future. This can then be thought of as a planned delivery.
In many modern warehouse scenarios, warehouse workers do not execute their work directly based on this business object. Instead, tasks associated with multiple business objects may be bundled together for execution. For example, a bundle may be instructions for one worker on a single picking path. As used herein, “task” is a work operation for a single worker. Optimization algorithms may be used to bundle tasks independent of what warehouse request (e.g., customer order) they are associated with. In some cases, the optimization algorithms split items within a warehouse request into multiple tasks that may be assigned to different task bundles. These tasks, and task bundles, are represented in a computer system as additional business objects. This permits users to report/confirm their work using these objects.
For the warehouse request BO to provide visibility and control its fulfillment, data in that BO needs to be updated whenever a task is created or its execution is confirmed. However, because of the task creation and bundling described above, multiple users may confirm task execution for the same warehouse request or even the same item within a warehouse request. In parallel, at substantially the same point in time. This need for substantive simultaneous update can result in lock collision and degrade performance of the system with a corresponding negative impact on efficiency in the warehouse.
SUMMARY OF THE INVENTION
A system and method of updating persistent objects in a persistent store is disclosed. In response to receipt of a confirmation of task competition, an attempt is made to acquire a lock for corresponding item data in the persistent store. Regardless of whether the lock is acquired, a successful update of the persistent store is acknowledged to the sender of the confirmation within a defined time period.
BRIEF DESCRIPTION OF DRAWINGS
The invention is illustrated by way of example and not by way of limitation in the figures of the accompanying drawings in which like references indicate similar elements. It should be noted that references to “an” or “one” embodiment in this disclosure are not necessarily to the same embodiment, and such references mean at least one.
FIG. 1 is a block diagram of a system of one embodiment of the invention.
FIG. 2 is a flow diagram of operation system of one embodiment of the invention.
DETAILED DESCRIPTION
FIG. 1 is a block diagram of a system of one embodiment of the invention. SCM node 102 , which is responsible for controlling supply chain management is coupled to a database 108 which persistently stores business objects such as is object 130 . Database may additionally include objects corresponding to individual tasks or task bundles. While a database is used in one embodiment, other types of persistent storage may be used in other embodiments. SCM node 102 may be instantiated on one or more physical boxes and may include one or more virtual machines (VM) executing on such physical boxes. A box may contain a single processor system or any of the various multi-processor systems as known in the art. In some embodiments, SCM node 102 and the persistent storage may not be at the same physical location. In such embodiment, SCM node may communicate with persistent storage 108 over a distributed network.
SCM node 102 may include a wireless interface within a transceiver 110 to permit wireless communications with SCM node 102 . A database manager 112 manages transactions with database 108 . An update module 116 may be used to update objects within the database and may, as further described below, interact with the timer 114 to identify appropriate timing to retry database updates.
A lock server 120 provides database locks to the update module 116 in connection with possible updates of objects within database 108 . In one embodiment, the lock server may be an enqueue server available from SAP AG of Walldorf, Germany. The general function of database lock to prevent inconsistent updates is well understood. In some embodiments, synchronization objects, such as semaphores or mutexes may be used in the locking.
Various user input devices may permit users to access the SCM node 102 . Input terminal 104 may provide user input using a keyboard or pointer device and may communicate with SCM node by a wired or wireless link. RF (radio frequency) scanner 106 may communicate wirelessly either directly to the SCM node 102 or to the input terminal 104 . In some embodiments, input terminal 104 may be a laptop or desktop computer or a work station and may communicate wirelessly or over a distributed network with SCM node 102 . In other embodiments, input terminal 104 may be a dumb terminal with a wired link to SCM node 102 . RF scanner 106 may be a barcode scanner, or for example, read RF identification (ID) tags. Other types of wireless signalling, such as bluetooth, infrared, etc. may be used in other embodiments of the invention. In some embodiments, when a worker is performing tasks in, e.g. a warehouse, the RF scanner 106 is used to signal a confirmation of task completion (or creation). A completion (or creation) of a task generally results in an update of a central object in database 108 . Thus, to update the database object, an update module 116 must acquire a lock for the material to be updated. The confirmation may also cause the creation of additional objects, such as follow on tasks. For example, if the task being confirmed is a picking task, the confirmation may generate a packing task object. Such objects may be necessary for continued efficient operation of the warehouse. Moreover, some time critical information, such as stock reservation, must be handled synchronously with the confirmation to avoid multiple allocations of the same stock.
As noted above, certain synchronous object creations and database updates may be necessitated by business constraints or are otherwise time or logically critical to efficient system operations. These updates to database 108 are performed synchronously when the confirmation is received. For example, stock reservation object 132 may be created synchronously to avoid multiple allocations of picked stock. Other object creations, such as following on task creation, may also be performed. These creations generally do not result in lock collision or lock collision with a meaningful time impact or system response. Conversely, updates to the central object 130 tend to have greater probability of lock collision and when they do, cause significant impact on response time.
In one embodiment of the invention, a data model is employed in the creation of the business objects such the global data 122 in the object is independent of item data 124 , 126 , 128 . In this context, “independent” means that changes to the item data, e.g. 124 , has no necessary effect on the global data 122 . In this manner, it is possible to increase the granularity of the locking to permit locking on a per item basis. Thus, while a lock on the global data 122 would prevent a subsequent requester from obtaining a lock or any of the items (because changes to the global data my affect the item data) a lock on an item data 122 does not prevent a lock on any other item data, e.g. 126 , 128 . This reduces the probability of a lock collision over, as has historically been the case, having a single lock for the entire object.
However, lock collisions still can and will occur. Thus, if as previously noted, lock collisions occur, this could result in significant delay before the update is acknowledged and, e.g. a worker using RF scanner 106 can continue with the next task. Accordingly, in one embodiment, if a lock cannot be obtained within a predetermined time, for example, some suitable fraction of a second, the update module 116 will queue the confirmation for the update of central business object 130 in queue 118 and send an acknowledgement signal acknowledging a successful update to the RF scanner 106 . Queue embodiments of the invention may use various types of data structures as or instead of queue 118 . For example, a FIFO, a linked list, or any other suitable data structure may be used. Queue 118 should ensure that updates for a particular item are processed in the order received at the SCM mode 102 . Thus, a physical queue may be associated with each item having pending delayed updates. In one embodiment, a plurality of queues are present and the queues may be allocated to the items as needed. This early acknowledgement permits the worker with the scanner 106 to proceed to the next task unconstrained by delay in the system. Moreover, because the time critical aspects of the database updates occurred synchronously, e.g., stock reservation, the acknowledgement is valid from the perspective of the recipient of the acknowledgement.
Subsequently, lock acquisition will be retried. For example, in one embodiment, relying on timer 114 , the update module 116 will retry to acquire appropriate locks for the queued confirmations after waiting a specified delay. In one embodiment, timer 114 permits a configurable amount of time between retries. In some embodiments, the waiting time between retries is a function of the number of retries that have been attempted. In this manner, parallel updates may occur to a central business object 130 without the lock collisions negatively impacting worker performance.
FIG. 2 is a flow diagram of operation system of one embodiment of the invention. At block 202 , the determination is made if a confirmation of task completion has been received. If the confirmation is received, at block 202 , the system creates any time critical objects and performs all time critical database updates. As previously noted, such time critical updates tend not to suffer from the same risk of lock collision as updates to the central object. At block 204 , a determination is made whether a lock is available that will permit appropriate update of the business object corresponding to the task. In one embodiment, by attempting to acquire the lock initially rather than immediately queuing the confirmation, the overhead of the queuing system is reduced. If it is, the database is updated at block 206 and acknowledge the successful update is sent to the remote source of the confirmation at block 208 . If it is not possible to acquire a lock at block 204 , the confirmation is queued at block 210 . Then, notwithstanding that the database update has not yet occurred a successful acknowledgement is sent to the source of the confirmation at block 212 . Then at block 214 , the system waits a defined time period after which will retry to acquire a lock to update the business object responsive to the confirmation. Some embodiments may immediately retry, however, because the item is often still locked, it has been found in some system to increase system load without a corresponding benefit.
At block 216 , a determination is made if the retry for lock acquisition was successful. If it was not, the system returns to wait an additional period. As previously noted, this wait period may be configurated and need not be the same between each subsequent retry. If the retry is successful, the database is updated at block 218 . After the successful update at block 218 or after the acknowledgement of successful update at block 208 , a lock is released at block 220 .
By employing a data model which permits high granularity locking, such as locking on an item basis and by further requiring independence of the item data from global data, the instance of lock collision can be reduced. By queuing confirmations when lock collisions occur, and preacknowledging successful updates impact of lock collisions on remote users can be mitigated or eliminated.
While embodiments of the invention are discussed above in the context of flow diagrams reflecting a particular linear order, this is for convenience only. In some cases, various operations may be performed in a different order than shown or various operations may occur in parallel. It should also be recognized that some operations described with respect to one embodiment may be advantageously incorporated into another embodiment. Such incorporation is expressly contemplated.
Elements of embodiments of the present invention may also be provided as a machine-readable medium for storing the machine-executable instructions. The machine-readable medium may include, but is not limited to, flash memory, optical disks, compact disks read only memory (CD-ROM), digital versatile/video disks (DVD) ROM, random access memory (RAM), erasable programmable read-only memory (EPROM), electrically erasable programmable read-only memory (BEPROM), magnetic or optical cards.
In the foregoing specification, the invention has been described with reference to the specific embodiments thereof. It will, however, be evident that various modifications and changes can be made thereto without departing from the broader spirit and scope of the invention as set forth in the appended claims. The specification and drawings are, accordingly, to be regarded in an illustrative rather than a restrictive sense.
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A system and method of updating persistent objects in a persistent store. In response to receipt of a confirmation of task competition, an attempt is made to acquire a lock for corresponding item data in the persistent store. Regardless of whether the lock is acquired, a successful update of the persistent store is acknowledged to the sender of the confirmation within a defined time period.
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FIELD OF THE INVENTION
[0001] The present invention generally relates to a fish bite alarms. More specifically, the system includes a device that releases the fishing line completely from its grasp due responsive to tension from a fish bite on the fishing line.
BACKGROUND OF THE INVENTION
[0002] Fisherman have long used many devices to hold fishing lines, and to alert fishermen of fish bites on fishing lines. As a result, there have been numerous inventions and modifications in the field of fish bite alarms, as well as devices to hold and then release fishing lines. However, these devices do not address the dilemma of alerting the fisherman that a fish has bitten without simultaneously alerting the fish itself. The most common cause of this problem in conventional devices is that the fishing line requires a significant pull (and in some cases a double pull) on it in order to operate the tension necessary to release it from the line holding device, thereby allowing the fishing reel to spin freely. That increases tension is often all a fish needs to realize that a danger is present, and the fish reacts accordingly.
[0003] Thus, there is a clear need for a fishing line holding device which does not require a strong pull to release the line so that the fish is not alerted to danger. A line holding device which provides an immediate, tangle-free release is also needed. Only a small tension on the line should be required in order to release the line from the grasp of the holding device. Also, since fishing environments can greatly vary, it is also desirable to provide tension control on the line holding device. In this way line tension can be adjusted to best suit the particular circumstances in which the fishing is carried out.
SUMMARY OF THE INVENTION
[0004] Accordingly, it is a first object of the present invention to overcome the drawbacks of the conventional art.
[0005] It is another object of the present invention to provide a fish bite alarm and fishing line release device that is more adaptable than in the conventional art.
[0006] It is a further object of the present invention to provide a fish bite alarm and fishing line release device that requires only a single, extremely slight tug on the fishing line in order to release the fishing line and activate the alarm.
[0007] It is an additional object of the present invention to provide a fish bite alarm and fishing line release device that does not require multiple tugs on the fishing line so that the fish will not shy from the line and hook.
[0008] It is still a further object of the present invention to provide a fish bite alarm and fishing line release device that does not require substantial tension upon the fishing line to release the fishing line held within the fishing line release device.
[0009] It is still another object of the present invention to provide a fish bite alarm and fishing line release device that ensures immediate tangle-free release of the fishing line.
[0010] It is again a further object of the present invention to provide a fish bite alarm and fishing line release device that completely frees the fishing line upon the occurrence of very little tension on the line.
[0011] It is still an additional object of the present invention to provide a fish bite alarm and fishing line release device that remains disengaged after the device is triggered.
[0012] It is yet a further object of the present invention to provide a fish bite alarm and fishing line release device with an alarm signal that can be activated before a fish realizes that it has been hooked.
[0013] It is also another object of the present invention to provide a fish bite alarm and fishing line release device with an alarm that remains active after triggering until manually deactivated.
[0014] It is still a further object of the present invention to provide a fish bite alarm and fishing line release device that is simple to operate.
[0015] It is again another object of the present invention to provide a fish bite alarm and fishing line release device that is easily attachable to a variety of fishing rods.
[0016] It is yet an additional object of the present invention to provide a fish bite alarm and fishing line release device that can be used with different fishing rods and fishing reels, without tangling the fishing line or hindering the reel.
[0017] It is also a further object of the present invention to provide a fish bite alarm and fishing line release device or which line tension can be carefully calibrated.
[0018] It yet an additional object of the present invention to provide a fish bite alarm and fishing line release device contained within a compact housing, and designed so that it provides minimal additional weight or volume to the fishing rod.
[0019] These and other goals and objects of the present invention are achieved by a fish bite alarm and fishing line release device, which is operable in conjunction with a fishing reel that contains the fishing line. The device includes two fingers arranged to hold the fishing line when in a closed position. It also includes an apparatus for opening the fingers when tension is applied to the fishing line.
[0020] In another embodiment, the fishing line release device is operable in conjunction with a fishing reel that contains the fishing line. The device includes a holding device for holding the fishing line. It also includes a spring bias mechanism for triggering the release of the fishing line from the holding device.
[0021] In a further embodiment, the fish bite alarm and fishing line device is operable in conjunction with a fishing reel that contains the fishing line. The device includes an alarm circuit. It additionally includes a spring bias mechanism for removing an insert from the alarm circuit, thereby activating the alarm circuit.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] [0022]FIG. 1 is a perspective view of the invention attached to a fishing rod after it has released a fishing line.
[0023] [0023]FIG. 2 is a side view of the invention depicting the entire fishing rod and fishing reel after it has released a fishing line.
[0024] [0024]FIG. 3 is a front sectional view of the invention while in the engaged mode.
[0025] [0025]FIG. 4 is a side sectional view of the invention while in the engaged mode.
[0026] [0026]FIG. 5 is a top sectional view of the invention while in the engaged mode.
[0027] [0027]FIG. 6 is a side sectional view of the invention while in the disengaged mode.
[0028] [0028]FIG. 7 is a top sectional view of the invention while in the disengaged mode.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0029] The following description provides a detailed explanation of how the present invention achieves the stated objects. As shown in FIG. 1, the device 1 of the invention is completely contained within a housing structure 8 . The compactness of the invention allows for ease of transport as well as ease of attachment to fishing rod 4 . The housing 8 is attached to a fishing rod 4 simply by using elastic bands 7 that hook onto corner protrusions 9 of the housing.
[0030] [0030]FIG. 2 depicts one arrangement in which the invention can be optimally placed close to the handle 3 of fishing rod 4 so that housing 8 is easily reached by a user. This position also affords the capability of attaching the fishing line 2 to the device 1 without pulling the line far from its natural relaxed position. Further, the small size and streamlined shape of device 1 preventing it from entangling the line 2 during the release or extension of the fishing line 2 from the reel 6 .
[0031] The fishing line 2 , when engaged by device 1 , is held between two fingers 12 , 14 . In one preferred embodiment, as depicted in FIG. 4, a plastic finger 12 and a metal finger 14 are used. The plastic finger 12 is rigidly attached to a rotating structure 16 . The metal finger 14 is also attached to structure 16 , next to Finger 12 . However, finger 14 is hinged. This is accomplished using a cylindrical clasp 13 on the base of the metal finger 14 . Clasp 13 is attached to a plastic strip 15 . The plastic strip 15 is joined by a screw 17 to the side of the same rotating structure 16 to which the plastic finger 12 is rigidly attached. The capability of separating fingers 12 and 14 helps to insure that they will be easily separated at the moment of triggering. Also attached to the rotating structure next to the base of the fingers 12 , 14 , is a stop 20 .
[0032] As depicted in FIG. 5, extending from the edge of the rotating structure 16 is an extension piece 19 , which itself is attached to one end of spring 22 . This spring 22 is connected at its other end to an adjustment structure 24 . This structure 24 can be rotated by an external knob 23 for adjusting the tension on spring 22 . The capability to adjust tension on spring 22 allows the selection of the tension necessary to trip the device 1 to be done very precisely. This adjustment feature makes the invention useful for different types of fishing, such as drift or still fishing.
[0033] On the other end of the rotating structure 16 , as depicted in FIG. 5, is another extension 40 . This extension is placed as an insert between one conductor 36 that is flat against the housing of the invention and a second conductor 38 that is flexibly attached to an alarm switch 30 . That the extension 40 and the fingers 12 , 14 are controlled by the same rotating structure 16 , and ensures that the alarm 32 will be activated simultaneously with the release of the fishing line 2 . The flat conductor 36 is connected to a battery 34 . This battery is connected through conductors 36 and 38 to the electronic alarm device 32 . The alarm switch 30 can be operated to cut off alarm device 32 . Alarm switch 30 is accessible through a hole in the invention's housing 8 .
[0034] In one preferred embodiment, the invention's housing 8 has a series of holes above the alarm device 32 in order to pass the sound clearly when triggered. Alternative alarm devices may also include flashing lights, vibrators, buzzers, bells, or any other type of aural or visual signal. There can also be variations in sound, with such alternatives as a constant tone, intermittent tone, or variable pitch. The alarm device 32 is connected to the alarm switch 30 , thus completing the circuit.
[0035] In operation, once the spring's 22 tension has been set, the fingers 12 , 14 can be rotated towards the engaged position as seen in FIG. 4. When the rotating structure 16 is moved towards the engaged position, the plastic finger 12 and metal finger 14 extend themselves outside of the invention's housing 8 . During the same rotation of structure 16 , the insert 40 is automatically placed between the flexible conductor 38 and immobile conductor 36 by the rotating action of structure 16 . The fishing line is manually placed between the plastic finger 12 and metal finger 14 .
[0036] When a fish first touches the fishing line 2 or a hook attached thereto a tension is applied to the line. The appropriate tension (as selected by the adjustment of spring 22 ) on the line is sufficient to force the rotating structure 16 to return to its disengaged position, as depicted in FIG. 6. The rotation is halted by the stop 20 hitting the inner wall of the invention. This prevents the plastic finger 12 from further movement. The metal finger 14 , however, is attracted by a magnet 26 attached to the wall of the invention. This attraction helps the metal finger 14 to continue rotating until it connects with the stationary magnet 26 . This separation of the fingers 12 , 14 quickly releases the fishing line 2 from their grasp. Simultaneous with the release of the fishing line 2 is the rotation of the insert 40 . When the insert 40 is drawn away from its engaged position, the flexible conductor 38 is spring biased to make contact with the immobile conductor 36 , completing the alarm circuit. The alarm 32 preferably remains on until manually disabled to ensure that the user is actively aware of the device 1 triggering.
[0037] In an alternative embodiment only a single finger need be used if positioned with the proper reel bail setting. In this embodiment the fishing line 2 is looped about the single finger, and the rotation of structure 16 allows the fishing line to slip off without undue tension on the line. In another arrangement using a single finger with an open reel bail, the line will slip off the finger with no rotation of 16 . The use of a magnet is similarly part of a preferred embodiment, but not necessarily required for all versions of the present invention.
[0038] While the present invention has been described with reference to certain specific embodiments, it should be clear that these are only examples, and the present invention is not limited thereto. Accordingly, the present invention should be construed to include any and all variations, modifications, adaptions, and embodiments, or equivalents that would occur to one skilled in the art, once having appreciated the present application. Therefore, the present invention should be limited only by the scope of the appended claims.
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An improved fish bite alarm and fishing line release device that provides immediate release of a fishing line and activation of a fish bite alarm due to the use of spring biasing. The line holding and release device preferably includes two fingers arranged for holding the fishing line, a spring bias means for triggering the release of the line, an alarm circuit, and a spring bias means for activating the alarm circuit.
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