A process for purifying p-phenylenediamine color developers in their free-base form. The process includes subjecting a solution containing p-phenylenediamine-type free base color developer to short path distillation which includes at least one of falling film evaporator, thin film evaporator, wiped film evaporator, or short-path evaporator.

This invention pertains to a process for purifying p-phenylenediarnine-type color developers used in photographic color development and reproduction applications. More particularly, the present invention relates to a process for purifying p-phenylenediamine-type photographic color developers in their free-base that are substantially free of sulfate ions. This invention permits the preparation of useful solid and solution compositions of p-phenylenediamine color developers in the free-base form. In another embodiment of the present invention, the method provides an improved process for preparing p-phenylenediamine color developers in the acid salt form.
The basic processes for obtaining useful color images from exposed color photographic silver halide materials include several steps of photochemical processing such as color development, silver bleaching, silver halide fixing and water washing or dye image stabilizing using appropriate photochemical compositions.
The photofinishing industry is comprised of three primary segments: the manufacture of photographic chemicals to supply photochemical formulators, the formulation of these chemicals into useful compositions for photochemical processing, and the processing of sensitized photographic color elements. Formulated photographic processing (photofinishing) solutions provided to the processors are complex, multi-part, multi-component mixtures, the specific compositions of which vary significantly according to the intended use and the formulator.
The types of materials which are ultimately mixed by a photofinisher just prior to use and delivered to the photo processing bath include: solubilizing agents, e.g., organic co-solvents; bases for pH control; color developing agents or color developers; preservatives; antifoggants; sequestering agents; buffering agents; clarifying agents; stain-reducing agents; anti-bacterial or anti-fungal agents; surfactants; and other function-specific materials.
In conventional silver halide color photography, photofinishing solutions in the final processing bath includes a color developer, a preservative, and a solvent or combination of solvents. The color developer agent, in its free base form, serves to amplify the latent image on the silver halide crystals by reacting, in its oxidized form, with a dye-forming color coupler and subsequently, produce a color image of the exposed, sensitized photographic color element.
Suitable color developing agents that are known in the art include aromatic amino color developing agents such as p-phenylenediamines, and particularly the N,N-dialkyl-p-phenylenediamines in which the alkyl groups or the aromatic nucleus can be substituted or unsubstituted. The p-phenylenediamine color developers most commonly present in photofinishing compositions include: N,N-diethyl-2-methyl-p-phenylenediamine monohydrochloride (CD-2); N-ethyl-N-2-(methanesulfonylaminoethyl)-2-methyl-p-phenylenediamine sesquisulfate monohydrate (CD-3); and N-ethyl-N-(2-hydroxyethyl)-2methyl-p-phenylenediamine sulfate (CD-4), listed here in the commonly used acid salt is form.
Color developing compositions are commonly supplied in multiple parts or solutions because of the requirement to separate components which are reactive or unstable over extended periods of time. One part normally includes an acid salt of a p-phenylenediamine color developer, typically in the form of a stabilized aqueous solution. These solutions are acidic since the color developer is formulated in this part as the acid salt. Another part typically contains a base or combination of bases which, upon mixing of the parts, serves to neutralize the acid associated with the part containing the color developer and to establish the desired alkalinity of the mixed color developing composition. These solutions are typically mixed immediately before use. Upon combination of all parts and water, a homogeneous color developing composition can usually be obtained for the working strength solution in the processing machine.
There is a desire in the industry to reduce the number of parts used to prepare color developing compositions, and particularly to prepare replenishing solutions. A wide range of compositions are described in the art or commercially available as xe2x80x9cready to usexe2x80x9d solutions, concentrates or dry formulations. Liquid concentrates have only to be diluted with water to provide a working strength solution. Dry formulations need only be dissolved in water.
The free-base forms of these color developers are presently industrially processed in solutions as non-isolated intermediates prepared from the acid salt form of the p-phenylenediamine. The free base form of the color developer is prepared by mixing an aqueous solution of the color developer salt with sodium hydroxide. For example, US Pat. Nos. 6,017,687 issued to Darmon et al. on Jan. 25, 2000 and 6,077,651 issued to Darmon et al. on Jun. 20, 2000 disclose a homogeneous, single-part, chloride ion-free color developing concentrate that is prepared using a critical sequence of steps. In the first step, an aqueous solution of the color developing agent is prepared typically from the sulfate salt and an alkali metal base to provide a stoichiometric proportion of alkali metal ions to render the color developer in a free base form. A disadvantage of obtaining the free base color developer in this manner is that an insoluble sulfate salt that precipitates from the solution. The solid precipitate must then be removed from the solution in an extra step. Additionally, due to the solubility of the sulfate salt there will always be some residual sulfate ions in solution, which these patents teach is detrimental to the composition stability of a photofinishing solution.
The use of such combined photofinishing solutions results in simplicity of operation with a reduction in the potential of mixing errors and poor photoprocessing results. The major incompatibility of the traditional parts of photofinishing solutions is that between the acidic aqueous part, containing the acid salt of the p-phenylenediamine color developer, and the alkaline part, containing the base or combination of bases. Since the active color developer in the final, mixed photofinishing composition is the free base form of the color developer, full consolidation of parts to produce a single-part formulation requires a source of the p-phenylenediamine color developer in free base form as the necessary ingredient. As used herein, the term xe2x80x9cfree-basexe2x80x9d refers to phenylenediamine compounds devoid, or essentially devoid, of acid addition salts of phenylenediamines.
The preparation of N,N-disubstituted p-phenylenediamines has been known for many years; the earliest and most complete summary of the preparation of these compounds is found in the Journal of the American Chemical Society (Bent, Dessloch, Fassett, James, Ruby, Sterner, Vittum, and Weissberger, JACS 73, 3100-3125, 1951). For the synthesis of each of 61 N,N-disubstituted p-phenylenediamines, the last step was a reduction of either a nitroso, nitro, or an azo precursor. These nitroso, nitro, or azo precursors were subsequently reduced to the desired N,N-disubstituted p-phenylenediarnines (Free Bases) under the conditions of zinc and hydrochloric acid in water or by catalytic hydrogenation in ethyl alcohol. Generally, for the purposes of the present invention, the p-phenylenediamine free bases are prepared by the hydrogenation of a water-wet nitro or nitroso precursor in an alcohol solution in the presence of a heterogeneous hydrogenation catalyst under hydrogenation conditions of temperature and pressure. The heterogeneous catalyst is separated from the solution, providing p-phenylenediamine free base solutions with typical composition ranges of 25-40 weight percent p-phenylenediamine free base, 40-50 weight percent of the alcohol solvent, 15-25 weight percent water, and 2-6 percent (by difference) of total impurities. These intermediate free bases were purified by either crystallization or distillation, then converted to their more stable acid salt form.
Manufacturers of p-phenylenediamine color developers have avoided the use of traditional batch distillation process technology of the free base form due to oxidative and thermal degradation. Degradation by-products have been found to impart adverse effects on the photographic quality, rendering such distilled products unfit as a photographic color developer. A secondary factor in avoiding conventional distillation has been the low process yield.
Recovery of the p-phenylenediamine color developers by crystallization is also not without its problems. The resulting solution of the free base color developer is generally purified by contacting the solution with a decolorizing agent, such as activated carbon, which results in significant product yield losses to the decolorizing agent. Following decolorization, an appropriate mineral acid is added to the solution to convert the free base to its respective acid salt. The solution is cooled and the acid salt of the color developer is isolated by filtration. Although the filtrate typically contains a significant amount of the desired product, it is usually discarded due to the high concentration of impurities in the stream. In addition, the presence of water in the filtrate increases the solubility of the color developer acid salt and contributes to further yield losses to the filtrate. Typically, the isolated acid salt precipitate undergoes a re-crystallization step to achieve acceptable purity. Re-crystallization can be performed in an alcohol or ether solvent with a diminished yield loss, compared to the initial crystallization. The filtrate from this second crystallization is generally pure enough to permit the recycle of all or a significant portion of it. Accordingly, in current industry practice, there are significant yield losses which negatively impact the process economics and purity of the free base precursor to the acid salt.
There is a need for a process whereby direct purification and isolation of the color developer free base can be achieved with acceptable purity and which overcomes the yield losses and additional costs associated with current process technology.
The present invention provides a process for the purification of p-phenylenediamine color developers in their free-base form. The process includes the steps of subjecting a solution containing said free base color developer to short path distillation having a temperature less than about 250xc2x0 C. and a pressure of less than about 10 mm of mercury and wherein said short path distillation includes at least one of falling film evaporator, thin film evaporator, wiped film evaporator, or short-path evaporator.
Yet another aspect of the present invention is an improved method for preparing an acid salt from the p-phenylenediamine free base color developer. The method includes the steps of: a) dissolving a purified p-phenylenediamine free base distillate in an organic solvent; b) contacting the dissolved free base distillate with an appropriate mineral acid; and c) crystallizing the color developer in the acid salt form.
It is an object of the present invention to provide a process for purifying p-phenylenediamine color developers, in their free-base form.
It is another object of the present invention to provide an improved method for preparing an acid salt of a p-phenylenediamine color developer.
These and other objects and advantages of the present invention will become more apparent to those skilled in the art in view of the following description and the accompanying drawing wherein like parts and objects have similar reference numerals. It is to be understood that the inventive concept is not to be considered limited to the constructions disclosed herein but instead by the scope of the appended claims.

Method for purifying free-base p-phenylenediamine-type photographic color developers

Abstract: Another aspect is a method for preparing an acid salt from a p-phenylenediamine free base color developer. The method includes the steps of: a) dissolving a purified p-phenylenediamine free base derived from the short path distillation process in an organic solvent; b) contacting the dissolved free base distillate with an appropriate mineral acid; and c) crystallizing the color developer in the acid salt form.


A catalyst used for trimerization of ethylene into 1-hexene is descrobed, which comprises (i) a specific organometallic complex having a neutral multidentate ligand having a tripod structure, (ii) an alkylaluminoxane, and an optional ingredient selected from:    (iii) a halogenated inorganic compound,    (iv) a specific alkyl group-containing compound,    (v) a combination of a halogenated inorganic compound with a specific alkyl group-containing compound,    (vi) an amine compound and/or an amide compound, and    (vii) a combination of an amine compound and/or an amide compound with a specific alkyl group-containing compound.

(1) Field of the Invention
This invention relates to a catalyst for trimerization of ethylene and a process for trimerizing ethylene using the catalyst. More specifically, it relates to a catalyst exhibiting an enhanced activity for trimerization of ethylene to produce 1-hexene, which is used as a comonomer for the production of linear low-density polyethylene (LLDPE), and further to a process for trimerizing ethylene by which 1-hexene can be produced effectively and highly selectively.
(2) Description of the Related Art
It is known to use a chromium compound as a catalyst for trimerization of ethylene to give 1-hexene. For example, a catalyst system comprising a chromium compound, polyhydrocarbylaluminum oxide and a donor ligand is described in Japanese Unexamined Patent Publication No. (hereinafter abbreviated to "JP-A") S62-265237. A catalyst system comprising a chromium compound, a pyrrole-containing compound, an alkyl metal compound and a halide is described in JP-A H6-239920. A catalyst system comprising a chromium compound, an alkyl metal compound, and an acid amide or imide compound is described in JP-A H8-59732. A catalyst comprising (i) a complex of chromium salt with a multidentate ligand selected from phosphine, arsine and stibine, and (ii) aluminoxane is described in JP-A H6-298673. A catalyst comprising (i) a chromium-chlorine complex or alkyl chromium complex having a specific nitrogen ligand and (ii) an aluminum compound is described in JP-A H10-7712. A catalyst comprising (i) a chromium complex having a cyclic polyamine or hydro-tris(pyrazolyl)borate ligand and (ii) an alkyl aluminum compound is described in JP-A H10-231317.
However, these chromium catalysts have problems as explained below.
When the catalyst of JP-A S62-265237 is used for trimerization of ethylene, a large amount of polyethylene is produced in addition to 1-hexene. When the catalyst of JP-A H6-239920 is used, the amount of polyethylene produced can be reduced. However, a pyrrole-containing compound, which is one ingredient of the catalyst, is extremely unstable to air, and readily deteriorated and colored. Thus, a pyrrole-containing compound is troublesome to handle, and a treating process or apparatus for removing a coloring matter from the catalyst or purifying the catalyst is needed.
As for the catalyst of JP-A H8-59732, among the acid amide or imide compounds, which are one ingredient of the catalyst, maleimide is optimum for the catalytic activity for trimerization of ethylene. However, maleimide has problems such that it has a poor solubility in an organic solvent and the catalyst is troublesome to prepare, and further that it is not readily commercially available and is expensive.
The catalyst of JP-A H6-298673 has a problem such that it is difficult to carry out a process for trimerization of ethylene with a good reproducibility. The catalyst of JP-A H10-7712 has a poor activity for trimerization of ethylene. The catalyst of JP-A H10-231317 has problems such that a large amount of polyethylene is undesirably produced, and that the selectivity to 1-hexene among oligomers is low.

Catalyst for trimerization of ethylene and process for trimerizing ethylene using the catalyst


An inspection system may receive inspection datasets from a defect inspection system associated with inspection of one or more samples, where an inspection dataset of the plurality of inspection datasets associated with a defect includes values of two or more signal attributes and values of one or more context attributes. An inspection system may further label each of the inspection datasets with a class label based on respective positions of each of the inspection datasets in a signal space defined by the two or more signal attributes, where each class label corresponds to a region of the signal space. An inspection system may further segment the inspection datasets into two or more defect groups by training a classifier with the values of the context attributes and corresponding class labels for the inspection datasets, where the two or more defect groups are identified based on the trained classifier.

Defect inspection systems identify and/or classify defects on semiconductor wafers. A given semiconductor wafer may include hundreds of chips, each chip containing thousands of components of interest, and each component of interest may have millions of instances on a given layer of a chip. Inspection systems may thus generate vast numbers of data points on a given wafer. As a result, properly segmenting these datapoints into different groups to efficiently generate useful information is an ongoing challenge for defect classification. For example, defect segmentation may facilitate various aspects of a fabrication process including, but not limited to, defect discovery, defect classification, nuisance filtering, or selecting optics to achieve a desired level of performance.
Defect segmentation is typically performed as a post-inspection step and is often carried out with the assistance of a human expert (e.g., supervised segmentation). However, the demand for ever-shrinking devices leads to increased demands on inspection systems. For example, as design rules shrink, differences between the noise floors associated with defects of interest relative to nuisance inspection datapoints may also shrink. As a result, segmentation based solely on attributes of a signal generated at a defect site or context attributes may be insufficient or ineffective. Further, the number of attributes that may be used for defect segmentation may make supervised segmentation inefficient or impractical. Therefore, it would be desirable to provide a system and method for curing shortcomings such as those identified above.


Benzyl-phosphonate compounds represented by the formula I: ##STR1## are disclosed as useful in treating bone wasting diseases and as an immunosuppresant.

Osteoporosis is a bone-wasting disease in which there is an imbalance or uncoupling between the rate of bone formation and resorption resulting in a decrease in total bone mass. As a result of this decrease in bone mass the skeleton becomes weakened and unable to bear the normal weight-bearing stresses. The effects of osteoporosis are generally seen in the weight-bearing bearing parts of the skeleton, especially the spine and hips, which can frature in the absence of trauma. Osteoporosis affects about 24 million people in the United States and 200 million people worldwide and is blamed for 2.5 million fractures a year in elderly women. The American Medical Association estimates that as many as 25% of women will suffer fractures of the hip or spine in their lifetime as a result of osteoporosis.
The current therapies for postmenopausal osteoporosis consist of treatments which are for the most part preventive; estrogen replacement, bisphosphonates, vitamin D metabolites and calcium supplements act to inhibit bone resorption associated with the onset of menopause. Estrogen replacement in these patients is quite effective in reducing further loss of bone mass but it does not induce an increase in bone mass which is needed to reduce fracture risk and pain. These treatments have little utility in the treatment of those patients with existing osteoporosis-induced loss of bone mass who have a high fracture risk and back/joint pain. Post-menopausal women with vertebral bone mass of less than 100 mg/cc would be considered below the "fracture threshold" and would be candidates for treatment with an agent which would increase bone mass and thereby restore lost bone. The present invention focuses on agents which are useful in treating bone wasting diseases by increasing an individuals bone mass and thus reducing fracture risk. The therapeutic need for this type of agent is clearly present, especially when one considers the poor patient compliance associated with estrogen replacement therapies. Modification of the immune system by pharmacologic agents is also rapidly emerging as a major area of therapeutics. While organ transplantation alone extends the lives of thousands of patients per year, disease such as diabetes mellitus, rheumatoid arthritis, multiple sclerosis and psoriasis affect millions more and have been shown to involve reactions to autoantigens. A role for immunosuppressive agents has not only been recognized in these cases but approved for therapy as well. These include Cyclosporine, FK-506, Azathioprine, adrenocorticosteroids and Methotrexate. These drugs all have serious toxicities associated with them such as renal toxicity (Cyclosporine, FK-506), leukopenia, thrombocytopenia (Azathioprine), hepatic fibrosis and cirrhosis (methotrexate) and psychoses, cataracts, glucose intolerance, bone dissolution (Adrenocorticosteroids). Clearly a need exists for an orally active specific inhibitor of T-cell function. The present invention describes agents which inhibit a crucial enzyme unique to T-cells (CD-45) and thus provide a more specific and less toxic approach to immunosuppression.
The assignees of the present invention recently filed an application Ser. No. 732,267 directed to certain novel benzylphosphonates. Such compounds were shown to have activity in treating bone wasting diseases. They are, however, structurally different from the compounds of the present invention.

Arylmethylphosphonic acid derivatives useful in treating bone wasting diseases


An electrostatic charge image developing toner includes toner particles and silica particles, wherein the silica particles have an average equivalent circle diameter of from 70 nm to 400 nm, an average circularity of from 0.5 to 0.9, and a pore volume of from 0.05 cm3/g to 2.5 cm3/g.

1. Technical Field
The present invention relates to an electrostatic charge image developing toner, a toner container, and an image forming apparatus.
2. Related Art
In electrophotography, typically, an image is formed through multiple processes including using various means to form an electrostatic charge image on a surface of a photoreceptor (image holding member) formed of a photoconductive material; developing the formed electrostatic charge image using a developer containing a toner to form a toner image; transferring the toner image onto a surface of a transfer medium such as paper, and optionally, through an intermediate transfer medium; and fixing the toner image on the surface of the transfer medium, for example, by applying heat or pressure or applying both heat and pressure.
As the toner for forming this image, a toner containing toner particles that contains a binder resin and a colorant; and an external additive that is externally added to the toner particles is used in many cases.

Electrostatic charge image developing toner, toner container, and image forming apparatus


A grain flour includes milled grains of at least one grain selected from the group consisting of barley and oat. In the grain flour, the average grain diameter is in the range of 40-100 μm. The content of grains having a grain diameter less than 20 μm is not greater than 20 mass %, the content of grains having a grain diameter in the range of 20-100 μm is in the range of 20-60 mass %, the content of grains having a grain diameter greater than 100 μm and not greater than 500 μm is in the range of 20-60 mass %, and the content of grains having a grain diameter greater than 500 μm is not greater than 5%. An application food using the grain flour is produced from a starting material which contains at least 5% of the grain flour. A method for producing the grain flour is also provided.

Barley is a grain that has been a familiar part of the Japanese diet since ancient times in the form of cooked barley and rice, and the like. With the spread of polished rice and the Westernization of food, the consumption of barley has decreased. In recent years, it has accounted for only a small part of grain consumption. The annual per capital consumption of barley in Japan is 0.3 kg, as compared to about 60 kg for polished rice and 33 kg for wheat (Non-Patent Reference 1). Additionally, grains such as barley and oats contain relatively large amounts of β-glucans, a water-soluble dietary fiber, physiological functions of which have drawn considerable attention. β-Glucans are polysaccharides with 1-3 and 1-4 glucose bonds ((1-3), (1-4)-β-D-glucans). They are also the primary component of the walls of barley endosperm cells, constituting about 70 percent. There have been many reports of the health functions of β-glucans. For example, the US Food and Drug Administration (FDA) has allowed health claims that barley β-glucans have the effects of lowering serum cholesterol levels and reducing the risk of coronary heart disease (for example, Non-Patent Reference 2).
In Japan, as well, there have been reports that the dietary consumption of barley and oats lowers blood cholesterol (for example, Non-Patent References 3 and 4) and inhibits a rise in blood sugar level following a meal (for example, Non-Patent Reference 5). There have also been reports of various researches on dietary fiber and cancer prevention (for example, Non-Patent Reference 6).
As stated forth above, barley and oats are grains known to contain relatively large amounts of β-glucans. The content thereof is normally said to be about 3 to 6 mass % (for example, Non-Patent Reference 7). Accordingly, numerous methods of extracting β-glucans have been investigated. Examples are the method of production by aqueous extraction employing barley as a starting material (for example, Patent Reference 1), the method of obtaining β-glucans by alkali extraction, neutralization, and alcohol precipitation employing barley and oats as starting materials (for example, Patent Reference 2), the method of extracting β-glucans in 80° C. to 90° C. hot water (for example, Patent Reference 3), and the like. While not an extraction method, the method of raising the content of β-glucans in grain by milling and sifting grain has also been proposed (for example, Patent Reference 4).
However, the methods are basically methods of separating and concentrating β-glucans from grains such as barley. As set forth above, the quantity of β-glucans in grains such as barley is about 3 to 6 mass %. Compared to other components such as starches and proteins, this content is quite low. Accordingly, the residue following extraction is quite large relative to the β-glucan finished product, and must be used in low value-added products such as animal feeds or discarded as waste. Thus, the cost per unit of the product necessarily rises, restricting its use to certain supplements and in common foods, and rendering its widespread use problematic.
Thus, most of the methods that have been proposed thus far consist of concentrating the components of natural materials with health functions by extraction and separation for use in supplements and common foods. The artificial use of some of the components of natural materials and their use in medical treatment is effective in cases such as when it is necessary to control the intake of other natural components. However, such uses are not necessarily suitable in cases of consumption as common foods. For example, the good compositional balance of natural components ends up being compromised, harmful substances end up being unintentionally concentrated and accumulated, and large quantities of unused waste end up being produced as by-products. As a result, there tends to be a drawback in the form of high production costs.
There have also been efforts to popularize barley foods in which barley is utilized as is as a foodstuff (for example, Non-Patent Reference 7). However, the consumption of cooked barley and rice is limited. There is thus a need to develop various applied foods. When employed in applied foods, it is necessary to utilize not just polished barley grains, but to produce flour and formulate it into various food materials.
The milling of grains for use in foods has been a common practice since ancient times. Dietary fibers, including grain flours containing β-glucans, are commercially available. However, most of the β-glucan-containing grain flours thus far have had coarse particles, and most have lacked whiteness and been grayish-brown. There have been limits to the ability to provide foods that are both tasty and appealing in appearance.
Various methods of reducing the size of the particles of barley flour have been examined for such purposes. For example, the effects of different methods of milling on properties have been examined with the goal of developing a hulless barley flour that is suitable to processing (for example, Non-Patent References 8, 9, 10).
The development of types of barley that contain high contents of dietary fiber, particularly β-glucans 7 to 10% or more, through the improvement of barley varieties has been advancing (for example, Non-Patent Reference 13). The possibility of taking in quantities of β-glucans that are suited to the health without separating and concentrating β-glucans is increased by using these barley varieties with high β-glucan contents.

NATIONAL UNIVERSITY CORPORATION SAITAMA UNIVERSITY


The present invention relates to a method for forming self-aligned metal silicide contacts over at least two silicon-containing semiconductor regions that are spaced apart from each other by an exposed dielectric region. Preferably, each of the self-aligned metal silicide contacts so formed comprises at least nickel silicide and platinum silicide with a substantially smooth surface, and the exposed dielectric region is essentially free of metal and metal silicide. More preferably, the method comprises the steps of nickel or nickel alloy deposition, low-temperature annealing, nickel etching, high-temperature annealing, and aqua regia etching.

The technological development of micro-sized semiconductor integrated circuit devices has required improved methods for making conductive contacts to the semiconductor impurity regions. Metal silicides have proven to be excellent contact materials, which can be readily formed in a self-aligned manner by a salicidation process.
Formation of metal silicide contacts through the salicidation process typically involves the steps of depositing a thin metal layer (e.g., less than about 15 nm in thickness) that contains a silicide metal or metal alloy (i.e., a metal or metal alloy that is capable of reacting with silicon to form metal silicide) uniformly over a semiconductor substrate that contains both silicon-containing device regions and dielectric isolation regions, heating the semiconductor substrate to form silicide over the device regions, and then selectively etching away the unreacted metal from the dielectric isolation regions. For successful fabrication of high performance semiconductor devices, the etching should be highly selective, i.e., it removes all unreacted metal or metal alloy from the dielectric isolation regions, without attacking or otherwise damaging the silicide on the device regions.
Nickel or nickel alloy, such as nickel-platinum alloy, have been commonly used as the silicide metal for forming the silicide contacts in the CMOS technology.
Specifically, for forming pure nickel silicide contacts, a rapid thermal annealing (RTA) step is typically employed to convert the deposited thin nickel layer located on the device regions into nickel silicide, followed by a nickel-etching step to remove the unreacted nickel from the dielectric isolation regions. However, residual material, probably nickel silicide, tends to form over the dielectric isolation regions after the RTA step. Such residual material cannot be satisfactorily removed by the etchant(s) used in the nickel-etching step. The presence of residue material on the dielectric isolation region significantly increases the risk of shorting between device regions and reduces the device reliability. This problem becomes more severe as the RTA temperature increases.
Further, for forming silicide contacts that contain nickel silicide as well as one or more other metal silicides, such as platinum silicide and/or rhenium silicide, a nickel alloy layer that contains nickel and one or more additional silicide metals, such as platinum and/or rhenium, is deposited over the semiconductor substrate. An RTA step is also employed to convert nickel and platinum/rhenium into nickel silicide and platinum/rhenium silicide in the device regions, followed by an aqua regia (AR) etching step to remove both the unreacted nickel and platinum/rhenium from the dielectric isolation regions. Similar problem exists due to presence of residual material over the dielectric isolation regions after the RTA step.
Moreover, when the RTA temperature equals or is less than about 400° C., the silicides formed by the RTA is highly susceptible to attacks by the AR etchant, and significant damages to the silicide contacts may result during the AR etching. On the other hand, when the RTA is carried out at a higher temperature (e.g., >600° C.), gross formation of residual material is observed over the dielectric isolation regions. FIGS. 1A and 1B illustrate silicon contacts formed by conventional RTA/AR etching processes. Specifically, silicide contacts 3 and 5, which preferably contain nickel silicide and platinum silicide, are formed over a semiconductor substrate 1 that includes two silicon-containing semiconductor device regions 2 and 4 with a dielectric isolation region 6 therebetween. When the RTA temperature is not high enough, the silicide contacts 3 and 5 will be severely damaged by the AR etching, thereby resulting in a very irregular surface morphology, as shown in FIG. 1A. On the other hand, when the RTA temperature is higher, residual materials (e.g., nickel-platinum-silicide), which are denoted by layer 7, can be formed over the dielectric isolation region 6, as shown in FIG. 1B.
There is therefore a continuing need for an improved method for fabricating the silicide contacts on semiconductor substrates, which is capable of both minimizing the formation of residual materials on the dielectric isolation regions and reducing etching damages to the silicide contacts.

This patent is subject to a terminal disclaimer.

Method for forming self-aligned metal silicide contacts

International Business Machines Corporation


An articulated railway bogie connector 10 is shown comprising a male connector component 12 and a female connector component 14. The articulated connector 10 is adapted to pivotally mount to a bolster 54 of a railway bogie 50. The male and female connector components 12, 14 are arranged to be welded to a skeletal body of adjacent railway wagons. The male and female connector components 12, 14 each include a pair of constant contact sidebearer outrigger brackets and associated wear plates located. The outrigger brackets such as 16A/B are in the form of a pair of wing members cast integral with and extending laterally of the male connector component 12. However the wing members such as 16A/B may be welded or otherwise formed integral with, in this instance, the male connector component 12. The outrigger brackets or wing members 16A/B and 18A/B are adapted for fixing of a wear plate which is arranged in use to contact corresponding constant contact sidebearers mounted to the articulated bogie 50.

Articulated railway freight trains where adjacent wagons are mounted at adjacent ends to an interconnecting railway bogie are known. The bogie includes a pair of side frames spaced apart by a bolster on which the wagons are mounted via an articulated connector. The articulated connection is provided by mating male and female components of the articulated connector which are respectively welded into the sill of adjacent wagons. Sidebearer support brackets are either cast or welded/fabricated separate of the bolster and thereafter welded or bolted to the bolster.
Adjacent ends of the wagons in an articulated railway freight train also include mountings for sidebearer wear plates which in use contact corresponding constant contact sidebearers mounted on the bogie bolster. In U.S. Pat. No. 4,233,909 wagon-mounted mountings for sidebearer wear plates are shown as very large support arms extending from the wagon ends.


The present invention provides a floatable golf ball for a driving range having excellent durability and good shot feel. The present invention relates to a floatable golf ball for a driving range comprising a core and a cover covering the core, wherein                the cover has a flexural modulus (F) of 80 to 300 MPa,        the golf ball has a specific gravity of not less than 0.5 and less than 1.0, and a deformation amount (D) of 3.0 to 6.0 mm when applying from an initial load of 98 N to a final load of 1275 N, and        a ratio (F/D) of the flexural modulus of the cover (F) to the deformation amount of the golf ball (D) is within the range of 15 to 50.

There are driving ranges for practicing golf, in which golf balls are hit facing water surface of a lake and collected from water. The golf balls should float on the water surface and therefore have a specific gravity of less than 1.0. These types of driving ranges are called hereinafter as "water-facing driving range" and these golf balls are called as "floatable golf ball". The performance, which is required for golf balls for usual land-facing driving ranges, is firstly excellent durability, and secondly good shot feel as good as golf balls for round games.
In case of the floatable golf balls for water-facing driving ranges, since it is further required to float on water in order to easily collect the golf balls after hitting, it is a necessary condition for the golf balls to have a specific gravity of less than 1.0. As a golf ball which satisfies the required performance, that is, durability, shot feel and specific gravity, one-piece golf ball has been mainly employed. This is because the one-piece golf ball is suitable for satisfying the required performance, and particularly because the golf ball has excellent durability.
Recently, it has been required also for the golf balls for usual driving ranges to have excellent performance nearly as good as golf balls for round games. Therefore so-called two-piece golf ball, which is formed by covering a cover, has been employed as a floatable golf ball for water-facing driving ranges. A two-piece floatable golf ball for water-facing driving ranges, which has low specific gravity and floats on water, and has good shot feel nearly as good as golf balls for round games, is proposed (Japanese Patent Kokai Publication No. 327791/1994 and the like).
However, the golf ball for round games has possessed very soft and good shot feel and high rebound characteristics by the recent remarkable improvement of performance of the golf ball. Therefore the two-piece floatable golf ball for water-facing driving ranges was evaluated to have good shot feel when it was proposed, but such a conventional golf ball for driving ranges does not agree with requirement for the existing golf ball. It is problem that the conventional golf ball for driving ranges is very hard and has poor shot feel, because the core is hard and stiffness of the cover is too high.


A method for selectively depositing a source material on a wafer is disclosed. In one embodiment, a wafer is having at least one recessed feature is provided. A top surface of the wafer is then coated with an inhibiting material. Finally, a source material is selectively deposited in the at least one recessed feature, the source material repelled by the inhibiting material. In another embodiment, the inhibiting material is one of a wax, a surfactant or an oil.

FIG. 1a illustrates a cross section of an integrated circuit (IC) employing multilevel metallization. A level of metallization contains electrical connections between elements in an IC. ICs can be manufactured having several layers of metallization to facilitate the increasing complexity and small size of microprocessors and other ICs.
An IC 100 has three layers of metallization 102, 104, and 106. The layers 102, 104, and 106 can be built on top of a single crystal silicon or other substrate 108. The substrate 108 can have semiconductor devices, such as transistors 110 and 112, formed in it. The layers 102, 104, and 106 can include conductive as well as insulating materials to isolate the conductive materials. The conductive materials, such as aluminum or copper, can form conductive lines connecting semiconductor devices such as the transistors 110 and 112, and can be separated and isolated by an insulating interlayer or interlevel dielectric (ILD) comprising a material such as silicon dioxide (SiO2). ILDs 114, 116, and 118 isolate conductive lines from each other and prevent cross-talk and electrical shorts. The IC 100 has several conductive lines, including interconnects 120, 122, 124, 126, 128, 130, and 132, vias 134 and 136, and contacts 138 and 140. The ILDs 114, 116, and 118 can have recessed features such as trenches and vias. Trenches can allow for the interconnects 120-132, which can connect different regions of the IC. Vias 134 and 136 can create electrical connections between the interconnects 120-132, and the contacts 138 and 140 can create connections with the transistors 110 and 112.
A damascene process can create either a trench or a via. A dual damascene process can create both a trench and a via at the same time by creating a via within a trench. Prior processes for fabricating conductive lines might have involved depositing a conductive material over an entire surface and etching away the excess material. This is a subtractive process. The damascene and dual damascene processes create trenches and/or vias in an ILD first, and then deposit metal in the trenches and vias. Excess metal is then removed. These processes are additive rather than subtractive.
FIGS. 1b, 1c, and 1d illustrate a dual damascene process. In FIG. 1b, trenches and vias have been created in an ILD. A layer 150 may have an ILD 152 having several trenches 154, 156, 158, and 160. The ILD 152 may also be patterned to hold vias such as via 162. In FIG. 1c, metal has been deposited on the ILD 152. When a material is being deposited in a trench or via, the deposition process usually leaves excess material 168 on a top surface 170 of the ILD 152. The excess material is typically removed using a chemical mechanical polishing (CMP) process. The CMP process uses a chemical slurry and a rotating polishing pad to polish the top surface 170 of the ILD 152. The rotating polishing pad removes the excess metal material 168 and planarizes the top surface 170 of the ILD 152.
An ILD 152 having a high dielectric constant (k) may be undesirable in many applications because a high-k ILD can promote capacitive coupling between conductive lines. Reducing the resistance and capacitance experienced by interconnects can increase the propagation speed of the signals that travel through the interconnects. Resistance is reduced by using copper rather than aluminum as an interconnect metal, and capacitance can be reduced by using a low-k ILD. SiO2 has a k of approximately 4.0. ILDs having a k of less than 4.0 are generally considered to be low-k.
Thus, in many ICs it may be desirable to use low-k ILDs in order to reduce capacitive coupling and propagation delay. One way to reduce the k of a material is to create pores or air pockets, because air has a very low k of approximately 1.0. However, low-k ILDs created in this way are mechanically weak. When CMP is performed on a low-k ILD, damage may occur to the ILD as a result of vibration and other mechanical forces and stresses caused by the rotating pad.
In FIG. 1d, material has been deposited in the trenches and vias and CMP has been performed to remove excess material. The deposition and subsequent CMP has created interconnects 172, 174, 176, and 178, and a via 180. The deposition of metal typically coats the up areas, or mesas, 170 with material, in addition to depositing material in the trenches 154, 156, 158, and 160. CMP can create various deformities in the ILD 152 such as a sheer induced via failure 182, a surface crack 184, subsurface delamination 186, and line-to-line "bent line" shorts. This damage can be caused by the stresses from mechanical polishing and the porosity of a low-K ILD 152. This physical damage can render an IC 100 useless, as it can cause electrical shorts and other problems.

Method and apparatus for selective deposition


A compressible sealing ring assembly seals an annulus between a radially outer member and a radially inner member. The sealing ring comprises one or more sealing ring members (28), a radially outer wall for sealing with the inner wall of the radially outer member and radially inner wall for sealing with the outer wall of the radially inner member. A compression ring member (10) having a concave lower surface and a convex upper surface exerts an axial force on a sealing ring member to deform the sealing ring member to maintain a seal.

The current method of sealing valve stems uses metal packing adapter rings having configurations to cause structural deformation of the end surface portions of the grafoil rings, so that the inside of the grafoil seal rings maintain sealing capability in response to wear during use.
While the prior art seals are satisfactory for some applications, they do not provide an optimum sealing capability due to their configuration. The flat bottom of such seals prevents sideways extrusion forces from occurring, thereby diminishing the sealing force in these areas. A mismatch shape of the top and bottom of the rings will eventually cause there to be some packing material to be left in the cavity upon metal to metal contract.
The disadvantages of the prior art are overcome by the present invention, an improved compressable sealing ring assembly is hereinafter disclosed.


A method is provided for triple extrusion of a foam material, a coating and one or more flexible flanges attached to the coating or foam material. All three materials are coextruded through a common die and are useful for forming window sashes.

Due to the increasing cost of wood and the attendant cost of detailing wood pieces for building construction, there is a demand for alternatives to solid wood construction products. A particularly detailed piece used in construction of homes and other buildings is a wood window frame, particularly the two panel sliding sashes (double hung) wherein the panels lock together when in the closed position. This type of window requires intricate wood detailing since the profiles of the sashes require grooves to interlock with the exterior (immovable) portion of the window frame, as well as grooves to accommodate single and double pane glass, as desired. The invention may also be used to manufacture other profiles, such as round top, tilt, casement, etc.
Typically, wood sashes are made by intricate cuts into solid pieces of wood, with the final assembly, such as cutting drainage ports, waterproofing and sealing, done by hand. The present invention obviates the need for much of this handwork, while also providing an energy-efficient, durable, and low maintenance product.
A particular advantage of the present invention is that frame profiles may be provided which are energy efficient by use of materials which are more insulative than wood without the need for metal (such as aluminum) sealing or weather-protection. The use of metal on a frame profile diminishes insulative properties. The energy-conservation considerations are particularly important in view of increasingly stringent energy rating compliance standards for windows based on NFRC (National Fenestration Rating Council) U-Values which are being imposed by building code jurisdictions. To meet or exceed these standards, it is desirable to provide a frame profile which is not solid wood, requires minimal hand-work, and which avoids use of metal or energy-inefficient butyl rubber sealers between the glass panes and frame profile.
The present invention provides frame profiles that are not made of solid wood and which can be formed by a triple co-extrusion process whereby the core material of the frame profile is an extrudable foam plastic, at least partially coated with a weather-resistant plastic co-extrusion coating, and further co-extruded with a fluid material to form flexible flanges or ridges to provide sealing and water deflection where desired. The present invention also provides a triple co-extrusion die for making such extruded profiles.
It is therefore an object of the present invention to provide an improved method for making an extruded window sash comprising a foam plastic core material, an outer weather-resistant coating and flexible flanges for sealing and/or water deflection on the coating or core material.
It is a further object of the present invention to provide improved, elongated frame members made of synthetic materials which have improved energy-ratings and which are formed by a triple extrusion process.
It is yet another object of the present invention to provide extrusion dies for triple extrusion of a foam core material, a coating material and flexible flange forming material.
These and other objects will be apparent from the following description and claims, and from practice of the invention.

Triple extruded frame profiles and method of producing same


A height adjustable column for a shipping container building structure. The height adjustable column has an upper sleeve portion, a middle sleeve portion and a lower sleeve. When the column is in the non-extended position the middle sleeve portion is fully slid within the lower and upper sleeve portions and a substantive length of the upper sleeve portion is slid within the lower sleeve portion such that ISO apertures in the middle sleeves are aligned whereby the height of the column is at a reduced height compared to that that of a standard shipping container. When the column is in the extended position locking means on the middle sleeve portion engage and lock with the corresponding slotted apertures on the lower and upper sleeve portions as to support and retain the column at a height equal to or greater than the height of a standard shipping container.

A problem with existing methods of shipping standard shipping containers lies in the height and transport costs of a product which does not take up the full space within the container particularly where the container is to be used as some form of accommodation. In such cases the interior of the container is often almost empty but because the eventual residential height in the container is full height the transport costs are high.
Equally, where accommodation which is greater than the height of a shipping container must be provided the only real option is to provide it as two containers, one without floor, which must be mounted on top of each other. Having a shipping container that can be raised from a height for transportation to a height for use as a building structure is desired.

Height adjustable column for a shipping container building structure


In the case of a method for producing samples for transmission electron microscopy, a sample is prepared from a substrate of a sample material. To this end, the sample material is irradiated by means of a laser beam along an irradiation trajectory in order to produce a weak path in the sample material. The irradiation is controlled such that the weak path crosses a further weak path, which is likewise preferably produced by laser irradiation, running in the sample material, at an acute angle in a crossing region. The substrate is broken along the weak paths. A sample is thereby produced which has a wedge-shaped sample section bounded by fracture surfaces and has in the region of a wedge tip at least one electron-transparent region.

1. Field of the Invention
The invention relates to a method for producing samples for transmission electron microscopy, and to an apparatus suitable for carrying out the method.
2. Description of the Related Prior Art
Since their introduction in the 1930s, transmission electron microscopes have found wide application in various branches of science and industry. Because of the resolution which is substantially better by comparison with light microscopy and lies in the sub-angstrom range for the currently best appliances, the microstructure and nanostructure of various types of preparations can be examined in great detail.
Particularly in the field of characterization of solids, information can be obtained on the atomic scale with the aid of transmission electron microscopy (TEM). In this case, it is possible on the one hand to examine the arrangement of the atoms, while on the other hand it is also possible to access the chemical composition and the electronic structure with the aid of dedicated analysis methods such as x-ray spectroscopy and electron energy loss spectroscopy. The presence of fewer, in exceptional cases even individual, atoms can be demonstrated in the case of electron energy loss spectroscopy.
Up to a few years ago, the electron optical systems used in transmission electron microscopes were not sufficiently good to allow images and analyses at the theoretical spatial resolution limit. The introduction of highly complex aberration correctors and monochromators, which enable control via limiting parameters such as the aperture aberrations and chromatic aberrations of electron lenses, a very much closer approach with regard to spatial resolution limit is presently being made. Whereas it was possible in the 1990s to attain spatial resolutions in the sub-angstrom range only by means of very high acceleration voltages of 1 MeV and more, and to attain the very short electron wavelengths associated therewith, it is presently possible through the use of corrector lenses to advance into the sub-angstrom resolution range even with moderate acceleration voltages of, for example, 80 to 300 keV. This results in advantages with respect, inter alia, to the frequently problematic beam damage of the very thin preparations, which should have only a very slight thickness (order of magnitude of a few 10 nm) for highly resolved imaging and analysis in the examined range.
Consequently, the question of efficient and low-damage methods for preparing the samples for transmission electron microscopy, which are also referred to below for short as TEM samples, arises to an increasing extent. The invention relates in this case specifically to a method for producing TEM samples in which is prepared from a substrate of a sample material a sample which has a wedge-shaped sample section which is bounded by wedge surfaces and has in the region of the wedge tip at least one electron-transparent region.
It is true that thinning is possible in principle in a purely mechanical way, but it requires great manual skill in order to lead to reproducible sample quality at least to some extent. Moreover, there is presently a multiplicity of partially very complex technologies for producing adequately thin, electron-transparent areas on TEM samples. These include, in particular, mechanical prethinning (grinding, polishing, cavity grinding), which is followed by an ion beam etching process, the cutting out of thin sections with the aid of a focused ion beam, and ultramicrotomy.
DE 10 2004 001 173 B4 describes a method for preparing TEM samples in the case of which material is removed from a substrate of a sample material by means of ultrashort pulse laser ablation in a vacuum chamber, this being done in such a way that there remains a narrow web which is subsequently bombarded in a flat angle with an inert gas ions such that an electron-transparent area is produced in the region of the web. Numerous further conventional preparation methods for TEM samples are described in the introduction to the description in this publication.
The methods used for ion beam thinning go hand in hand in principle with the formation of a near-surface amorphization/damage of the sample material, the extent of which is a function of the acceleration voltage of the ions. The amorphization/damage can be more than 10 nm, for example, when use is made of 3 keV gallium ions, while damage thickness of between 3 and 6 nm is frequently observed in the case of typical low-angle ion etching at 3 keV. According to results of relevant investigations, a reduction to below 1 nm is scarcely possible even when use is made of low-energy ion beams (typically 200 eV to 500 eV energy).
For the special case of substrates made from materials with defined cleavage planes, the so-called "Small Angle Cleavage Technique (SACT)" has been proposed (see, for example, J. P. McCaffrey, Ultramicroscopy 38, 149 (1991) or J. P. McCaffrey, Microscopy Research and Technique 24, 180 (1993)). In the case of a piece of a sample material thinned by grinding, with this technique a diamond tip introduces parallel scratch paths of approximately 500 μm width in the direction which assumes an angle of approximately 18.5° relative to a known cleavage plane of the sample material. Subsequently, the preparation is broken along the scratch paths and along the material-specific cleavage plane. In favourable cases, the breaking of the samples results in a tapering preparation with an enclosed angle of approximately 18.5° between the fracture surfaces. In the ideal case, electron-transparent areas which can be examined by means of TEM are located at the outermost end of the wedge-shaped sample section. An advantage of this technique consists in that because of the missing action of ion beams, the prepared TEM samples have no amorphization caused by preparation, and are free from chemical contaminations. Ideally, atomically flat surfaces result on the wedge-shaped sample section. However, the possibilities for using the method are restricted, because it can be used in essence only with sample materials with crystallographically defined cleavage planes. In addition, the method does not lead as a rule to reproducible results. Furthermore, it is difficult to impossible for it to be automated. Finally, it is scarcely possible to implement even a target preparation, since the exact location of the crack initiation cannot be determined accurately enough owing to the coarse scoring.
It is particularly difficult and complicated to prepare cross-sectional preparations that are intended to enable examination of layers, layer systems or structured surfaces substantially perpendicular to the surface normals of the layer structures. Such questions arise to a particular degree in the semiconductor industry, where many thousand cross-sectional preparations are inspected per year in transmission electron microscopes for the purpose of quality control and fault analysis. The benefit of transmission electron microscopy resides here, inter alia, in an extremely high spatial resolution which enables the examination of ever smaller structures on structured semiconductor components. It is becoming increasingly evident that the preparation of high-quality TEM samples with sufficiently thin electron-transparent areas is the step which is limiting throughput. This circumstance is frequently countered by procuring a number of preparation machines, but this, by way of example, is associated with high costs in the case of systems for focused ion beam (FIB) processing.
A plurality of boundary conditions which are to be rendered compatible only with difficulty are typically to be considered when examining structured semiconductor components in the course of quality control and fault analysis. What is frequently involved is to obtain cross-sectional preparations from structured sample material in the case of which the electron-transparent area suitable for examination lies at a position which can be determined with great accuracy and can ideally be derived from the positioning in machines from the process chain. This task is denoted in specialist circles as "target preparation" (or "site-specific preparation"). This target preparation should be performed as quickly as possible so that the results of the quality control can be fed back quickly into the production process of the components. Furthermore, the sample preparation technology should be optimized so as largely to avoid introducing artefacts into the preparation. Typical artefacts include near-surface amorphization (problematic, for example, when cutting out with the aid of a focused ion beam) as well as structural modifications, diffusion, phase changes owing to heat input etc. Finally, the attempt is made, particularly in industrial use, to automate the preparation process as far as possible in order to be able to attain reproducible preparation results in as wide a process window as possible.

Method and apparatus for producing samples for transmission electron microscopy


A hinge for an LCD monitor of a video movie camera is composed of a vertical axle, a barrel, a horizontal axle, a positioning disk, two resilient dished washers, and a seat. The vertical axle is secured on the camera. The barrel is pivotally mounted on the vertical axle. The horizontal axle is rotatably mounted on the barrel. The positioning disk and the resilient dished washers are provided on an end of the horizontal axle. The seat is mounted at the other end of the horizontal axle and the LCD monitor is installed on the seat. The LCD monitor can be smoothly turned about the vertical axle and the horizontal axle, and be stably positioned at any desired positions.

1. Field of the Invention
The present invention is related to an LCD monitor of a video movie camera, and more particularly to a hinge for an LCD monitor by which the LCD monitor can be rotated about a horizontal axis and a vertical axis.
2. Description of Related Art
A video movie camera generally has an LCD monitor pivotally mounted at a left side. A user can turn outwards the LCD monitor to watch images during filming whereby the user can be sure of what is being recorded. The LCD monitor can be turned about a vertical axis and a horizontal axis for adjustment. However, the LCD monitor pivotally mounted on the camera by a conventional hinge cannot be stably positioned at desired positions, so that the user needs to hold the LCD monitor with one hand, which is very inconvenient. Moreover, the LCD monitor is not rotated very easily and smoothly.
Therefore, the invention provides a hinge for the LCD monitor to mitigate and/or obviate the aforementioned problems.

Hinge for an LCD monitor of a video movie camera


A dispenser for the dispensing of particulate solids such as salt and pepper. The dispenser comprises a dispenser body having a plurality of open-ended cylindrical bores, each bore defining a space adjacent the bottom end thereof into which particulate material can be inserted and the open ends of the bores being threaded to receive a threaded closure. A threaded closure is associated with each of the bores. The threaded open ends of the bores include openings which allow the spaces to communicate with the exterior of the body only when the threaded closures are partially unthreaded.

The dispensing of condiments, such as salt and pepper, has long been commonplace. However, most such dispensers will dispense only a single material, that material has minimal protection from the environment, and the material will spill out if the dispenser is tossed about. As a result the ordinary dispenser is poorly adapted to be taken on camping trips where humid atmospheres are frequently encountered and where the dispenser is often inverted and shaken unintentionally.
Moreover, only a single material is dispensed when the dispenser is used, so a plurality of dispensers must be carried when plural materials are to be dispensed, and the fewer items taken on a camping trip the better. Also, the outlet openings are a fixed aspect of a dispenser, and these are either all open or all closed at any given moment and there is no way to adjust the number of these openings in use at any time. There is thus little opportunity to adjust the amount of material which is dispensed with a single shake of the dispenser.
Other aspects of this invention will become apparent from the description which follows.

Dispenser having shreaded bores for dispensing particulate material


The disclosure relates to a power supply module. The power supply module may include a flexible substrate and a plurality of battery cells distributed in an array on one side of the flexible substrate. Adjacent battery cells of the plurality of battery cells on each line in a first direction may be connected in series by a flexible connector to form a plurality of lines of battery cells, and the plurality of lines of battery cells may be connected in parallel through a first electrode.

A flexible screen is one which is bendable. However, the rigid nature of the motherboard and battery limits the flexing of the flexible screen on the display device, which can only be bent in the edge region. In addition, the thin and light features of the flexible screen cannot be fully obtained.

Power supply module, flexible display panel and display apparatus

CHENGDU BOE OPTOELECTRONICS TECHNOLOGY CO., LTD.


Provided herein are systems, devices, and methods for sample collection. A sample collection device may comprise a vessel, a lid, and pre-loaded liquid solutions. The sample collection device may collect a liquid sample, such as a biological sample. The liquid solutions may comprise reagents for preserving and/or stabilizing biological samples, such as saliva, collected in the vessel. A chamber comprising the liquid solutions may be located in the vessel and/or the lid. In some instances, the liquid solution may be released from the chamber upon closure of the vessel with the lid. In some instances, the liquid solution may be released from the chamber upon actuation of an implement, such as a plunger. In some instances, the liquid solution may be released upon compression of an absorbent member. The sample collecting device may be delivered to a remote location for further processing and/or analysis.

Bodily fluids, such as saliva, sweat, urine, and blood, can be collected from a subject and analyzed to determine information contained in such samples of bodily fluids. For example, a sample may contain information pertaining to the subject. The sample may contain information pertaining to the environment inhabited by the subject. In some instances, the samples may comprise deoxyribonucleic acid (DNA) molecules that can be further processed and/or analyzed to determine genetic information about the subject.
Saliva is a bodily fluid generally secreted by the major salivary glands, such as the parotid, submandibular, and sublingual glands. Saliva may be collected non-invasively, such as by expelling directly from the mouth or inserting a collector, such as a swab, in the mouth to collect.

Systems, devices, and methods for sample collection


A static charge neutralizer for a moving component of an apparatus includes a plurality of filaments on a conductive strip, with tips of the filaments disposed adjacent but spaced from the moving component. The filaments induce ionization in the presence of an electrical field from the statically charged surface of the moving component.

It is known to use non-conductive bearings or sleeves in conveyor rollers and other rollers in various process equipment to provide non-corrosive assemblies and to reduce costs for such equipment. A non-conductive bearing is known to be composed of nylon, polyurethane or other synthetics for durability and anti-corrosion properties. Such non-metallic bearings do not require grease or other lubrication and are often preferred for machinery used in food processing equipment, medical supplies production facilities and other installations that require protection from contamination.
A disadvantage from the use of such non-conductive bearings on rollers and shafts is that static charges are generated and stored in the roller or shaft, particularly under high speed operating conditions. The static charges result from the separation of two sliding surfaces that are not conductive and are isolated. Although it is common to form the shaft of metal, a metal shaft will store static charges if the shaft is isolated by non-conductive bearings. When the charge level of the shaft reaches a critical limit, a spark can occur, arcing to conductive components that are nearby. It is known in such installations that the static charge may reach twenty thousand volts, and can destroy critical electronic components near the conveyer roller or shaft, and may shock personnel in close proximity thereto.
Another common occurrence of shaft-induced current is experienced with three-phase motors utilizing variable speed control devices. Static charges can accumulate to a level that overcomes air insulation, approximately 3,000 volts/mm between the shaft and bearing races. An instantaneous burst of electrical energy can occur, draining the high level current to ground. Arcing creates potential danger to persons nearby and can cause damage to nearby components, including sputtering of metal from the bearing races at the point of current flow, thus damaging the bearing.
It is known to provide conductive grounding brushes in contact with a roller or shaft that becomes charged during operation. The brush is electrically grounded, providing a path to ground for a static charge that would other wise build in the roller or shaft. A disadvantage of the use of such discharge brushes is the difficulty of ensuring contact of the fixed position brush with the moving surface of a rotating roller or shaft. The sliding contact between the brush and the rotating shaft or roller also causes significant and relatively rapid wear of the brush, which can generate dust or liberate fibers from the brush. Contamination from such dust or fibers can be detrimental to the process in which the roller or shaft operates.
In electric motors, it is known to use spring-loaded copper brushes to provide a substantially continuous flow of current to ground. While copper brushes work well to control the build-up of static charges, the copper brushes wear out quite rapidly and require frequent service and/or replacement. Copper brushes can allow a burst of energy on power-up because of metal-to-metal contact design.
What is needed in the art is a static neutralizing device for conveyor rolls, motor shafts and the like, that can be used easily to dissipate static charges effectively, and which eliminates intimate contact between the device and the roller or shaft to minimize wear and the need for service or replacement.

Static charge neutralizing assembly for use on rollers and shafts


Provided are an image processing device, an imaging device, a program, and an image processing method which can suppress a reduction in the visibility of a split image when distortion is corrected. A first display image which is used as a live view image and a second display image which is used to check a focus are generated on the basis of an image signal output from an imaging element including first and second pixel groups on which an object image that passes through first and second regions of an imaging lens and is pupil-divided is formed (S403, S415). The distortion of the first display image is corrected (S403, S411). The distortion of the second display image in a division direction is corrected and distortion in a direction orthogonal to the division direction is not corrected (S409, S417).

1. Field of the Invention
The present invention relates to an image processing device, an imaging device, a program, and an image processing method, and more particularly, to an image processing device, an imaging device, a non-transitory recording medium storing a program, and an image processing method which generate an image for checking the focus state of an object image and display the image.
2. Description of the Related Art
In recent years, a technique has been used which displays a split image in a live view image (so-called through image) in order to facilitate a manual focus adjustment operation in an imaging device, such as a digital camera or a mobile phone with a camera. The split image is an image obtained by combining a portion of a left eye image and a portion of a right eye image corresponding to a predetermined region of an object image. In the split image, the deviation between the left eye image and the right eye image occurs in a direction in which parallax occurs according to a focus state. This technique makes it possible for the user to check the deviation between the left eye image and the right eye image in the split image and to check the focus state.
As a technique related to the above, JP2009-147665A discloses an imaging device which generates a split image using signals obtained from pupil-divided imaging pixels. When displaying the split image, the imaging device adds the color information of signals obtained from the imaging pixels which are not pupil-divided to a left eye image and a right eye image and displays a chromatic split image.
Distortion caused by an imaging lens occurs in an object image which is formed on an imaging element through the imaging lens. Therefore, in the imaging device according to the related art, a process for correcting the distortion is performed.
However, when the distortion correction process is performed on a signal obtained from a normal imaging pixel, the accuracy of detecting a focus is reduced in automatic focus control.
JP2010-191390A discloses an imaging device which suppresses a reduction in the accuracy of detecting a focus in automatic focus control even when the distortion is corrected. The imaging device separately performs the distortion correction process on a signal obtained from a normal imaging pixel and a signal obtained from a pixel for automatic focus control to suppress a reduction in the accuracy of detecting the focus.

Image processing device, imaging device, program, and image processing method suppressing a reduction in visibility of an image to check focus when distortion is corrected


A rigid midsole structure for footwear extends from the metatarsal area to a rear-most portion proximate the heel of a wearer. The rigid midsole accepts any form of replaceable undercarriage structure, and includes means for attaching the undercarriage structure to the bottom side of the rigid midsole. The rigid midsole is preferably formed with an upper surface configured to conform with the bottom of a wearer's foot to provide sufficient rigidity and comfort.

The invention relates to a rigid midsole structure for footwear, such as shoes and boots. In particular, the rigid midsole structure is incorporated into footwear and is sufficiently rigid to provide an adequate, comfortable and total support for a wearer's foot. The rigid midsole extends from the general metatarsal area of a wearer's foot to the rearmost portion of the footwear. The rigid midsole is constructed to accept any form of undercarriage structure, and will include means for attaching any undercarriage structure.
Presently, footwear does not include a rigid midsole extending from the metatarsal area of a wearer to the rearmost portion of footwear and extending across the width of the foot, and thus existing footwear have some degree of flexibility. At most, known footwear have included stabilizers that merely extend over a portion of the width and only a portion of the length of footwear. This type of structure does not support the entire wearer's foot from the metatarsal area to the rear portion of the foot, and has been found to be uncomfortable due to its limited support of the foot.

Rigid midsole footware structure with removable undercarriage attaching means


Disclosed herein is a magnetostatic wave device that employs a single-crystal thin film of the formula Y.sub.3-x M.sub.x Fe.sub.5-y N.sub.Y O.sub.12 (where M denotes at least one member selected from La, Bi, Lu, and Gd, N denotes at least one member selected from Al, In, and Sc, and x and y are defined as 0<x.ltoreq.1.0 and 0<y.ltoreq.1.5, respectively) which is formed by liquid phase epitaxy on a single-crystal substrate of Gd.sub.3 Ga.sub.5 O.sub.12, characterized in that said single-crystal thin film has a lattice constant larger than that of said single-crystal substrate, with the difference (.increment.a) between the two lattice constants being in the range defined by 0.0004 nm.ltoreq..increment.a.ltoreq.0.001 nm. It has good characteristic properties (e.g., low insertion loss and ripple).

1. Field of the Invention
The present invention relates to a magnetostatic wave device which employs a magnetic garnet single-crystal thin film.
2. Description of the Prior Art
Among magnetic materials used for bubble memory and optical isolator is a single-crystal thin film of magnetic garnet which is grown on a substrate of single-crystal garnet by liquid phase epitaxy.
Magnetostatic wave devices employ a spherical magnetic garnet, which is conventionally produced by spherically grinding with high accuracy a single-crystal magnetic garnet (bulk) obtained by the flux technique or floating-zone technique. The spherical grinding has been a bottleneck in mass production.
A recent approach to this situation is to make magnetostatic wave devices from a magnetic garget single-crystal thin film grown on a garnet single-crystal substrate by liquid phase epitaxy. The advantage of liquid phase epitaxy is an ability to give a magnetic garnet single-crystal thin film of high quality which does not need spherical grinding or precision grinding for the fabrication of the magnetic garnet single-crystal bulk into a sphere. The consequence is a simplification of the device structure.
One of the magnetic properties of magnetic garnet single-crystal thin film is saturation magnetization (Is), which is associated with the working frequency of a magnetostatic wave device. Therefore, it is common practice to reduce saturation magnetization for low working frequencies. This is usually accomplished by substituting non-magnetic ions (such as Ga.sup.3+ and Al.sup.3+) for part of the Fe.sup.3+ in Y.sub.3 Fe.sub.5 O.sub.12 (which is a typical magnetic garnet). The result of substitution is an increased mismatching of lattice constant between the garnet single-crystal substrate and the magnetic garnet single-crystal thin film grown thereon. This mismatching is due to the difference in their ionic radii. To preserve the crystallographic quality, it is common practice to substitute La.sup.3+ or Bi.sup.3+ for part of Y.sup.3+ in Y.sub.3 Fe.sub.5 O.sub.12 and Sc.sup.3+ for part of Fe.sup.3+ in Y.sub.3 Fe.sub.5 O.sub.12.
The magnetostatic wave device with a conventional magnetic garnet single-crystal thin film formed by liquid phase epitaxy is poor in characteristic properties because of its high insertion loss and its tendency to cause ripples.


A circuit for determining an initial winding combination for motor startup of a polyphase dc motor having a transistor driver circuit comprising a plurality of high side winding drivers and low side winding drivers operably connected to first and second voltage sources comprises a current mirror circuit and a plurality of sense FETs each operably connected between one of the voltage sources and the gate of one of the winding driver transistors in each phase combination. The sense FETs are operably connected to one side of the current mirror circuit. The mirror circuit compares the current through the sense FET with a current threshold provided on the other side of the current mirror and produces an output signal when the threshold is reached. At the same time, the time to reach the threshold is measured and the phase combination having the longest time is stored. Also when the threshold is reached, the sequencer advances to the next phase combination for measurement until all phase combination have been sequenced. The motor is then started with the phase combination having the longest time measurement energized first.

1. Field of the Invention
This invention relates generally to the field of polyphase DC motor control circuits, and more particularly to a circuit and method for determining the phase winding combination to energize in a motor such as a disk drive motor prior to startup of the motor.
2. Description of the Related Art
Polyphase dc motors are widely used in fixed disk drive applications in personal computers. Typically, such a drive utilizes a magnetic medium on a flat circular disk to store binary data on the disk. The disk is spun by the polyphase dc motor, commonly called a spindle motor, at a relatively constant speed. One or more magnetic heads supported on an actuator arm are selectively moved radially inwardly or outwardly over the surface of the spinning disk by an actuator voice coil motor to read and write data from and to selective locations on the disk. When power is removed from the spindle motor, for example, on power off of the personal computer or on a power failure, routines are automatically implemented to physically move the heads to a predetermined parked position on or off of a landing zone adjacent the data portion of the disk surface, and the rotation of the disks is stopped. When the drive is off, the position of the actuator arm and heads is thus known.
When power is again restored or the PC is turned on again, the disk drive spindle motor starts. It is desirable that the power consumed and time duration of disk drive startup be minimized. This may be desirable for several reasons, the predominant ones of which are that the user cannot access the drive until the disk is running at constant speed and power consumption should be minimized. However, in order to efficiently start the polyphase dc motor, the correct starting point, i.e. phase combination, for the sequence of winding energizations must be determined. This is typically done by passing a small current sequentially through each of the winding combinations in a predetermined sequence and measuring time it takes for the voltage developed across a common sensing resistor in series with each of the winding combinations to reach a predetermined value. A comparator is then used to determine which winding combination takes the longest time to reach the predetermined voltage value and thus senses the winding combination having the highest reluctance from intersecting the magnetic field generated by the stationary permanent magnet pole pieces of the rotor. Passing drive current through this particular winding combination will provide the most starting torque and therefore will be the optimum combination that should be first energized on motor startup.
Typical disk drive spin motor control systems and circuits are described in U.S. Pat. Nos. 5,294,877, 5,317,243, and 5,866,998, which are hereby incorporated herein by reference in their entirety. Hard disk drive spin motors are typically three phase dc motors which have three sets of stator windings, A, B, and C having sets of series coils connected in a Y configuration. The rotor is typically a four pole device. Electrical current is fed through two legs of the "Y" with the third leg left floating in a series of repetitive combinations to cause the rotor to rotate. A sequencer controls a power stage of transistor switches to connect the windings to the voltage sources in the proper order. The six combinations of winding connections are thus AH,BL; AH,CL; BH,CL; BH,AL; CH,AL; and CH,BL; where A, B, C, indicates the winding leg and the "H" and "L" indicates the high side driver transistor, typically a field effect transistor (FET) switch being turned on and the low side driver FET being turned on.
Voltage developed across an external sensing resistor is typically utilized to determine which winding combination to energize first on motor startup. This sensing resistor is typically in series with the low side driver FET. In order to accurately determine which winding combination for the sequencer to use, this resistor must be highly accurate and dependable. Consequently, the cost of this high precision, high reliability sense resistor is rather high. In addition, the sense resistor is typically separate and distinct from the driver IC chip. A separate comparator circuit is also required for implementing the voltage comparison. This conventional configuration is relatively expensive. Therefore there is a need for a more economical approach to sensing the position of the rotor for startup of polyphase dc motors. In addition, there is a need for a circuit which eliminates the need for a precision resistor and eliminates the need for a comparator circuit without loss of reliability and accuracy.

Circuit and method for determining optimal phase combination for startup of a polyphase DC motor


Systems and methods for data collection and processing. A system includes a forms processing subsystem including a form designer and a form processing and workflow module, and a client subsystem including a form submission manager and a client data store. User provided information is maintained locally in the client data store.

1. Field of Invention
The present invention relates to the field of data processing and, more specifically, to data processing methods and systems for creating and populating forms.
2. Description of Related Art
The use of standardized HTML forms to collect and capture data has proven to be a useful way to organize and collect information. The use of such forms is commonplace today. The widespread availability of computers has led to the development of automated forms processing methods and systems that provide increased efficiency, reliability, and data persistence. In particular, existing automated forms processing methods and systems make possible the collection and retention of vast amount of information. Such information may include personal or confidential information. Government agencies, in particular, collect large amounts of such information using standardized forms.
Various organizations have developed their own unique or proprietary forms based on the information needed to be collected by the organization. For example, the Internal Revenue Service collects taxpayer information using a Form 1040 as well as many other related forms. Within a given organization, as well as among organizations, the information to be collected may include much of the same information such as, for example, a person's first and last names. Despite the similarities of the information collected using different forms of the same organization or of other organizations, existing systems and methods do not allow for fast and efficient reuse of information already collected when the same or similar information has to be subsequently collected from a user.
Furthermore, in existing data processing systems having a client-server architecture, the data processing and maintenance functions tend to be concentrated on the server side. This approach can lead to service delays to client users, because the client user has to wait for a response from the server, thereby impacting system response time from the client's perspective. In addition, existing systems require the server side to provide storage capacity for vast amounts of collected information. The cost required to provide and maintain this capacity involves a substantial and ongoing outlay of time, money, and technical resources. Furthermore, concentrated personal or company information at the server side leaves the information more vulnerable to a single security attack, giving rise to privacy concerns for massive amounts of personal information. Still further, existing systems and methods require large amounts of program data to be downloaded from a server to a client in order for a client user to be able to enter data into form templates.
Thus, there is a need for systems and methods to address these limitations as well as others readily discernable from review of this disclosure.

Data collection and processing system and methods


A laser scanner comprising a distance measuring light projecting unit for emitting at least two distance measuring lights at a known deflection angle with respect to a projecting optical axis, a distance measuring unit for receiving at least two reflected distance measuring lights and performing a distance measurement, respectively, an optical axis deflector for deflecting optical axes of the distance measuring lights and the reflected distance measuring lights at the same deflection angle in the same direction, a projecting direction detecting module for deflecting a deflection angle and a deflecting direction by the optical axis deflector, and an arithmetic control module, wherein the arithmetic control module performs a two-dimensional scanning with the distance measuring lights, draws at least two loci on a plane to be measured, and measures the plane to be measured along at least the two loci substantially at the same time by the distance measuring unit.

The present invention relates to a laser scanner and a surveying system for acquiring three-dimensional point cloud data of a plane to be measured.
For example, in a case where a topography of a plane to be measured such as a ground or the like is measured, a laser scanner is mounted on a moving body such as an unmanned aerial vehicle or the like, the plane to be measured is scanned by the laser scanner, three-dimensional point cloud data is acquired, and the topography of the plane to be measured is measured.
However, the laser scanner mounted on the moving body is usually a one-dimensional laser scanner. Therefore, in order to scan the plane to be measured by the laser scanner and acquire accurate three-dimensional point cloud data, the moving body must move at a constant speed, and a means for measuring an attitude of the laser scanner such as a tilt and the like need to be additionally provided.
Therefore, a control of a moving speed of the moving body and a device configuration of the laser scanner mounted on the moving body become complicated, and the device itself becomes expensive.


Database system query optimizers use several techniques such as histograms and sampling to estimate the result sizes of operators and sub-plans (operator trees) and the number of distinct values in their outputs. Instead of estimates, the invention uses the exact actual values of the result sizes and the number of distinct values in the outputs of sub-plans encountered by the optimizer. This is achieved by optimizing the query in phases. In each phase, newly encountered sub-plans are recorded for which result size and/or distinct value estimates are required. These sub-plans are executed at the end of the phase to determine their actual result sizes and the actual number of distinct values in their outputs. In subsequent phases, the optimizer uses these actual values when it encounters the same sub-plan again.

In database systems, a query optimizer determines the execution plans of queries. For any given query, the query optimizer chooses the plan with the lowest estimated cost. To estimate the cost of a plan, the optimizer uses knowledge of the result sizes of the operators comprising the plan. The optimizer also uses knowledge of the number of distinct values in the output of these operators. More accurate knowledge of these two quantities results in more accurate cost estimates, and hence a better choice of query execution plan.
The result size of an operator and the number of distinct values in its output depend on the data distribution of the query. To estimate these two quantities, database systems use various techniques to approximate input data distributions, such as histograms or sampling. The estimated values provided by these techniques, no matter how accurate, are only approximations that invariably deviate from the true values to some extent. Since query optimizer cost models are highly sensitive to result size and distinct value estimates, the errors in estimating these quantities lead to errors in estimating plan costs. Estimation errors increase as they propagate through the large query execution plans. For table joins, which are used in almost all database queries, the estimation error can be exponential in the number of joins. These errors can ultimately cause the optimizer to choose a sub-optimal plan. However, the plans chosen using these techniques, while not necessarily optimal, are usually "good enough." These techniques are used because they quickly provide the required estimates. Query optimization, including all the necessary estimation steps, must not take more than a very small fraction of the time to execute the query. Query optimizers therefore use these fast but possibly inaccurate estimation techniques since the performance of the chosen plans is typically acceptable for many applications.
This reasoning assumes that the database system mostly handles ad hoc queries—queries for which optimization must be fast and for which sub-optimal plans are acceptable. This is not true for queries embedded in applications, which comprise a large portion of the workloads handled by modern database systems. These queries can be (and often are) optimized off-line to produce a compiled version of the query that is then used whenever the query is executed. Such optimizations do not necessarily have to be fast since they are off-line processes. Furthermore, these queries are typically executed frequently since they are part of the application. Thus, the cost of optimization is amortized over many executions of the query. Moreover, finding the optimal execution plan in this setting is more important than for ad hoc queries, because the repeated execution of the queries will increase the effect of any savings in execution time. For these embedded queries, the user may be willing to spend more time optimizing the query and obtaining more accurate cost estimates if this results in choosing a faster execution plan.
Several techniques for estimating result sizes have been proposed in the literature. All these techniques deal with estimating the result size of a single selection or join operator. Some of these techniques can also be extended to estimating the number of distinct values in the output of these operators.
One technique for estimating result sizes is to sample the data at query optimization time. One disadvantage of this approach is the overhead it adds to query optimization. Furthermore, sampling cannot be used to accurately estimate the number of distinct values of an attribute. Sampling is more useful for other applications such as building histograms or approximate query processing.
A second technique for estimating result sizes is using histograms. Histograms are now used by most commercial database systems for result size estimation. Although one-dimensional equi-depth histograms are used in most systems, more accurate histograms have been proposed for use with single and multiple dimensions. A novel approach for building histograms based on wavelets is presented in a paper by Y. Matias, J. S. Vitter, and M. Wang entitled "Wavelet-based Histograms for Selectivity Estimation" in Proceedings of the ACM SIGMOD Conference, pages 448-459, 1998. Histograms, by their very nature, only capture an approximation of the data distribution, and incur varying degrees of estimation errors.
A third technique for estimating result sizes is using feedback from the query execution engine. This approach eliminates the overhead of histogram construction and maintenance, so it is potentially less expensive than traditional histograms. However, it is still an approximate technique with significant estimation errors.
The importance of estimating the result size of joins is discussed in the literature as early as 1986. See L. F. Mackert and G. M. Lohman, "R* Optimizer Validation and Performance Evaluation for Local Queries" in Proceedings of the ACM SIGMOD Conference, pages 84-95, 1986. In this paper, it is noted that the cost model used by the R* System query optimizer for nested loop joins is very sensitive to the estimated result size of the join. Inaccurate result size estimation can lead to sub-optimal plans being chosen. This conclusion demonstrates the usefulness of our approach.

Query optimization by sub-plan memoization


An x-ray optical system for producing high intensity x-ray beams. The system includes an optic with a surface formed by revolving a defined contour around a revolving axis that is different than the geometric symmetric axis of the optic. Accordingly, the system may use a source that has a circular emission profile or a large source to provide increased flux to a sample.

The present invention relates to x-ray optical systems.
Researchers have long employed focusing x-ray optics in x-ray diffraction experiments to increase the flux incident on a sample and to thereby increase the signal to noise ratio. A focusing optic increases the flux through a sample by directing a large number of photons from a source. Moreover, by positioning a detector near or at the focus of the optic, resolution of the system can be greatly improved.
The intensity of conventional x-ray beam systems, however, is limited by the brilliance of the source that can be achieved without damaging the source target. Although a large optic, such as an ellipsoidal optic or a parabolic optic with a large capture angle, can deliver high flux, the cross section of the x-ray beam and divergence tends to be too large to be fully utilized. Improving the performance of an x-ray beam system by increasing the brilliance of the source is typically limited or too costly.
In view of the above there is a need for an improved x-ray optical system that produces high-intensity x-ray beams.