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High throughput mechanical alloying and screeningRelated Patent Categories: Chemical Apparatus And Process Disinfecting, Deodorizing, Preserving, Or Sterilizing, Analyzer, Structured Indicator, Or Manipulative Laboratory Device, Miscellaneous Laboratory Apparatus And Elements, Per Se, ContainerHigh throughput mechanical alloying and screening description/claimsThe Patent Description & Claims data below is from USPTO Patent Application 20070178019, High throughput mechanical alloying and screening. Brief Patent Description - Full Patent Description - Patent Application Claims CROSS-REFERENCE TO RELATED APPLICATIONS [0001] This application is a continuation-in-part of U.S. application Ser. No. 11/197,180, filed Aug. 3, 2005, and claims priority to international patent application no. PCT/US2006/030257, filed Aug. 2, 2006, both of which applications are incorporated herein by reference for all purposes. BACKGROUND OF THE INVENTION [0002] 1. Field of the Invention [0003] The present invention relates to an apparatus and methods for simultaneously producing multiple alloys of ultra-fine powder particles, and for high-throughput assaying of the alloys to identify those having desired gas storage properties. [0004] 2. Background [0005] Materials science has shown that materials having a desired property can often be found by making a massive library of different materials from various combinations of precursor substances and assaying the resulting materials for the desired property. [0006] One method that is suitable for making different materials is mechanical alloying, which was invented by J. S. Benjamin and is described in U.S. Pat. No. 3,591,362. Mechanical alloying involves forming alloys from pure starting materials by milling a mixture of the powders in a high energy ball mill. During the milling, the starting particles undergo repeated collisions with grinding balls, causing deformation, welding and fracture of the particles which result in microstructural refinement and composition changes leading to the formation of nanocrystalline or amorphous alloys. The process can result in two or more particulate starting substances becoming so intimately mixed that the resulting particulate product is either a true alloy or a remarkably homogenous blend, or a combination of a true alloy and a homogeneous blend. [0007] Previously known devices and methods for mechanical alloying are not suitable for forming the massive libraries of materials that are necessary for optimal screening to identify materials that have desired properties. Therefore, a need exists for a mechanical alloying apparatus and methods for the production of large libraries of different materials in a high throughput manner. The present invention fulfills this and other needs. SUMMARY OF THE INVENTION [0008] The invention provides a multiwell ball milling fixture that is useful for performing multiple ball milling operations in a high throughput manner. In some embodiments, the fixture can be used not only for the ball milling, but also for further operations such as gas storage assays. The fixture includes a multiwell plate and a lid. The multiwell plate has a plurality of sample wells, wherein each sample well has a sidewall and a bottom surface. Generally, the bottom surface is joined to the sidewall by a rounded surface. The lid has a bottom surface that defines a planar expanse sufficient to cover the sample wells when the lid is placed on the multiwell plate. The lid has a plurality of gas outlet ports that each include: i) a first opening on the bottom surface of the lid that is spatially positioned such that when the lid is positioned on the multiwell plate, the first opening is in fluid communication with a sample well; ii) a second opening in the top surface of the lid; and iii) a valve that regulates gas flow through the gas outlet port. [0009] The multiwell ball milling fixture typically has one or more seals disposed between the multiwell plate and the lid, which seals allow gas flow between a sample well and an associated gas outlet port but prevent gas flow between sample wells and between a sample well and a non-associated gas outlet port. If a cap is used, the fixture generally has one or more seals disposed between the lid and the cap, which seals prevent gas flow from one gas outlet port to a second gas outlet port associated with a second sample well. When the lid is attached to the multiwell plate and the valve is in a closed position, no gas can flow into or out of the sample wells (i.e., the sample wells are gas-tight or air-tight). [0010] The lids of the multiwell ball milling fixtures can have a plurality of recessed areas on the bottom surface. In some embodiments, the recessed areas have a top surface that is concave relative to the bottom surface of the lid. The recessed areas can, in some embodiments, have a cross-sectional shape that corresponds to the cross-sectional shape of the sample wells. For example, the top surface of the recessed areas can have a concave radius of curvature that is similar to or identical to the radius of the rounded surface that joins the sidewall and the bottom surface of the multiwell plate. The positions of the recessed areas spatially correspond to the positions of the sample wells when the lid is placed on the multiwell plate. In some embodiments, the recessed areas have a diameter that is the same as the diameter of the sample wells. [0011] In some embodiments, the lids of the multiwell ball milling fixtures have a plurality of valves that regulate gas flow through the gas outlet ports. The valves can be operably connected to each other, for example, such that when a first valve is changed from an closed position to an open position, one or more additional valves are also changed from the closed position to the open position. For example, the lid can include one or more spool valves that each includes a plurality of valve elements, wherein movement of the spool valve in a first direction positions the valve elements in the open position and movement of the spool valve in a second direction positions the valve elements in the closed position. The lid can have one spool valve for each row of gas outlet ports, or one spool valve for each column of gas outlet ports, The spool valves can be inserted into a bore that traverses through the lid. [0012] The multiwell ball milling fixtures can, in some embodiments, also have a charging cap. The charging caps have a gas portal and a bottom surface that defines a planar expanse sufficient to cover each of the second openings of the plurality of gas conduits of the lid when the cap is positioned on the lid. The charging cap has an air passage that is in fluid communication with each of the second openings and with the gas portal when the charging cap is placed on the lid. The gas portal is connected to a vacuum source that applies a vacuum to the sample wells when the valves of the lid (if present) are in an open position. The gas portal can also be connected to a milling gas source that introduces a milling gas into the sample wells when the valves of the lid (if present) are in an open position. [0013] The invention also provides multiwell ball milling fixtures that include a multiwell plate and a removable lid, wherein: (a) the multiwell plate has a plurality of sample wells, wherein each sample well comprises a sidewall and a bottom surface, wherein the bottom surface is joined to the sidewall by a rounded surface; and (b) the removable lid has a bottom surface that defines a planar expanse sufficient to cover the sample wells, which lid comprises a plurality of gas outlet ports that are positioned such that two or more of the sample wells are each in unimpeded fluid communication with an associated gas outlet port when the lid is positioned on the multiwell plate; wherein when the lid is attached to the multiwell plate and the gas outlet ports are blocked, no gas can flow into or out of the sample wells. The fixtures can further include one or more seals disposed between the multiwell plate and the lid, which seals allow gas flow between a sample well and an associated gas outlet port but prevent gas flow between sample wells and between a sample well and a non-associated gas outlet port. In some embodiments, the lids have a plurality of recessed areas which have a cross-sectional shape that corresponds to the cross-sectional shape of the sample wells, and the positions of which spatially correspond to the sample wells when the lid is placed on the multiwell plate. [0014] The invention also provides a high throughput ball milling apparatus. This apparatus typically includes: (a) a rotary platform which rotates about a first axis, (b) a plurality of receptacles that are rotatably supported on the rotary platform, wherein each receptacle rotates about an axis that is substantially parallel to the first axis and is configured to hold at least one multiwell ball milling fixture; and (c) a motor in drive relation to the rotary platform that provides rotational forces thereto. Each receptacle can hold at least one multiwell ball milling fixtures, and in many embodiments can hold two or more plates. The apparatus also has a motor or other means for driving rotation of the receptacles. The rotating platform and the receptacles can rotate at the same speed, or at different speeds. The apparatus can have one motor that provides rotational force to both the receptacles and to the rotary platform, or can have two different motors. [0015] Also provided by the invention are gas storage assay caps for a multiwell plate. The assay cap has a bottom surface and a top surface and includes: (a) a plurality of gas outlet ports that each have a first opening on the bottom surface and a second opening in a second surface of the cap, wherein the first openings of the gas outlet ports are spatially arranged such that each gas outlet port is in fluid communication with a sample well of a multiwell plate when the assay cap is positioned either (i) on a multiwell plate, or (ii) on a lid for a multiwell plate, which lid comprises a plurality of gas outlet ports that are in fluid communication with a sample well of a multiwell plate when the lid is positioned on a multiwell plate; and (b) a pressure sensor in fluid communication with the second opening of each of at least one of the gas outlet ports. Typically, each of the gas outlet ports is in fluid communication with a pressure sensor. [0016] In some embodiments, gas storage assay cap is attached to a multiwell plate lid that has a bottom surface and a top surface and defines a planar expanse sufficient to cover sample wells of a multiwell plate. The lid has a plurality of gas outlet ports that each have a first opening on the bottom surface of the lid and a second opening in the top surface of the lid, wherein the first openings of the gas outlet ports are spatially arranged such that each gas outlet port is in fluid communication with a sample well of a multiwell plate when the assay cap is positioned on a multiwell plate, and the second openings are spatially arranged such that each gas outlet port in the lid is in fluid communication with a conduit in the assay cap. In some embodiments, the first opening of a gas outlet port in the multiwell plate lid is positioned in a recessed area that spatially corresponds to the sample wells when the lid is placed on a multiwell plate. The second openings of the gas outlet ports are in fluid communication with (a) a gas source, and (b) a vacuum source. [0017] The invention also provides a high throughput gas storage assay device. These devices include: (a) a multiwell plate that has a plurality of sample wells; (b) a lid defining a planar expanse sufficient to cover the sample wells, which lid has a plurality of gas outlet ports, wherein the gas outlet ports are positioned such that two or more of the sample wells are each in fluid communication with an associated gas outlet port when the lid is positioned on the multiwell plate; and (c) a gas storage assay cap that comprises a top surface and a bottom surface that defines a planar expanse sufficient to cover the gas outlet ports of the multiwell plate lid when the assay cap is positioned on the lid, wherein the assay cap comprises a plurality of gas conduits that are positioned such that at least one conduit in the cap is in fluid communication an associated gas outlet port in the multiwell plate lid. [0018] In some embodiments, the gas storage assay device has a pressure sensor in fluid communication with each of the gas conduits. The device also can have a vacuum source and a test gas source, both of which are in fluid communication with the gas conduits of the assay cap. One or more valves that regulate gas flow between the conduits and the vacuum source, and one or more valves that regulate gas flow between the gas conduits and the test gas source can also be included in the gas storage assay device. A single valve can be used for switching between the test gas source, the vacuum source, and the pressure sensor being in fluid communication with the gas conduit. [0019] The gas storage assay device can also include a controller that comprises logic instructions that direct the device to perform a method that comprises the following steps: [0020] (a) open a valve between the vacuum source and the gas conduit, thereby applying a vacuum to a sample well; [0021] (b) close the valve between the vacuum source and the gas conduit; Continue reading about High throughput mechanical alloying and screening... 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