JP2011524249A - High-pressure apparatus and crystal growth method for nitride crystal growth - Google Patents

Abstract

A high pressure apparatus and associated method for processing a supercritical fluid is provided. The apparatus includes a capsule, a heater, and at least one ceramic ring, but may be a plurality of rings, optionally having one or more scribe marks and / or cracks. To do. The apparatus optionally has a metal sleeve that includes each ceramic ring. In addition, the apparatus includes a high strength enclosure, an end flange with associated thermal insulation, and a power control system. The device can be at a pressure of 0.2-2 GPa and a temperature of 400-1200 ° C.
[Selection] Figure 3

Description

Cross-reference of related applications

  This application is commonly assigned U.S. patent application Ser. No. 12 / 133,364 filed Jun. 5, 2008, Attorney Docket No. 027364-000300 US, and Jun. 18, 2008. Claims priority to filed US Provisional Patent Application No. 61 / 073,687, Attorney Docket No. 027364-001100US. Both of these specifications are hereby incorporated by reference for all purposes.

Background of the Invention

  The present invention generally relates to a method for treating a material with a supercritical fluid. More specifically, embodiments of the present invention include a method for controlling parameters associated with a material processing capsule disposed within an enclosure of a high pressure device. By way of example only, the present invention can be applied to grow GaN, AlN, InN, InGaN, AlGaN, and AlInGaN crystals, as well as other materials, to produce bulk or patterned substrates. be able to. Such bulk substrates or patterned substrates include devices such as optoelectronic devices, lasers, light emitting diodes, solar cells, photoelectrochemical water splitting and hydrogen generating units, photodetectors, integrated circuits, and transistors. It can be used for various purposes.

  Supercritical fluids are used to process a variety of materials. A supercritical fluid is usually defined as a substance that exceeds its critical point, i.e., critical temperature and critical pressure. The critical point means the maximum temperature and pressure at which a substance can exist stably as a vapor and liquid. In some supercritical fluid applications, the material to be processed is placed inside a pressure vessel or other high pressure device. In some instances, it may be desirable to first place the materials inside a container, liner, or capsule, and then place them inside a high pressure device. The high pressure device has a structure that supports the high pressure generated in the container or capsule holding the material during operation. The container, liner, or capsule has a closed / sealed environment that is chemically inert and impervious to solvents, solutes, and gases contained in or generated by the process. is doing.

  Scientists and engineers have synthesized crystalline materials using high pressure techniques. As an example, synthetic diamond is frequently produced using high pressure and temperature conditions. Synthetic diamonds are frequently used for industrial purposes, but can also be grown large enough for jewelry and other applications. In addition, scientists and engineers can use high pressure to synthesize complex materials such as zeolites and use these materials to filter toxins and the like. In addition, geologists have used high pressure techniques to simulate conditions and / or processes occurring deep in the earth's crust. High pressure technology often relies on a supercritical fluid (referred to herein as SCF).

  Supercritical fluids provide a particularly ideal environment for growing high quality crystals in large quantities and at low cost. In many cases, supercritical fluids have the ability to solvate liquids with gas transport properties. Therefore, on the other hand, the supercritical fluid can dissolve a large amount of recrystallization solute. On the other hand, it has a high diffusion coefficient suitable for transport properties, so it is possible to quickly transport solutes through the boundary layer between the bulk of the supercritical fluid and the growing crystal, and even lower viscosity. As a result, the boundary layer is very thin and a small temperature gradient can facilitate the self-convection and self-stirring of the reactor. Combining these properties allows, for example, the growth of hundreds or thousands of large α-quartz crystals in a single growth process of supercritical water.

  In addition, supercritical fluids are a medium for extracting solvents, for example for extracting caffeine from coffee, for synthesizing novel materials such as zeolites, and relatively inert under general conditions. Resulting in an attractive medium for decomposing and / or dissolving biofuels and toxic waste.

  Further, in some applications, such as crystal growth, the pressure vessel or capsule includes a baffle plate that divides the interior into different chambers, for example, an upper half and a lower half. Typical baffle plates have spaced holes arranged at irregular or regular intervals to allow fluid flow and heating and mass transfer between these different chambers, and the different chambers Holds different materials that are processed with a supercritical fluid. For example, in a typical crystal growth application, one part of the capsule contains seed crystals and the other half contains nutrient material. In addition to the material to be treated, the capsules are intended to improve the solubility of the solid or liquid that forms the supercritical fluid at elevated temperatures and pressures, generally further the material to be treated with the supercritical fluid. Contains mineralizer. The baffle plate may not be used to operate in other applications, such as zeolite or nanoparticle synthesis or ceramic processing. In operation, the capsule is heated and pressurized towards or beyond the critical point, thereby turning the solid and / or liquid into a supercritical fluid. In some applications, the fluid may remain subcritical, i.e. the pressure or temperature may be below the critical point. However, in all cases covered here, the fluid is superheated, i.e. the temperature is higher than the boiling point of the fluid at atmospheric pressure. The term “supercritical” shall be used throughout in the sense of “superheated” regardless of whether the pressure and temperature are above the critical point. Note that it may not be recognized as suitable for a specific fluid composition having a dissolved solute.

  Although effective to some extent for conventional crystal growth, conventional processing vessels have drawbacks. As an example, the throughput of conventional steel hot wall pressure vessels (eg, autoclaves) is generally limited to a maximum temperature of about 400 degrees Celsius and a maximum pressure of 0.2 gigapascal (GPa). Manufacturing a conventional pressure vessel from a nickel-based superalloy allows operation at a maximum temperature of about 550 degrees Celsius and a maximum pressure of about 0.5 GPa. Thus, these conventional hot wall pressure vessels are often inadequate for some processes such as the growth of gallium nitride crystals in supercritical ammonia. The supercritical ammonia often requires a much higher range of pressures and temperatures than this range in order to achieve growth rates higher than about 2-4 microns per hour. Furthermore, nickel-based superalloys are very expensive and difficult to process, limiting the practical maximum size and significantly increasing costs compared to conventional steel pressure vessels.

  Attempts have been made to overcome the disadvantages of conventional pressure vessels. D'Evelyn et al., US Patent Application No. 2003 / 0140845A1, is a so-called zero stroke high pressure adapted to the type of belt device used to synthesize diamond using high pressure and high temperature. An apparatus is described. Sintered tungsten carbide is used as a mold material, but it is quite expensive and large in size but difficult to manufacture. In addition, the use of a hydraulic press to house the device increases costs and further limits the maximum volume. Finally, the use of a pressure transfer medium surrounding the capsule used to contain the supercritical fluid reduces the volume available in the hot zone for processing the material.

  U.S. Patent Application No. 2006/0177362 A1 to D'Evelyn et al. Has the ability to handle pressures and temperatures well beyond those of conventional autoclaves and is improved with respect to the zero stroke press apparatus described above. Multiple types of devices with high scalability are described. To reduce both the pressure and temperature to which the inner diameter of the high-strength enclosure is exposed compared to the corresponding value of the capsule, a series of wedge-shaped radial ceramic segments are connected between the heater surrounding the capsule and the high-strength enclosure. Arranged between. However, the production and use of these wedge-shaped radial ceramic segments can be difficult and expensive. These and other limitations of conventional devices are described throughout this specification.

  From the above it can be seen that a method for improving a high pressure apparatus for crystal growth is highly desirable.

Brief summary of the invention

  In accordance with the present invention, a method is provided that relates to processing a material with a supercritical fluid. More specifically, embodiments of the present invention include a method for controlling parameters associated with a material processing capsule disposed within a high pressure apparatus / enclosure. By way of example only, the present invention can be applied to grow GaN, AlN, InN, InGaN, AlGaN, and AlInGaN crystals, as well as other materials, to produce bulk or patterned substrates. . Such bulk substrates or patterned substrates include various devices such as optoelectronic devices, lasers, light emitting diodes, solar cells, photoelectrochemical water splitting and hydrogen generating units, photodetectors, integrated circuits, and transistors. Can be used for

  In certain embodiments, the present invention provides a high pressure apparatus and associated methods for processing supercritical fluids. In certain embodiments, the apparatus includes a capsule, a heater, and at least one ring (eg, made of ceramic), but may be a plurality of rings, optionally including one or more rings. There are scribe marks and / or cracks. In certain embodiments, the apparatus has a metal sleeve that optionally includes each ceramic ring. In addition, the apparatus includes a high strength enclosure, an end flange with associated thermal insulation, and a power control system. The device is scalable to very large volumes and is cost effective. In certain embodiments, the apparatus can be at a pressure of 0.2-2 GPa and a temperature of 400-1200 ° C, respectively. As used in certain embodiments herein, the term “high strength” generally refers to a high pressure enclosure such as a pressure vessel (which may be airtight but may not be airtight and / or gas tight). By means of suitable mechanical and other features that allow its use as a tensile strength, Young's modulus, yield strength, toughness, creep resistance, chemical resistance, etc. As an example, the term “high pressure” generally refers to pressures greater than 0.1 GPa, 0.2 GPa, 0.5 GPa, and other pressures, particularly GaN, AlN, InN, AlGaN, InGaN, AlInGaN, and other By a suitable pressure to grow a crystalline material, including but not limited to nitride or oxide or metal, or a dielectric or semiconductor material. In certain embodiments, a high strength enclosure material is provided to withstand a load greater than about 0.1 GPa (or 0.2 GPa or 0.5 GPa) for a period of time at a temperature below about 200 degrees Celsius. Forms a high strength enclosure that is constructed. Of course, other variations, modifications, and alternatives are possible.

  In certain alternative embodiments, the present invention provides an apparatus for high pressure crystal or material processing, eg, GaN, AlN, InN, InGaN, AlGaN, and AlInGaN. The apparatus includes a capsule region (eg, for a capsule) having a first region and a second region and a length defined therebetween. The apparatus has an annular heating member that surrounds the capsule region. The apparatus comprises at least one (eg, two or more) continuous annular members made of ceramic (or metal or cermet) having a predetermined thickness arranged sequentially and continuously around the annular heating member. Have In a preferred embodiment, the continuous annular member is made from a material having a compressive strength greater than about 0.5 GPa and a thermal conductivity less than about 4 watts per meter Kelvin. In certain embodiments, the two or more irregularly shaped surface regions are spatially disposed within one or more of the annular members and are substantially coupled to one another along a portion of the common boundary region. Pair with. In addition, the apparatus has a high strength enclosure material disposed on a ceramic annular member to form a high strength enclosure.

  Still further, the present invention provides a method of growing crystals of, for example, GaN, AlN, InN, InGaN, AlGaN, and AlInGaN. The method includes providing an apparatus for high pressure crystal growth or material processing. The device includes a capsule region having a first region and a second region and a length defined therebetween (eg, a cylindrical shape). Furthermore, the device has an annular heating member surrounding the capsule region. The apparatus has at least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness continuously arranged around the annular heating member. In a preferred embodiment, the continuous annular member is made from a material having a compressive strength greater than about 0.5 GPa and a thermal conductivity less than about 4 watts per meter Kelvin. In addition, the apparatus includes a high strength enclosure material disposed on a ceramic annular member. Further, in certain embodiments, the method includes providing a capsule comprising a solvent and placing the capsule within an interior region of the capsule region. In certain embodiments, the method includes treating the capsule with thermal energy to raise the temperature inside the capsule to a temperature greater than 200 degrees Celsius and superheating the solvent.

  Further, depending on the embodiment, the method may include one of a plurality of optional steps. Optionally, the method includes forming the crystalline material from a solvent heat treatment. Further, the method includes removing thermal energy from the capsule to change the temperature of the capsule from a first temperature to a second temperature lower than the first temperature. Further, the method uses the steps of removing the first flange and the second flange from the high pressure device and using the hydraulic driving force to move the mechanical member from the first region of the capsule region toward the second region. And moving the capsule from the capsule region. In a preferred embodiment, the device allows the capsule volume to be expanded to a size greater than 0.3 liters to about 300 liters. Of course, other variations, modifications, and alternatives are possible.

  Still further, the present invention provides a method of forming a crystalline material, such as GaN. The method includes providing an apparatus for high pressure crystal or material processing. The device includes a capsule region having a first region and a second region and a length defined therebetween. Furthermore, the device has an annular heating member surrounding the capsule region. At least one continuous annular member is included. The annular member includes a predetermined thickness that is continuously disposed around the annular heating member. In certain embodiments, the continuous annular member is made of a material having a compressive strength greater than about 0.5 GPa and a thermal conductivity less than about 100 watts per meter Kelvin. In addition, the apparatus has a high strength enclosure material disposed on the annular member to form a high strength enclosure. The method includes providing a capsule containing a solvent and placing the capsule within an interior region of the capsule region. The method includes treating the capsule with thermal energy to raise the capsule to a temperature greater than 200 degrees Celsius and superheating the solvent.

  Advantages over the prior art are realized using the present invention. In particular, the present invention enables a cost effective high pressure apparatus for growing crystals such as GaN, AlN, InN, InGaN, and AlInGaN and others. In certain embodiments, the methods and apparatus of the present invention can work with components that are relatively simple and cost effective to manufacture, such as ceramic tubes and steel tubes. Further, certain embodiments utilize one or more cracks provided in a ceramic member that insulates the heater. Depending on the embodiment, conventional materials and / or methods by those skilled in the art can be used to produce the apparatus and methods of the present invention. The apparatus and method of the present invention, according to a particular embodiment, is greater than 0.3 liters, greater than 1 liter, greater than 3 liters, greater than 10 liters, greater than 10 liters, greater than 30 liters, 100 liters. Allows cost-effective crystal growth and material processing under maximum pressure and temperature conditions in batch volumes greater than and greater than 300 liters. In a preferred embodiment, the apparatus and associated methods of the present invention allow for the selection of dimensions and parameters that are important for expanding larger gallium nitride reactors that have not been realized using the prior art. Depending on the embodiment, one or more of these benefits may be realized. These and other advantages will be described in greater detail throughout the specification.

  The present invention realizes these and other advantages in connection with known processing techniques. Further understanding of the features and advantages of the present invention may be realized by reference to the remaining portions of the specification and the attached drawings.

It is the schematic of the conventional apparatus. 1 is a schematic view of a high pressure apparatus according to an embodiment of the present invention. It is a schematic sectional drawing of the high voltage | pressure apparatus by one Embodiment of this invention. It is a schematic sectional drawing of the high voltage | pressure apparatus by one Embodiment of this invention. FIG. 6 is a schematic cross-sectional view of an alternative high pressure device according to an alternative embodiment of the present invention. 2 is a schematic flowchart of a method of processing a material with a supercritical fluid according to an embodiment of the present invention. 6 is a schematic flowchart of an alternative method of processing a material with a supercritical fluid, according to an alternative embodiment of the present invention.

  The present invention includes a method for treating a material with a supercritical fluid. More specifically, embodiments of the present invention include a method for controlling parameters associated with a material processing capsule disposed within a high pressure apparatus / enclosure. By way of example only, crystals of GaN, AlN, InN, InGaN, AlGaN, and AlInGaN can be grown by applying the present invention to produce a bulk substrate or a patterned substrate. Such bulk or patterned substrates can be used in a variety of applications including optoelectronic devices, lasers, light emitting diodes, solar cells, photoelectrochemical water splitting and hydrogen generating units, photodetectors, integrated circuits, and transistors. Can be used for.

  In certain embodiments, the present invention provides a high pressure apparatus for processing materials. Depending on the embodiment, the apparatus will be described in relation to a specific direction relative to the direction of gravity. As an example, the device is described as being oriented vertically. Instead, in other embodiments, the device is oriented horizontally or at an intermediate oblique angle between vertical and horizontal, and can swing to cause convection of the supercritical fluid within the capsule. Is possible. Of course, other variations, modifications, and alternatives are possible.

  The force wedge device described in U.S. Patent Application No. 2006/0177362 A1 by D'Evelyn et al., Referenced throughout this specification to provide a baseline, is shown in FIG. 1. Capsules as described in US Pat. No. 7,125,453 are placed in a heater as described in US Patent Application No. 2008 / 0083741A1, each of which Are referred to herein. Both the capsule and the heater are housed in a high strength enclosure that can be manufactured from SA 723 pressure vessel steel. Here, from paragraph 51, “The method includes placing a plurality of radial segments (block 126) between the high-strength enclosure and the capsule. These radial segments include each radial segment. Are continuously arranged around the capsule to be a wedged portion of a divided cylinder, and the radial segments may include ceramics such as alumina, silicon nitride, silicon carbide, zirconia, etc. In addition, the radial segment may include a sparingly soluble metal such as tungsten, molybdenum, or a TZM alloy, or a cermet such as cobalt sintered tungsten carbide. " As described above, the conventional force wedge device has limitations. That is, it is expensive to manufacture a device having a large number of radial segments. Furthermore, it is difficult to accurately manufacture each of the radial segments and assemble them into the device. Providing one or more cracks in the radial segment has been found to reduce the performance of the radial segment unless they form an interconnected network. Making it possible or intended to introduce one or more cracks in a segment allows the production of devices with fewer segments. In addition, the manufacturing cost of the segment can be reduced by allowing one or more cracks to be present in the segment, since small cracks in the ceramic portion that can grow in the crack can now be tolerated.

  FIG. 2 is a schematic view of a high pressure apparatus according to an embodiment of the present invention. This drawing is only an example, and should not unduly limit the scope of the claims herein. Those skilled in the art will appreciate other variations, modifications, and alternatives. As shown, the present invention provides an apparatus for high pressure crystal or material processing, eg, GaN, AlN, InN, InGaN, AlGaN, and AlInGaN. Other processing methods include hydrothermal crystal growth of oxides and other crystalline materials, hydrothermal synthesis or hot ammonia synthesis, and hydrothermal decomposition, and others. Of course, other variations, modifications, and alternatives are possible.

  Referring to FIG. 2, a high pressure apparatus 200 and associated method for processing a supercritical fluid is shown. In certain embodiments, the apparatus 200 includes a capsule 210, a heating member or heater 212, and at least one ceramic ring 214, which may be a plurality of rings, optionally 1 There are more than one scribe mark and / or crack. In certain embodiments, the apparatus optionally has one or more metal sleeves (not shown) that include each ceramic ring. In addition, the apparatus includes a high strength enclosure 218, end flanges 226 and 228 with associated thermal insulation, and a power control system 230. The device is scalable to very large volumes and is cost effective. In certain embodiments, the apparatus can be at a pressure of 0.2-2 GPa and a temperature of 400-1200 ° C, respectively. Further, in certain embodiments, the apparatus includes a temperature controller 232. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the apparatus 200 comprises a plurality of heating zones, including at least one heating zone, optionally more, eg, two or more. The heating zone includes an uppermost first zone 220, a growth zone 222, a baffle zone 224, and a filling or nutrient zone 226 according to certain embodiments. According to certain embodiments, an internal baffle (not shown) aligns with the baffle gap zone when the capsule is inserted into the volume defined by the heater inner surface. The baffle, according to a particular embodiment, defines two chambers inside the capsule, namely a nutrient chamber and a growth chamber. The two chambers communicate through a perforated baffle that can have a variety of shapes and configurations. In an exemplary embodiment suitable for crystal growth where the solubility of the material to be recrystallized is a function of increasing temperature, the growth zone is located above the nutrient zone. In other embodiments suitable for crystal growth where the solubility of the material to be recrystallized is a decreasing function of temperature, i.e., reduced solubility, the growth zone is located below the nutrient zone. In still other embodiments, the device 200 is substantially horizontal rather than vertical and can include a rocking mechanism (not shown).

  In one embodiment, a capsule suitable for insertion into the heater is formed from a noble metal. Examples of noble metals include platinum, palladium, rhodium, gold, or silver. Other metals can include titanium, rhenium, copper, stainless steel, zirconium, tantalum, alloys thereof, and the like. In one embodiment, the metal functions as an oxygen getter. Suitable capsule dimensions may be greater than 2 cm in diameter and longer than 4 cm in length. In one embodiment, the diameter dimension is in a range selected from 2-4 cm, 4-8 cm, 8-12 cm, 12-16 cm, 16-20 cm, 20-24 cm, and any larger than 24 cm. In the second embodiment, the ratio of capsule length to diameter is greater than 2. In still other embodiments, the ratio of length to diameter is 2-4, 4-6, 6-8, 8-9, 9-10, 10-11, 11-12, 12-14, 14-16, 16-18, 18-20, and in any range greater than 20. Of course, other variations, modifications, and alternatives are possible.

  In one embodiment, the volume of the growth zone 222 is twice the volume of the filling zone 226. The electrical circuit for each heating element segment is controlled independently. Independent control is flexibly done to achieve and maintain a thermal evaporation profile along the capsule height. The physical discontinuity from the top between the second and third heater segments is at a temperature close to the baffle plate located in the capsule and separating the filling zone 226 and the growth zone 222, Create a local dip. In one embodiment, the filling zone and the growth zone are isotherms at different temperatures. The baffle zone has a temperature gradient over a relatively short distance between the isotherm of the filling zone and the isotherm of the growth zone. The resulting isotherm with the winding pattern of the heating elements and the minimum temperature gradient over the distance between the heating elements minimizes or eliminates nucleation of the walls inside the capsule and in or on the baffle. In one embodiment, the growth zone may be at the bottom and the filling zone may be at the top. Such a configuration can be based on specific chemistry and growth parameters.

  With particular reference to FIG. 2, the heater 212 is disposed in a device 200 that includes a container or high-strength enclosure 218. A first end flange 228 can be attached to the top end of the container and a second end flange 226 can be attached to the bottom end. A plurality of fasteners 216 (only one is indicated by a symbol) secures the end flange to the container end.

  Within the container 218, a continuous ceramic annular member 214 is arranged along the inner surface of the container and contacts the outer surface of the heater 212. Examples of annular materials include but are not limited to zirconium oxide or zirconia. First and second end caps 232 (only the first and second ones are shown in the figure) are disposed proximate to the end of the heater 212 inside the container. The annular plug 234 is shown as a stacked disk, but may be an annular body surrounding the end cap 232. Annular plug 234 can optionally be placed at at least one end and in the cavity between the capsule and end flange to reduce axial heat loss, zirconium oxide or zirconia. Can be included. Alternative plug materials may include magnesium oxide, salts, and phyllosilicate minerals such as aluminum hydroxide silicate or pyrophyllite according to certain embodiments.

  The device 200 may include a pressure transmission medium between the axial end of the capsule (see 106) and the end cap and / or annular plug, according to certain embodiments. The pressure transmission medium can include sodium chloride, other salts, or phyllosilicate minerals such as aluminum hydroxide silicate or pyrophyllite, or other materials, according to certain embodiments. Furthermore, between the outer diameter of the capsule and the inner diameter of the heating member, despite the selective presence of a coating or foil to reduce friction and facilitate the sliding and removal of the capsule after operation. The interface may be substantially free of pressure transmission media. The interface between the outer diameter of the heating member and the inner diameter of the continuous annular ring is also substantially free of pressure transmission media.

  The illustrated apparatus 200 can be used to grow crystals under pressure and temperature conditions desirable for crystal growth, for example, gallium nitride crystals can be grown under relevant process conditions. The high pressure apparatus 200 can include one or more structures operable to support the heater 212 in a radial direction, axially, or both radially and axially. The support structure of one embodiment insulates the device 200 from the ambient environment, such insulation can improve or improve process stability and maintain and control a desired temperature profile. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the device includes a capsule region that includes a first region and a second region and a length defined therebetween (eg, having a cylindrical shape). In certain embodiments, a capsule is placed within the capsule region. As an example, the capsule can be manufactured from a suitable material that is chemically inert, can withstand pressure, and can be easily handled in other features. Depending on the embodiment, the capsule is made from a material selected from gold, platinum, silver, or palladium. Of course, depending on the particular embodiment, other suitable materials may also be included that may include alloys, coatings, and / or multilayer structures. Other metals can include titanium, rhenium, copper, stainless steel, zirconium, tantalum, alloys thereof, and the like. In certain embodiments, the capsule is characterized by a deformable material and is substantially chemically inert to one or more reactants within the capsule region. An example of a capsule is described in US Pat. No. 7,125,453, which is hereby incorporated by reference for all purposes. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the apparatus has an annular heating member that surrounds the capsule region. Another example of a heating member is described in US Patent Application No. 2008 / 0083741A1, which is also referenced herein. The heating element can have at least two independently controllable high temperature zones, with heating power as large as 3 kW, 10 kW, 30 kW, 100 kW, 300 kW, or 1000 kW. Can be generated. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the apparatus has at least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness continuously disposed around the annular heating member. In certain embodiments, the continuous annular member is made of a material having a compressive strength greater than about 0.5 GPa and a thermal conductivity less than about 4 watts per meter Kelvin. As an example, ceramic materials include rare earth metal oxides, zirconium oxide, hafnium oxide, magnesium oxide, calcium oxide, aluminum oxide, yttrium oxide, sialon (Si—Al—O—N), silicon nitride, silicon oxynitride, garnet, Can include cristobalite and mullite. The ceramic material can be a composite comprising two or more phases. Alternatively, as an example, the metal may be a poorly soluble metal such as tungsten, molybdenum, a TZM alloy, and others. The cermet can be cobalt sintered tungsten carbide, and others. In an alternative embodiment described further below, the continuous annular member made of ceramic, metal, or cermet is asymmetrically disposed and the inner diameter of the continuous annular member made of ceramic, metal, or cermet and the ceramic, metal Or a plurality of crack regions arranged between the outer diameter of a continuous annular member made of cermet. In certain embodiments, the annular member is one of a plurality of members that are stacked on top of each other. Of course, other variations, modifications, and alternatives are possible.

  Furthermore, in certain embodiments, the apparatus has a cylindrical sleeve member disposed on at least an annular member made of ceramic, metal or cermet. As an example, the cylindrical sleeve member is manufactured from a material selected from stainless steel, iron, steel, iron alloys, nickel or nickel alloys, cobalt or cobalt alloys, or any combination thereof. In certain embodiments, the cylindrical sleeve member comprises a first end and a second end. In certain embodiments, the cylindrical sleeve defines dimensions.

  Depending on the embodiment, the first end is first to form a taper angle in the range of about 0.1 to 5 degrees between the axis of the cylindrical sleeve member and the outer region of the cylindrical sleeve member. And the second end is characterized by a second outer diameter that is smaller than the first outer diameter. Of course, other variations, modifications, and alternatives are possible.

  Furthermore, the cylindrical sleeve member has a substantially constant inner diameter from the first end to the second end, according to certain embodiments, but the inner diameter may vary depending on the embodiment. it can. In a preferred embodiment, the cylindrical sleeve member is configured to cooperate with the high pressure enclosure material to compress a continuous annular member made of ceramic. In a preferred embodiment, the cylindrical sleeve member is configured to provide a mechanical support to maintain the defined shape of the ceramic continuous annular member. In a more preferred embodiment, the cylindrical sleeve is configured to cooperate with the high pressure enclosure material to compress the ceramic continuous annular member, and is provided with a mechanical support to provide the ceramic continuous It is configured to maintain a defined shape of the annular member. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the device has a high strength enclosure material disposed on a ceramic annular member. In certain embodiments, the high-strength enclosure is manufactured from a suitable material to contain internal contents including capsules, heaters, and sleeves among other elements. In certain embodiments, the high strength enclosure is steel, low carbon steel, SA 723 steel, SA 266 carbon steel, 4340 steel, A-286 steel, iron-based superalloy, 304 stainless steel, 310 stainless steel, 316 stainless steel. Steel, 340 stainless steel, 410 stainless steel, 17-4 precipitation hardened stainless steel, zirconium and its alloys, titanium and its alloys, and commonly known as Monel, Inconel, Hastelloy, Udimet 500, Stylete, Rene 41, and Rene 88 Manufactured from a material selected from the group consisting of other materials. In a preferred embodiment, the high strength enclosure provides maximum tensile strength and yield strength characteristics as rated by the American Society of Mechanical Engineers for continuous operation of pressure vessels at pressures greater than 50,000 pounds per square inch. A material having Of course, those skilled in the art will appreciate other variations, modifications, and alternatives.

  Furthermore, the high strength enclosure has a desired length and width, according to certain embodiments. In certain embodiments, the high strength enclosure has a length and an inner diameter to define an aspect ratio of about 2 to about 25. The high strength enclosure has a length and an inner diameter to define an aspect ratio of about 10 to about 12. In certain embodiments, the inner diameter is about 2 inches to about 50 inches. In certain embodiments, the height of the high strength enclosure is between 6 inches and 500 inches. The ratio of the outer diameter to the inner diameter of the high strength enclosure can be 1.2-5. In certain embodiments, the diameter ratio can be about 1.5 to about 3. Of course, other variations, modifications, and alternatives are possible. Further details of the device can be found throughout the present specification and in more detail below.

In a particular embodiment, the apparatus 300 is shown in FIG. This drawing is only an example, and should not unduly limit the scope of the claims herein. Those skilled in the art will appreciate other variations, modifications, and alternatives. One or more rings 307 may be stacked in the device instead of individual radial segments arranged sequentially in the device. The ring may include ceramics such as alumina, silicon nitride, silicon carbide, zirconia, etc., including other materials described herein as well known to those skilled in the art. Alternatively, the ring may include a refractory metal such as tungsten, molybdenum, or a TZM alloy, or a cermet such as cobalt sintered tungsten carbide. The ring can have an inner diameter of 0.5 to 24 inches, an outer diameter of 1 to 48 inches, and a height of 1 to 96 inches. In certain embodiments, the inner diameter is about 1.5 inches to about 8 inches and the height is 1.5 inches to 8 inches. The ratio of the outer diameter to the inner diameter of the ring can be 1.05-60. In certain embodiments, the diameter ratio can be about 1.5 to about 3. The ring can have a density greater than 95% of theoretical density. The rupture factor of the ring material may be greater than 200 or 450 MPa. The fracture toughness of the ring material may be greater than 9 MPa-m ^1/2 . Depending on the dimensions of the ring and the high-strength enclosure, it is possible to stack 1 to 200 rings on top of each other within the high-strength enclosure.

  In certain embodiments, spacers having a thickness of 0.001 inch to 0.1 inch can be placed between successive rings of the stack to allow thermal expansion. A sleeve 309 can be placed around each ring. The sleeve may include steel or other suitable material, according to certain embodiments. The sleeve may be 0.020 inches to 0.5 inches thick, and the height of the sleeve is from 0.25 inches lower than the ring height to higher than the ring height, depending on the embodiment. It may be in the range up to 0.1 inch. In addition, the apparatus includes a capsule 301, a thermocouple 303, a heater 305, and a high strength enclosure 311 that are electrically connected to the temperature controller and / or power controller among other elements. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the ceramic ring hardly cracks under operating conditions, as shown in FIG. For example, the breaking strength of the ring can be greater than the operating pressure of the capsule. In other embodiments, an interference fit with a high strength enclosure provides a radial compressive load on the ring. In one embodiment, an interference fit is achieved by heating the high strength enclosure and / or cooling the ring prior to assembly. In other embodiments, at the inner diameter of the high strength enclosure and at the ring and / or the sleeve surrounding it, grinding to a slight taper, for example about once, and then pressing the ring and sleeve against the high strength enclosure, By realizing an interference fit, the interference fit is realized.

  In other embodiments, the ring has at least one crack under the operating condition of the device 400, as shown in FIG. In certain embodiments, the ring 407 can be inserted into a high strength enclosure and cracked during initial operation. By scribing the inner diameter of the ring at the desired crack start point, cracking at a particular location can be facilitated. The resulting cracks can extend all the way from the inner diameter to the outer diameter, or can terminate in the volume of the ring and / or have any combination of these structures. In other embodiments, the ring breaks prior to insertion into the high strength enclosure. Pre-cracking can be achieved by sliding a precision rotating rod with a higher coefficient of thermal expansion than the ring into the inner diameter of the ring and heating. If the crack penetrates the ring completely at various radial positions, the sleeve 409 surrounding the ring holds and maintains all parts of the ring so that they are correctly oriented together and relative to each other. In other embodiments, cracks are present in the volume of the ring but do not contact the inner or outer diameter of the ring. In addition, the device 400 includes a capsule 401, a thermocouple 403 electrically connected to the temperature controller and / or power controller, a heater 405, and a high strength enclosure 411 among other elements. Of course, other variations, modifications, and alternatives are possible.

  FIG. 4A is a schematic cross-sectional view of another high pressure device that is an alternative embodiment of the present invention. In certain embodiments, two or more annular segments 457 forming a continuous ring structure can be inserted into the high strength enclosure and cracked during initial operation. In certain embodiments, there are two or more annular segments, or three or more annular segments, or four or more annular segments, or other combinations, where each of the segments has a similar length or It may have different lengths. By scribing the inner diameter of two or more annular segments at the desired crack initiation point, cracking at a particular location can be facilitated. The resulting crack can extend all the way from the inner diameter to the outer diameter, or can terminate in the volume of two or more annular segments and / or have any combination of these structures. Is possible.

  In other embodiments, two or more annular segments are cracked prior to insertion into a high strength enclosure. Pre-cracking can be achieved by sliding a precision rotating rod having a higher coefficient of thermal expansion than two or more annular segments into the inner diameter of the split ring and heating. If the crack penetrates the segment completely at various radial positions, the sleeve 409 surrounding the segment holds and maintains all parts of the segment so that they are accurately oriented together and relative to each other. In other embodiments, cracks are present in the volume of the segment but do not contact the inner or outer diameter of the segment. In addition, the device 450 includes a capsule 451, a thermocouple 453, a heater 455, and a high strength enclosure 461 that are electrically connected to the temperature controller and / or power controller, among other elements.

  In certain embodiments, the method and associated annular segments include slight irregularities and / or defects. In certain embodiments, the segments are manufactured from a suitable material that can fit itself by cracking. In addition, slight changes in the dimensions of each of the ceramic members are also accepted by the cracks, which allows the assembly to be placed approximately continuously around the heating member. In certain embodiments, the apparatus and associated devices prevent breakage of the capsule and / or high-strength enclosure by providing a buffer area and / or a thermal insulation area between the capsule and the high-strength enclosure. Of course, other variations, modifications, and alternatives are possible.

  The vertical dimension is a dimension in the direction perpendicular to the paper surface of FIGS. 3, 4, and 4A. The top and bottom of the cavity defined by the inner diameter of the ring are terminated by a thermally insulating plug positioned close to the end flange, as shown in FIG. Bolts can attach the end flange to the high strength enclosure. The ratio of cavity length to diameter should be at least 2: 1 and more preferably in the range of 5: 1 to 15: 1.

  In order to measure temperature at various heights of the outer diameter of the capsule, at least one axial recess or groove is placed on the outer diameter of the capsule at a particular radial position prior to assembly. In the example shown in FIGS. 3 and 4, the four recesses or grooves are arranged at 90 degrees along the outer diameter of the capsule. The groove or recess can extend over the entire height of the capsule or can terminate at a height along the capsule, where temperature measurement is desired. The width or depth of the groove or recess may be about 0.025 inches to 0.130 inches. A hole with a diameter slightly larger than the diameter of the thermocouple can be placed in one or both end flanges. Furthermore, a hole or groove can be arranged in at least one insulating cylinder separating the end flange and the capsule. After inserting the capsule into the heater, it is possible to insert a thermocouple into the groove or recess and then place the end flange on the high strength enclosure. Alternatively, before placing the end flange, insert one or more thermocouples into the grooves or recesses, before placing the end flange and before attaching the electrical connection to the free end of the thermocouple. The ends may be arranged on the end flange. Further details of the method according to embodiments of the invention are described below.

A brief overview of the method according to certain embodiments is provided below.
1. To provide an apparatus for high pressure crystal growth or material processing, such as the above apparatus, but may be others. The apparatus includes a first region and a second region, a capsule region having a length defined therebetween (for example, a cylindrical shape), an annular heating member surrounding the capsule region, and the annular heating member At least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness continuously disposed around the periphery of the substrate and a high strength enclosure material disposed thereon.
2. To provide a capsule containing a solvent.
3. Place the capsule within the inner area of the capsule area.
4). Treating the capsule with thermal energy, raising the temperature inside the capsule to a temperature higher than 200 degrees Celsius and heating the solvent.
5. Form crystalline material from solvent heat treatment.
6). Removing thermal energy from the capsule and changing the temperature of the capsule from a first temperature to a second temperature lower than the first temperature.
7). Removing the first flange and the second flange from the high pressure device;
8). Using a hydraulic driving force, the mechanical member is moved from the first region of the capsule region toward the second region to move the capsule from the capsule region.
9. Open the capsule.
10. Remove the crystalline material.
11. Perform other steps as desired.

  The order of the above steps performs the method according to an embodiment of the present invention. In certain embodiments, the present invention provides a method performed by a high pressure apparatus having a configured support member and the resulting crystalline material. Further, other alternative methods in which steps are added, one or more steps are eliminated, or one or more steps are performed in a different order, depart from the claims herein. Can be done without. Details of the method and structure of the present invention can be found throughout the present specification and in more detail below.

  FIG. 5 is a schematic diagram 500 of a method of processing a supercritical fluid, according to one embodiment of the present invention. This drawing is only an example, and should not unduly limit the scope of the claims herein. Those skilled in the art will appreciate other variations, modifications, and alternatives. In certain embodiments, the method begins at the beginning of step 501. Otherwise, the method begins by providing an apparatus for high pressure crystal or material processing (step 503), which may be other such as the above apparatus. In certain embodiments, the device has a capsule region having a first region and a second region and a length defined therebetween. Furthermore, the device comprises an annular heating member surrounding the capsule region, at least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness continuously disposed around the capsule member, and thereon. With high strength enclosure material disposed. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the method provides a capsule containing a solvent, such as ammonia (step 505). In certain embodiments, the method places a capsule containing the solvent and the starting crystal within the interior region of the capsule region (step 507). The method treats the capsule with thermal energy, raises the interior of the capsule to a temperature greater than 200 degrees Celsius, and superheats the solvent (step 509). Of course, other variations, modifications, and alternatives are possible.

  Referring again to FIG. 5, the method forms a crystalline material from a solvent heat treatment (step 511). In a preferred embodiment, the crystalline material is gallium, including crystals such as GaN, AlGaN, InGaN, and others. In certain embodiments, the method removes thermal energy from the capsule and changes the temperature of the capsule from a first temperature to a lower second temperature (step 513). When energy is removed and the temperature is reduced to an appropriate level, the method removes at least one or more flanges that mechanically hold the capsule in place (step 515). In a preferred embodiment, the method uses a mechanical member, such as a plunger, wherein the mechanical member is hydraulically moved from a first region of the capsule region to a second region (step 517), so that the capsule is in the capsule region. Is released from the apparatus.

  In certain embodiments, the capsule is now released from the device. In certain embodiments, the capsule is opened (step 519). In a preferred embodiment, the crystalline material is removed from the inner region of the capsule (step 521). Depending on the embodiment, other steps that can be inserted or added can be used, or some steps can be eliminated. In certain embodiments, the method ends with a stop at step 523. Of course, other variations, modifications, and alternatives are possible.

  The order of the above steps performs the method according to an embodiment of the present invention. In certain embodiments, the present invention provides a method performed by a high pressure apparatus having a configured support member and the resulting crystalline material. Further, other alternative methods in which steps are added, one or more steps are eliminated, or one or more steps are performed in a different order, depart from the claims herein. Can be done without.

A brief overview of the method according to certain alternative embodiments is given below.
1. Assembling an apparatus for high pressure crystal or material processing, such as the above apparatus, but may be others. The apparatus continuously includes a first region, a second region, a capsule region having a length defined therebetween, an annular heating member surrounding the capsule region, and a periphery of the annular heating member. At least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness disposed thereon and a high strength enclosure material disposed thereon.
2. Providing the capsule with the material to be treated and the solvent.
3. Place the capsule within the inner area of the capsule area.
4). Place the annular plug, end cap, and end flange on the end of the device.
5. Attach the end flange using at least one fastener.
6). Applying electrical energy to the heating member to raise the inside of the capsule to a temperature higher than 200 degrees Celsius and superheat the solvent.
7). Form crystalline material from solvent heat treatment.
8). Removing thermal energy from the capsule and changing the temperature of the capsule from a first temperature to a second temperature lower than the first temperature.
9. Removing the first flange and the second flange from the high pressure device;
10. Using a hydraulic driving force, the mechanical member is moved from the first region of the capsule region toward the second region to move the capsule from the capsule region.
11. Open the capsule.
12 Remove the crystalline material.
13. Perform other steps as desired.

  The order of the above steps performs the method according to an embodiment of the present invention. In certain embodiments, the present invention provides a method performed by a high pressure apparatus having a configured support member and the resulting crystalline material. Further, other alternative methods in which steps are added, one or more steps are eliminated, or one or more steps are performed in a different order, depart from the claims herein. Can be done without. Details of the method and structure of the present invention can be found throughout the present specification and in more detail below.

  FIG. 6 is a schematic flowchart 600 of an alternative method of processing a material with a supercritical fluid, according to an alternative embodiment of the present invention. This drawing is only an example, and should not unduly limit the scope of the claims herein. Those skilled in the art will appreciate other variations, modifications, and alternatives. In certain embodiments, the method begins at the beginning of step 601. The method begins by assembling an apparatus for high pressure crystal or material processing (step 603), such as the above apparatus, but may be others. In certain embodiments, the device has a capsule region (eg, a cylindrical shape) having a first region and a second region and a length defined therebetween. The apparatus further comprises an annular heating member surrounding the capsule region and at least one continuous annular member made of ceramic or metal or cermet having a predetermined thickness continuously disposed around the capsule region, The annular heating member and the continuous annular member are assembled together at step 605. In certain embodiments, the capsule, the heating member, and the annular member are inserted into a high strength enclosure material that is disposed on the ceramic annular member. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the method provides a capsule containing a material to be treated, including a solvent such as ammonia (step 607). In a preferred embodiment, the capsule is sealed (step 609). In certain embodiments, each of the capsule ends is welded and / or brazed to form a sealed capsule structure. In certain embodiments, the method provides for assembly by placing a capsule containing the solvent and the starting crystal within the interior region of the capsule region (step 611). In a preferred embodiment, the method places an annular plug, end cap, and end flange at each end of the device (step 613). See, for example, FIG. In a preferred embodiment, each end flange is secured by one fastener or a plurality of fasteners. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the method provides electrical energy in the form of power to the heating member (step 617). A heating member provides thermal energy to the capsule to a predetermined process temperature and pressure, and according to certain embodiments, causes the solvent to be in a supercritical state. By this method, the capsule is treated with thermal energy, the inside of the capsule is raised to a temperature higher than 200 degrees Celsius, and the solvent is overheated. Of course, other variations, modifications, and alternatives are possible.

  In certain embodiments, the method forms crystalline material from solvent heat treatment. In a preferred embodiment, the crystalline material is gallium, including crystals such as GaN, AlGaN, InGaN, and others. In certain embodiments, the method removes thermal energy from the capsule and changes the temperature of the capsule from a first temperature to a lower second temperature. When energy is removed and the temperature is reduced to an appropriate level, the method removes at least one or more flanges that mechanically hold the capsule in place. In a preferred embodiment, the method uses a mechanical member, such as a plunger, wherein the mechanical member is hydraulically moved from a first region of the capsule region to a second region, and the capsule is moved from the capsule region. Released from the device.

  In certain embodiments, the capsule is now released from the device. In certain embodiments, the capsule is opened. In a preferred embodiment, the crystalline material is removed from the inner region of the capsule. Depending on the embodiment, other steps that can be inserted or added can be used, or some steps can be eliminated. In certain embodiments, the method ends with a stop at step 619. Of course, other variations, modifications, and alternatives are possible.

  The order of the above steps performs the method according to an embodiment of the present invention. In certain embodiments, the present invention provides a method performed by a high pressure apparatus having a configured support member and the resulting crystalline material. Further, other alternative methods in which steps are added, one or more steps are eliminated, or one or more steps are performed in a different order, depart from the claims herein. Can be done without.

  While the above is a complete description of a particular embodiment, various modifications, alternative constructions and equivalents can be used. Therefore, the above description and drawings should not be taken as limiting the scope of the invention which is defined by the appended claims.

Claims (28)

A high-pressure apparatus for processing high-pressure crystals or materials,
A first region and a second region, and a capsule region having a length defined between the first region and the second region;
An annular heating member surrounding the capsule region;
At least one continuous annular member having a predetermined thickness continuously disposed around the annular heating member, having a compressive strength greater than about 0.5 GPa and greater than about 100 watts per meter Kelvin At least one continuous annular member made of a material having low thermal conductivity;
A high-strength enclosure material disposed on the annular member to form a high-strength enclosure;
A high pressure apparatus for processing high pressure crystals or materials.   The high-strength enclosure is configured to withstand loads greater than about 0.1 GPa over a period of time and temperatures below 200 degrees Celsius, the capsule region is configured in a cylindrical shape, and the continuous annular member The high pressure apparatus for high pressure crystal or material processing according to claim 1, wherein the high pressure crystal or material is manufactured from a material selected from at least ceramic, metal, or cermet.   The high-strength enclosure is configured to withstand loads greater than about 0.1 GPa over a period of time and temperatures below 200 degrees Celsius, the capsule region is configured in a cylindrical shape, and the continuous annular member is The high pressure apparatus for high pressure crystal or material processing according to claim 1, wherein the high pressure crystal or material processing is made of at least ceramic and the thermal conductivity is lower than 4 watts per meter Kelvin.   The high-pressure device further includes a capsule disposed in the capsule region, and the capsule is gold, platinum, silver, palladium, rhodium, titanium, rhenium, copper, stainless steel, zirconium, tantalum, or an alloy thereof. 2. The high pressure crystal or material processing high pressure apparatus of claim 1 comprising a material selected from:   The high-pressure device further includes a cylindrical sleeve member disposed on the at least one annular member, and the cylindrical sleeve member is stainless steel, iron, steel, an iron alloy, nickel or a nickel alloy, or a combination thereof. 2. The high-pressure apparatus for processing high-pressure crystals or materials according to claim 1, manufactured from a material selected from any combination.   The cylindrical sleeve member comprises a first end and a second end, and is between about 0.1 and 5 degrees between the axis of the cylindrical sleeve member and the outer region of the cylindrical sleeve member. To form a range of taper angles, the first end is characterized by a first outer diameter, and the second end is characterized by a second outer diameter that is smaller than the first outer shape. The high-pressure apparatus for processing a high-pressure crystal or material according to claim 5 attached.   5. The high pressure crystal or material processing high pressure of claim 4, wherein the high pressure device further comprises one or more reactants in the capsule, the one or more reactants comprising ammonia and a mineralizer. apparatus.   The high-strength enclosure is steel, low carbon steel, SA 723 steel, SA 266 carbon steel, 4340 steel, A-286 steel, iron-based superalloy, 304 stainless steel, 310 stainless steel, 316 stainless steel, 340 stainless steel , 410 stainless steel, 17-4 precipitation hardened stainless steel, zirconium and its alloys, titanium and its alloys, Monel, Inconel, Hastelloy, Udimet 500, Stellite, Rene 41, and Rene 88. The apparatus of claim 1, wherein:   The high strength enclosure has a length and an inner diameter to define an aspect ratio of about 2 to about 25, the inner diameter is about 2 inches to about 50 inches, and the length of the high strength enclosure is 6 2. The high-pressure apparatus for high-pressure crystal or material processing according to claim 1, wherein the ratio of the outer diameter to the inner diameter of the high-strength enclosure is 1.2 to 5 inches.   The at least one continuous annular member has an inner diameter of 1.5 inches to 8 inches, a height of 1.5 inches to 8 inches, and a ratio of the outer diameter to the inner diameter of 1.5-3. The high-pressure apparatus for processing a high-pressure crystal or material according to claim 1. A high-pressure apparatus for processing high-pressure crystals or materials,
A first region and a second region, and a capsule region having a length defined between the first region and the second region;
An annular heating member surrounding the capsule region;
Two or more annular members having a predetermined thickness arranged sequentially and continuously around the annular heating member, wherein the compressive strength is greater than about 0.5 GPa and about 100 watts per meter kelvin Two or more annular members made from a material having a lower thermal conductivity;
Two or more irregularly shaped surface regions that are spatially disposed within one or more of the annular members and that are paired to substantially bond together along a portion of a common boundary region;
A high-strength enclosure material disposed on the two or more annular members to form a high-strength enclosure;
A high pressure apparatus for processing high pressure crystals or materials.   The high-strength enclosure is configured to withstand loads greater than about 0.1 GPa over a period of time and temperatures lower than 200 degrees Celsius, and the two or more annular members are made of at least metal, ceramic, or cermet The high-pressure apparatus for processing high-pressure crystals or materials according to claim 11, wherein the high-pressure crystal or material is manufactured from a selected material and the capsule region is formed in a cylindrical shape.   The high-strength enclosure is configured to withstand a load greater than about 0.1 GPa over a period of time and a temperature lower than 200 degrees Celsius, and the two or more annular members are made of at least ceramic, the capsule region The high pressure apparatus for high pressure crystal or material processing according to claim 11, wherein the high temperature crystal is configured in a cylindrical shape and the thermal conductivity is lower than 4 watts per metric kelvin.   The high pressure apparatus for high pressure crystal or material processing according to claim 11, wherein the common boundary region has one or more cracks.   The high-pressure apparatus for high-pressure crystal or material processing according to claim 11, wherein the irregularly shaped surface area is constituted by a root mean square surface roughness greater than about 0.1 mm, 0.5 mm or 1 mm.   The high-pressure apparatus further includes a capsule disposed in the capsule region, and the capsule is at least gold, platinum, silver, palladium, rhodium, titanium, rhenium, copper, stainless steel, zirconium, tantalum, or the like The high-pressure apparatus for processing high-pressure crystals or materials according to claim 11 manufactured from a material selected from the alloys of:   The high-pressure device further includes a cylindrical sleeve member disposed on the at least two annular members, and the cylindrical sleeve member is at least stainless steel, iron, steel, iron alloy, nickel or nickel alloy, cobalt Or a high pressure apparatus for processing high pressure crystals or materials according to claim 11 manufactured from a material selected from a cobalt alloy or any combination thereof.   The cylindrical sleeve member comprises a first end and a second end, and is between about 0.1 and 5 degrees between the axis of the cylindrical sleeve member and the outer region of the cylindrical sleeve member. To form a range of taper angles, the first end is characterized by a first outer diameter, and the second end is characterized by a second outer diameter that is smaller than the first outer diameter. 18. A high-pressure apparatus for processing high-pressure crystals or materials according to claim 17.   The cylindrical sleeve member is configured to provide a mechanical support to maintain a defined shape of the continuous annular member, wherein the continuous annular member is asymmetrically disposed and the continuous 18. The high-pressure apparatus for high-pressure crystal or material processing according to claim 17, wherein the high-pressure crystal or material processing device is configured to include a plurality of crack regions disposed between an inner diameter of an annular member and an outer diameter of the continuous annular member.   The high pressure crystal or material processing high pressure of claim 11, wherein the high pressure device further comprises one or more reactants in the capsule, the one or more reactants comprising ammonia and a mineralizer. apparatus.   The high-strength enclosure is steel, low carbon steel, SA 723 steel, SA 266 carbon steel, 4340 steel, A-286 steel, iron-based superalloy, 304 stainless steel, 310 stainless steel, 316 stainless steel, 340 stainless steel , 410 stainless steel, 17-4 precipitation hardened stainless steel, zirconium and its alloys, titanium and its alloys, Monel, Inconel, Hastelloy, Udimet 500, Stellite, Rene 41, and Rene 88. The high-pressure apparatus for processing a high-pressure crystal or material according to claim 11.   The high strength enclosure has a length and an inner diameter to define an aspect ratio of about 2 to about 25, the inner diameter is about 2 inches to about 50 inches, and the length of the high strength enclosure is 6 The high-pressure apparatus for high-pressure crystal or material processing according to claim 11, wherein the ratio of the outer diameter to the inner diameter of the high-strength enclosure is 1.2 to 5 inches.   The at least one continuous annular member has an inner diameter of 1.5 inches to 8 inches, a height of 1.5 inches to 8 inches, and a ratio of the outer diameter to the inner diameter of 1.5-3. The high-pressure apparatus for processing high-pressure crystals or materials according to claim 11. A crystal growth method using a high pressure crystal or a high pressure apparatus for material processing,
The high-pressure device is
A first region and a second region, and a capsule region having a length defined between the first region and the second region;
An annular heating member surrounding the capsule region;
Two or more annular members made of ceramic or metal or cermet having a predetermined thickness arranged sequentially and continuously around the annular heating member, the compression strength being greater than about 0.5 GPa; Two or more annular members made from a material having a thermal conductivity of less than about 100 watts per metric kelvin;
Two or more irregularly shaped surface regions that are spatially disposed within one or more of the annular members and that are paired to substantially bond together along a portion of a common boundary region;
A high strength enclosure material disposed on said ceramic or metal or cermet annular member;
Providing a capsule containing a solvent;
Disposing a capsule within an internal region of the capsule region;
Treating the capsule with thermal energy to raise the inside of the capsule to a temperature higher than 200 degrees Celsius and superheating the solvent;
A crystal growth method using a high-pressure crystal containing or a high-pressure apparatus for material processing.   The crystal growth method using the high-pressure crystal or material processing high-pressure apparatus according to claim 24, further comprising a step of forming or recrystallizing a crystal material from the heat treatment of the solvent.   The crystal growth method using the high-pressure crystal or the high-pressure apparatus for material processing according to claim 24, further comprising a step of forming a crystal material used for manufacturing an optical device or an electric device. A crystal growth method using a high pressure crystal or a high pressure apparatus for material processing,
The high-pressure device is
A first region and a second region, and a capsule region having a length defined between the first region and the second region;
An annular heating member surrounding the capsule region;
At least one continuous annular member having a predetermined thickness continuously disposed around the annular heating member, having a compressive strength greater than about 0.5 GPa and greater than about 100 watts per meter Kelvin At least one continuous annular member made of a material having low thermal conductivity;
A high strength enclosure material disposed on the annular member to form a high strength enclosure;
Providing a capsule containing a solvent;
Disposing the capsule within an internal region of the capsule region;
Treating the capsule with thermal energy to raise the interior of the capsule to a temperature higher than 200 degrees Celsius and superheating the solvent;
A crystal growth method using a high-pressure crystal containing or a high-pressure apparatus for material processing.   28. The crystal growth method using the high-pressure crystal or material processing high-pressure apparatus according to claim 27, further comprising forming a crystal material to be used for manufacturing an optical device or an electric device.

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