EP3126548A1 - High pressure reactor for supercritical ammonia and method for producing crystalline group iii nitride - Google Patents
High pressure reactor for supercritical ammonia and method for producing crystalline group iii nitrideInfo
- Publication number
- EP3126548A1 EP3126548A1 EP15715951.8A EP15715951A EP3126548A1 EP 3126548 A1 EP3126548 A1 EP 3126548A1 EP 15715951 A EP15715951 A EP 15715951A EP 3126548 A1 EP3126548 A1 EP 3126548A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- gasket
- taper
- reactor
- reactor according
- angle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/042—Pressure vessels, e.g. autoclaves in the form of a tube
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/008—Processes carried out under supercritical conditions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
- C30B7/105—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes using ammonia as solvent, i.e. ammonothermal processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/02—Apparatus characterised by their chemically-resistant properties
- B01J2219/025—Apparatus characterised by their chemically-resistant properties characterised by the construction materials of the reactor vessel proper
- B01J2219/0277—Metal based
- B01J2219/029—Non-ferrous metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Definitions
- the invention is related to a high-pressure reactor used to hold supercritical ammonia.
- the reactor is used to grow bulk crystal of group III nitride in supercritical ammonia.
- the reactor is also used to synthesize various metal nitride materials such as vanadium nitride, iron nitride, and titanium nitride.
- Group III nitride crystals are used to produce semiconductor wafers for various devices including optoelectronic devices such as light emitting diodes (LEDs) and laser diodes (LDs), and electronic devices such as transistors. More specifically, the group III nitride includes gallium. Description of the existing technology.
- Gallium nitride (GaN) and its related group III nitride alloys are the key material for various optoelectronic and electronic devices such as LEDs, LDs, microwave power transistors, and solar-blind photo detectors.
- LEDs are widely used in displays, indicators, general illuminations, and LDs are used in data storage disk drives.
- the majority of these devices are grown epitaxially on heterogeneous substrates, such as sapphire and silicon carbide because GaN substrates are extremely expensive compared to these heteroepitaxial substrates.
- the heteroepitaxial growth of group III nitride causes highly defected or even cracked films, which hinder the realization of high-end optical and electronic devices, such as high-brightness LEDs for general lighting or high-power microwave transistors.
- HVPE hydride vapor phase epitaxy
- the present invention discloses a high-pressure reactor and gasket suitable for a high-pressure process using supercritical ammonia.
- the reactor is suited to grow a bulk crystal of group III nitride and has a lateral dimension (e.g. diameter) greater than 2 inches.
- the reactor can instead synthesize various transition metal nitrides using supercritical ammonia.
- the reactor body has, for example, a cylindrical shape and is made of precipitation hardenable Ni-Cr based superalloy.
- the reactor has a lid made of precipitation hardenable Ni-Cr based superalloy on one end of the reactor body.
- the lid and body are in physical contact with a gasket made of Ni-based metal, and the Ni content of the gasket is higher than the Ni content of the precipitation hardenable Ni-Cr based superalloy of both the lid and reactor body.
- the gasket preferably contains more than 90% Ni and does not contain more than 10% copper.
- the gasket thickness may also decrease along the radial direction of the gasket so that the gasket is thinner at its outer radial edge than at its inner radial edge, and the thinnest part of the gasket is more than 0.2 inch thick.
- the gasket has sufficient compressive strength to withstand a compressive pressure of 60,000 psi or higher, and the gasket has a sufficiently high elastic limit or yield strength that the gasket can be reused at least 10 times before a replacement gasket is needed. This construction provides a consistent seal of the reactor for repeated use.
- FIG. 1 is a schematic drawing of the high-pressure reactor. In the figure, each number represents the following:
- FIG. 2 is one example of a gasket. In the figure, each number represents the following:
- FIG. 3 has examples of cross-sections of gaskets and measurement of thinnest thickness and taper angle. In the figure, each number represents the following:
- the inventor theorizes that the invention is based in a technical finding that makes the reactor and gasket as described herein exceptionally well-suited to commercial manufacturing of large ingots of group III- nitride materials using an ammonothermal method.
- the inventor found that a gasket having decreasing thickness toward its outer periphery, having a thickness no less than 0.20 inch at its thinnest point, and being formed of a Ni-based alloy as described below provides a gasket that can be used in a high-pressure ammonothermal reactor at least 10 times without suffering mechanical or performance failure.
- the high-pressure reactor of this invention is designed to grow group III nitride crystals or to synthesize various transition metal nitride materials such as vanadium nitride, iron nitride and titanium nitride.
- Bulk crystals of group III nitride such as GaN can be grown in supercritical ammonia.
- various metal nitride powders, nano-crystals, micro- crystals, and bulk crystals can be synthesized in supercritical ammonia. Crystal growth or material synthesis in supercritical ammonia is called ammonothermal process.
- high-pressure (1,000 psi ⁇ 60,000 psi) and high-temperature (300 ⁇ 600 °C) ammonia is prepared in a high-pressure reactor.
- crystal growth of GaN typically requires pressure higher than 25,000 psi and temperature higher than 450 °C.
- a high-pressure reactor of such pressure and temperature range is not commonly available.
- Parr Instruments Company provides a high-pressure reactor that can hold up to 5000 psi at 500 °C with internal diameter of 3.25".
- Another example is a High Pressure Equipment Company's high-pressure reactor that can reach 12,000 psi at 427 °C with internal diameter of 1 ".
- a high-pressure reactor having inner diameter larger than 2" which can reach 25,000 psi at temperature higher than 450 °C requires a specialized technology. Since, the structure of the high-pressure reactor must withstand such pressure and temperature, it is typically constructed with precipitation hardenable Ni-Cr based superalloys.
- typical ammonothermal process requires a chemical additive called a mineralizer to enhance the reaction.
- a mineralizer typically requires alkali metal mineralizers such as lithium, sodium or potassium, or halide mineralizer such as ammonium fluoride, ammonium chloride, ammonium bromide, or ammonium iodide.
- Alkali metal mineralizer creates basic supercritical ammonia whereas halide mineralizer creates acidic supercritical ammonia. In either case, the reactor material must be carefully selected to avoid corrosion by the supercritical ammonia.
- precipitation hardenable Ni-Cr based superalloy can be used as disclosed in United States Utility Patent Application Serial No. 61/058,910.
- Figure 1 illustrates a high-pressure reactor of this invention.
- the high-pressure reactor body 1 has a cylindrical shape and is made of precipitation hardenable Ni-Cr based superalloy.
- the high-pressure reactor body has an opening on one end and optionally a second opening at its opposite end so that internal components including source material, seed crystals, and baffles can be installed.
- the high-pressure reactor has at least one lid 2 made of precipitation hardenable Ni-Cr based superalloy at an end.
- the lid 2 is sealed with a gasket 4 made of Ni-based metal having an ultimate tensile strength in the range of 50-100 ksi and a Ni content that is greater than the nickel content of the body's precipitation hardenable Ni-Cr based superalloy, or preferably greater than 90%.
- the gasket material preferably contains little or no copper.
- the copper content may be less than 10% or, more preferably, less than 1%.
- a closing mechanism for the high-pressure reactor having inner diameter larger than 2" is preferably a clamp type closure 3 rather than a screw type closure.
- the reactor body 1 and the lid 2 each have a shoulder or flange (15 and 16, respectively) so that clamp 3 can push the reactor body and lid toward one another and against gasket 4 to seal the reactor's chamber 17 from its ambient during use.
- the clamp is typically split into two or three sections, and each section is connected with bolts.
- the number of bolts is preferably at least 2 for each joint, i.e. if the clamp is split into three sections, a total of 6 or more bolts is preferably used. When the bolts are tightened, gaps between the clamp sections are narrowed so that the diameter of the clamp reduces.
- the reactor body shoulder 15, lid shoulder 16, and inner contacting surfaces of the clamp 3 that contact the reactor body shoulder and lid shoulder are preferably tapered, so that the clamp presses upon and squeezes the reactor body shoulder and lid shoulder together as the clamp is tightened and the clamp diameter decreases.
- the tapered shoulders on the reactor body and lid and the tapered, contacting inner surfaces of the clamp transfer the radial force to vertical force so that the gasket is compressed.
- the angle of taper is selected to provide the compressive force needed to draw the reactor body and lid together and compress the gasket a sufficient amount to fully close the reactor, so that the contents of the reactor do not leak from within it during operation.
- hydraulic wrenches are preferably used.
- the chamber 17 of the high-pressure reactor 1 is divided into at least two regions with baffles 7.
- a source material called nutrient 9 is held in a nutrient basket 8 located in the upper dissolution region. Seed crystals 10 are located in the lower crystallization region.
- the high-pressure reactor is heated with external heaters 5 and 6.
- the heater temperature is controlled from the outside of the containment cell.
- Ammonia within the reactor's chamber can be released to the exhaust line 13 by opening the exhaust valve 12 from outside of the containment cell 1 1 via a valve operation device 14.
- the valve operation device can utilize mechanical means, pneumatic means, or electromagnetic means.
- the gasket of this invention is intended to be used many times, at least 10 times.
- the high-pressure reactor in the present invention utilizes a Ni-based gasket having moderate strength.
- the typical ultimate tensile strength of the precipitation hardenable Ni- Cr superalloy used to make the reactor body, lid, and/or clamps is more than 150 ksi at room temperature.
- the ultimate tensile strength of the gasket material is within the range of 50-100 ksi at room temperature. This value is higher than the tensile strength of copper alone (30-50 ksi at room temperature), which is more commonly used as a gasket material.
- the Ni-based gasket has a Ni content greater than that of the reactor material or preferably greater than 90%, more preferably at least 99%.
- the copper content of the gasket is preferably 10% or less, preferably less than 1%, more preferably less than 0.5%, and in some embodiments, less than 0.3% or less than or equal to about 0.25%.
- Ni alloy 200 is one example of a material that can be used to form a gasket. Ni alloy 200 has a nickel content of 99.0% or more and copper content of 0.25% or less.
- the gasket can be used repeatedly for at least 10 times by maintaining the thinnest part of the gasket 4 to be greater than 0.2 inch thick and having the gasket 4 tapered along its radial direction.
- the gasket surface is compressed at 60,000 psi or higher in order to hold an operating pressure of over 25,000 psi at a temperature greater than 450 °C.
- the compression force to seal the surfaces of reactor lid and body to the gasket can be attained by utilizing a clamp 3, or other mechanisms such as a screw lid in which a lid is clamped to a reactor body by screws passing through the lid and engaging with threads in the body.
- the high compression force can be obtained by using hydraulic wrench.
- a gasket that tapers from its thicker point along the inner circumference or radius of the gasket towards a thinner point at or near the outer circumference or radius allows part of the compression force to be applied towards outer radial direction, enabling self-sealing of the mating surface between the gasket and the reactor body, and between the gasket and the lid.
- the gasket preferably does not have a knife edge design because an indentation caused by the knife edge becomes a leak path during the next use of the gasket.
- a knife edge-type gasket is typically for one time use.
- a high-pressure gasket for an ammonothermal reactor is designed for one-time use because of extremely high
- the gasket changes its shape to fit the sealing surface of the high-pressure reactor body and the lid, thus sealing the high-pressure fluid well.
- the gasket deforms too much, it can only be used for one time because it loses the original shape.
- the gasket material has higher Ni concentration than the material of the high-pressure reactor and/or lid.
- the high-pressure reactor and/or lid is typically constructed with precipitation hardenable Ni-Cr superalloys such as R-41, 1-720, 1-718, 1-706 and/or Waspalloy.
- the typical Ni content of R41, 1-720, 1-718, 1-706 and Waspalloy is 54%, 57%, 53%, 42% and 58%, respectively. Therefore, the gasket's Ni concentration is higher than these values, or preferably higher than 90%, more preferably at least 99%.
- the material for the high-pressure reactor and the material for the lid are different.
- the Ni content of the gasket is higher than the maximum Ni content of either the reactor body or lid.
- the copper content is preferably less than 10%, and more preferably no more than 1%.
- Elimination of copper from the gasket material is important for maintaining the ultimate tensile strength and corrosion resistance of the gasket needed for ammonothermal applications.
- the gasket Due to the high compression pressure, the gasket slightly deforms and becomes thinner.
- the thinnest part of the gasket 4 is preferably more than 0.2 inches.
- the thinnest part of the gasket is defined as the minimum distance from one side to the other side of the disk-shaped gasket. As explained in the Examples below, we discovered that this minimum thickness is needed for repeated and reliable use of the gasket. When the gasket is too thick, however, the gasket may rupture outward due to internal pressure.
- gasket thickness is preferably greater than or equal to about 0.2 inches and less than or equal to about 1 inch, more preferably greater than or equal to about 0.2 inches and less than or equal to about 0.5 inch, and in another embodiment, gasket thickness is as close to the minimum thickness as practical.
- Figure 2 shows one example of the gasket.
- the top view of the gasket 21 shows how the gasket has an annular shape with inner circumference or radius at inner edge 23 and outer circumference or radius at outer edge 24.
- the gasket is tapered from the gasket's inner radius or circumference and toward the outer radial direction.
- the taper is on a gasket surface that engages the reactor body.
- the angle of taper as measured to a horizontal line drawn through the horizontal gasket is between 10 degrees and 23 degrees for the gasket depicted in Figure 2, and the taper angle is preferably between 15 degrees and 20 degrees.
- a conventional gasket for a high-pressure reactor has either no taper angle (0 degrees) on either surface or a high taper angle (over 23 degrees) on at least one surface, as disclosed in United States Patent No. 8,871,024, United States Patent No. 8,236,237 or Japanese Patent Application publication number JP2006-193355 (also published as US2009013926), the gaskets designed for these high-pressure reactors are not suitable for repeated use due to too much deformation of the gasket.
- the thinnest part of the gasket is the outer most thickness of the gasket.
- Figure 3 shows a few examples of various designs with location of thinnest part and taper angle measurement.
- the gasket can have taper on both surfaces as shown in Figure 3 (gasket 32).
- each taper can be same (i.e. symmetrical) or different (asymmetrical).
- the taper angle to the horizontal line is between 10 degrees and 23 degrees, preferably between 15 degrees and 20 degrees, for either or both surfaces.
- the gasket can have a second and optionally a third taper angle in addition to the primary taper angle as shown in Figure 3 (see gaskets 33, 34, 35 and 36). These second and third tapers have an effect of reducing crack formation due to gasket deformation. If the second taper is on the inner edge, the taper angle is preferably larger than that of the first taper angle. If the second taper is on the outer edge, the taper angle is preferably smaller than that of the first taper angle.
- the gasket can optionally have both inner and outer tapers in addition to the primary gasket taper.
- gasket 36 has a second taper angle on the outer edge which acts as an alignment guide so that the gasket is aligned easily to the high-pressure reactor body or lid.
- the thinnest part does not correspond to the outer most point.
- the alignment guide can be located at the inner edge. In either case, the alignment guide is characterized as a bump along the outer circumference of the gasket.
- a cylindrical high-pressure reactor having inner diameter more than 2", made of precipitation hardenable Ni-Cr superalloy has a cylindrical reactor body that is open on both ends.
- the lids for each end are made of another type of precipitation hardenable Ni-Cr superalloy.
- the gasket is made of Ni-based alloy having Ni content higher than 99%.
- the gasket material contains up to 1% of copper.
- the gasket had second and third taper angles in addition to the primary taper angle (Fig. 3 gasket 35).
- the primary taper angle was 18 degrees
- the inner taper at the gasket's inner circumference was 8 degrees
- the outer taper at the gasket's outer circumference was 31.31 degrees.
- the thickness at the thinnest part (at the gasket's outer edge) was 0.195".
- Two gaskets were used to seal the lids, one on each end. Before closing the lid, water was added to conduct a pressurization test with water.
- the gasket compression pressure was estimated to be 58,520 psi. With this setting, the vapor leaked out from the gasket when the reactor was heated to 600 °C and was self-pressurized at about 21,000 psi.
- the gasket compression pressure was estimated to be 63, 151 psi. With this setting, the reactor held the pressure of 34,000 psi when the reactor was heated to 600 °C.
- the same high-pressure reactor and lids were used to grow GaN crystals.
- the gaskets had the same taper angles as the gaskets in Example 1 and Example 2.
- the minimum thickness was 0.255" and was located at the outer edge of the gaskets.
- a high-pressure reactor of this invention comprises a high-pressure reactor and lid(s) made of precipitation hardenable Ni-Cr superalloy and gasket of which ultimate tensile strength is preferably in the range of 50-100 ksi.
- the Ni content of the gasket is greater than the Ni content of the precipitation harden able Ni-Cr superalloy, or preferably greater than 90% or more and, more preferably, greater than 99%. Greater Ni content makes the gasket soft enough to ensure reliable seal of the lid(s).
- using a Ni or Ni- based alloy with less than 1% copper makes the gasket hard enough for repeated use. Due to the high-compression pressure needed to seal the lid, the gasket deforms and becomes thinner during use.
- the gasket of the current invention can avoid leakage even after thinning occurs due to gasket compression.
- An advantage of this invention is extended lifetime of the gasket and optionally a reduction of tightening torque needed to reliably seal the lid and reactor body. All of these advantage contributes to lower cost manufacturing of metal nitride materials by the ammonothermal process.
- gasket having Ni content higher than 90% the same benefits can be expected as long as the Ni content is higher than that of the precipitation hardenable Ni-Cr superalloy used to construct the reactor body and/or lid.
- the compression pressure needed to effectively seal the reactor during use would be higher due to the gasket's greater hardness.
- the preferred embodiment describes gaskets of a certain design, the same benefits can be expected with different design as long as (a) the gasket is tapered down from the inner radius or circumference in a radial direction toward the outer radius or circumference of the gasket, (b) the thinnest part of the gasket is more than 0.2", and/or (c) the primary taper angle of the gasket to the horizontal plane is between 1 and 45 degrees. Also, the gasket may not have a second or third taper.
- a transition metal nitride may be formed using a method as disclosed in e.g. U.S. Pat. No. 8,920,762 (entitled “Synthesis Method Of Transition Metal Nitride And Transition Metal Nitride”) or in U.S. Pat. No. 8,971,018 (entitled “Ultracapacitors Using Transition Metal Nitride-Containing Electrode And Transition Metal Nitride”), each of which is incorporated by reference herein as if put forth in full below. References
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201461973359P | 2014-04-01 | 2014-04-01 | |
PCT/US2015/023843 WO2015153737A1 (en) | 2014-04-01 | 2015-04-01 | High pressure reactor for supercritical ammonia and method for producing crystalline group iii nitride |
Publications (1)
Publication Number | Publication Date |
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EP3126548A1 true EP3126548A1 (en) | 2017-02-08 |
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Family Applications (1)
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EP15715951.8A Withdrawn EP3126548A1 (en) | 2014-04-01 | 2015-04-01 | High pressure reactor for supercritical ammonia and method for producing crystalline group iii nitride |
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EP (1) | EP3126548A1 (en) |
WO (1) | WO2015153737A1 (en) |
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IT201900008556A1 (en) * | 2019-06-10 | 2020-12-10 | Levati Food Tech S R L | PRODUCT HEAT TREATMENT APPARATUS |
Family Cites Families (5)
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JP4498661B2 (en) * | 2001-07-11 | 2010-07-07 | 株式会社バックス・エスイーブイ | Metal gasket for vacuum apparatus and method for manufacturing the same |
TWI460323B (en) * | 2008-06-04 | 2014-11-11 | Sixpoint Materials Inc | High-pressure vessel for growing group iii nitride crystals and method of growing group iii nitride crystals using high-pressure vessel and group iii nitride crystal |
KR20120127397A (en) * | 2009-11-27 | 2012-11-21 | 미쓰비시 가가꾸 가부시키가이샤 | Method for producing nitride crystals, and production vessel and members |
WO2011152332A1 (en) * | 2010-06-03 | 2011-12-08 | 株式会社フルヤ金属 | Gasket for pressure vessel, and method for producing said gasket |
EP2725123A4 (en) * | 2011-06-23 | 2014-07-30 | Asahi Chemical Ind | Method for producing nitride single crystal and autoclave used therefor |
-
2015
- 2015-04-01 WO PCT/US2015/023843 patent/WO2015153737A1/en active Application Filing
- 2015-04-01 EP EP15715951.8A patent/EP3126548A1/en not_active Withdrawn
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