CN114849590A - Hot isostatic pressing ammonothermal method reation kettle - Google Patents
Hot isostatic pressing ammonothermal method reation kettle Download PDFInfo
- Publication number
- CN114849590A CN114849590A CN202210740531.9A CN202210740531A CN114849590A CN 114849590 A CN114849590 A CN 114849590A CN 202210740531 A CN202210740531 A CN 202210740531A CN 114849590 A CN114849590 A CN 114849590A
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- kettle
- lining
- subassembly
- hot isostatic
- kettle body
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- 238000001513 hot isostatic pressing Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title description 8
- 238000007789 sealing Methods 0.000 claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 238000003466 welding Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000005242 forging Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000009529 body temperature measurement Methods 0.000 claims description 2
- 238000009434 installation Methods 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 125000003003 spiro group Chemical group 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 8
- 229910002601 GaN Inorganic materials 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Images
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
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a hot isostatic pressing ammonothermal reaction kettle, which comprises a kettle body assembly, a kettle cover assembly and a clamp (3), wherein the kettle cover assembly is arranged on the upper end surface of the kettle body assembly, a reaction chamber is arranged in the kettle body assembly, a sealing ring (4) is arranged between the contact surface of the upper end surface of the kettle body assembly and the lower end surface of the kettle cover assembly, the kettle body assembly and the kettle cover assembly are fixedly connected through the clamp (3) arranged in the circumferential direction and generate sealing pretightening force, the kettle cover assembly is provided with an air inlet which is used for filling ammonia and penetrates through the reaction chamber of the kettle body assembly, and the kettle cover assembly, the kettle body assembly, the sealing ring (4) and the clamp (3) are made of nickel-based alloy materials.
Description
Technical Field
The invention relates to a reaction kettle, in particular to a reaction kettle for preparing a gallium nitride single crystal material by a hot isostatic pressing ammonothermal method.
Background
Gallium nitride (GaN) as one of the third generation wide bandgap semiconductor core materials has the excellent characteristics of high breakdown field strength, high saturated electron drift rate, strong radiation resistance, good chemical stability and the like, and is an ideal material for manufacturing wide spectrum, high power and high efficiency photoelectrons, power electronics and microelectronics. The ammonothermal method is a method for culturing crystal from supersaturated critical ammonia at high temperature and high pressure, the ammonothermal method is used for preparing gallium nitride single crystal material, the reaction kettle is divided into a dissolving area for culturing gallium nitride raw material and a crystallization area for suspending gallium nitride seed crystal, ammonia gas and mineralizer for assisting raw material dissolution are filled in the kettle, convection is generated due to temperature difference between the crystallization area and the dissolving area, saturated solution in the dissolving area is brought to the crystallization area to form supersaturated precipitated solute, and the seed crystal grows. The solution with reduced solubility and separated partial solute flows to the dissolving zone to dissolve the culture material, and the above steps are repeated to make the seed crystal grow continuously. The reaction kettle is arranged in the hot isostatic pressing machine, the temperature difference is generated in the reaction kettle by utilizing the temperature difference characteristic of a growth furnace designed in the hot isostatic pressing machine, two high-temperature and low-temperature regions, namely a crystallization region and a dissolution region, are formed in the reaction kettle, and gallium nitride generates crystallization due to the difference of the solubility in the reaction kettle, so that the method is a process application of the hot isostatic pressing machine. A reaction kettle generally used for growing gallium nitride comprises a kettle body assembly and a kettle cover assembly which is hermetically connected with the kettle body assembly. Although the hot isostatic pressing ammonothermal reaction kettle contains alkaline substances such as ammonia and an acidic mineralizer inside and outside and 8OMPa axial and radial high-pressure gas, the pressure difference in the hot isostatic pressing machine is not about 20MPa or is more similar, so the sealing structure and the pressure structure of the reaction kettle are different from those of the traditional reaction kettle, and therefore, the hot isostatic pressing ammonothermal reaction kettle which can bear high pressure and resist corrosion and has a relatively simple structure and high-temperature mechanical property needs to be newly designed.
Disclosure of Invention
The invention aims to provide a hot isostatic pressing ammonothermal reaction kettle which can bear high pressure and resist corrosion, has a relatively simple structure and high-temperature mechanical property.
The invention is realized by the following technical scheme: a hot isostatic pressing ammonothermal reaction kettle is characterized in that: including cauldron body subassembly, kettle cover subassembly and clamp, kettle cover subassembly set up cauldron body subassembly up end, cauldron body subassembly inside open and to have reaction chamber, cauldron body subassembly up end with kettle cover subassembly under the contact surface of terminal surface between be provided with the sealing washer, cauldron body subassembly with kettle cover subassembly through the clamp fastening connection that circumference set up and produce sealed pretightning force, kettle cover subassembly open and to have the link up that is used for filling the ammonia cauldron body subassembly reaction chamber's air inlet, cauldron cover subassembly cauldron body subassembly the sealing washer with the clamp adopt nickel base alloy material to make.
Further, the kettle cover assembly comprises an end cover and an upper inner lining, the end cover is a cylinder with a flange arranged at the lower part, an inner concave cavity is formed in the bottom surface of the end cover, an acid gas in the end cover and the kettle body assembly is isolated and sealed by the inner concave cavity, an air inlet for filling ammonia gas is formed in the top surface of the end cover, the air inlet penetrates through the end cover and the upper inner lining, the air inlet is connected with an ultrahigh pressure connector in threaded connection with a connecting pipe for filling ammonia gas, and a sealing groove for installing a sealing ring is formed in the lower end surface of the upper inner lining.
Further, cauldron body subassembly include the cauldron body, lower inside lining ring cover, bush subassembly, spherical base and low head, the cauldron body be the tubbiness body of upper end area flange, cauldron body up end open and to have the cavity, lower inside lining ring cover adorn admittedly through the screw in the cavity, lower inside lining ring up end be provided with the concave groove of the sealed recess cooperation installation sealing washer of the last inside lining of end cover, the tubbiness body of the cauldron body in set up the bush subassembly, the upper end of bush subassembly with the lower extreme welding of lower inside lining ring cover link firmly, the inside reaction chamber that has opened of bush subassembly, bush subassembly lower extreme with spherical base's upper end contact, spherical base's lower extreme with low head upper end contact, the low head spiro union be in the cauldron internal.
Further, the length-diameter ratio of the kettle body is 12: 1, adopting integral forging to manufacture.
Furthermore, a plurality of measuring holes for thermocouple temperature measurement are opened on the outer surface of the kettle body.
Further, the lining assembly comprises a lining barrel and a supporting barrel, wherein the inner wall of the lining barrel forms the reaction chamber, the lining barrel is made of silver, the lining barrel is arranged in the supporting barrel, and the lining barrel is connected with the supporting barrel through a pure silver material filled with holes.
Further, the spherical base with the low head between set up the snap ring platform, spherical base upper surface with support barrel bottom laminating, the spherical base in the middle of open and to have the through-hole, the snap ring platform in the middle of open and to have the through-hole, the low head set up zigzag external screw thread section, cauldron body lower part make zigzag internal thread section, the low head with the cauldron body pass through zigzag threaded connection.
Further, the clamp is a pair of opposite semicircular arches, the inner surfaces of the pair of opposite arches are provided with circumferential grooves, the circumferential grooves are buckled on the end cover and the flange of the kettle body, the pair of opposite arches are provided with bolt through holes which are opposite to each other, and the pair of opposite arches are fastened and connected through tightening bolts and nuts which are arranged in the bolt through holes.
Compared with the prior art, the invention has the following advantages and beneficial effects: according to the hot isostatic pressing ammonothermal reaction kettle, the strength structure part comprises the end cover, the sealing ring, the hoop and the kettle body, the sealing structure part comprises the upper inner lining sleeve, the sealing ring and the lower inner lining sleeve, and stable fastening force and sealing pretightening force are applied through the hoop to realize fastening and sealing connection; the bushing assembly, the spherical base, the clamping ring table and the lower end socket bear axial pressure through the zigzag threads, so that the high-pressure and corrosion-resistant bushing assembly can bear high pressure and is simple in structure and has high-temperature mechanical properties.
Drawings
FIG. 1 is a schematic diagram of a hot isostatic pressing ammonothermal reactor of the present invention.
FIG. 2 is a schematic view of a hot isostatic pressing ammonothermal reactor lid assembly of the present invention.
FIG. 3 is a schematic structural view of a hot isostatic pressing ammonothermal reactor vessel assembly of the present invention.
FIG. 4 is a perspective view of a hot isostatic pressing ammonothermal reactor band of the present invention.
In the figure, 1, an end cover, 2, a kettle body, 3, a clamp, 4, a sealing ring, 11, an upper inner lining, 12, a connecting pipe, 13, an ultrahigh pressure joint, 21, a lower inner lining ring sleeve, 22, a lining component, 23, a spherical base, 24, a clamping ring table, 25, a lower end cover, 31, a bolt through hole, 201, a lining barrel and 202, a supporting barrel are arranged.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Fig. 1 to 4 show a hot isostatic pressing ammonothermal reactor of the present invention, characterized in that: including cauldron body subassembly, kettle cover subassembly and clamp 3, the kettle cover subassembly set up cauldron body subassembly up end, cauldron body subassembly inside open and to have reaction chamber, cauldron body subassembly up end with the kettle cover subassembly under the contact surface of terminal surface between be provided with sealing washer 4, cauldron body subassembly with the kettle cover subassembly through 3 fastening connection of clamp that circumference set up and produce sealed pretightning force, make sealing washer 4 seal up inside and outside gas, kettle cover subassembly open and to have the link up that is used for filling the ammonia cauldron body subassembly reaction chamber's air inlet, kettle cover subassembly cauldron body subassembly sealing washer 4 with 3 adoption nickel base alloy materials of clamp make.
The kettle cover assembly comprises an end cover 1 and an upper inner bushing 11, wherein the end cover 1 is a cylinder with a flange arranged at the lower part, an inner concave cavity is formed in the bottom surface of the end cover 1, the upper inner bushing 11 used for isolating and sealing acid gas in the end cover 1 and the kettle body assembly is fixedly arranged in the inner concave cavity, an air inlet used for filling ammonia gas is formed in the top surface of the end cover 1, the air inlet penetrates through the end cover 1 and the upper inner bushing 11, the air inlet is in threaded connection with an ultrahigh pressure joint 12 connected with a connecting pipe 12 filled with ammonia gas, a sealing groove for mounting the sealing ring 4 is formed in the lower end surface of the upper inner bushing 11, the end cover 1 is made of nickel-based alloy GH4169, the upper inner bushing 11 is made of nickel-based alloy 706, and a silver coating or silver spraying coating is arranged on the surface of the nickel-based alloy 706, so that the acid resistance and the corrosion resistance are achieved, Corrosion of alkaline materials.
The kettle body assembly is used for installing gallium nitride raw materials, mineralizer and filling liquid ammonia, the kettle body assembly comprises a kettle body 2, a lower lining ring sleeve 21, a lining assembly 22, a spherical base 23 and a lower end enclosure 25, the kettle body 2 is a cylindrical body with a flange at the upper end, a concave cavity is arranged on the upper end surface of the kettle body 2, the lower lining ring sleeve 21 is fixedly arranged in the concave cavity through a screw, the upper end surface of the lower lining ring sleeve 21 is provided with a concave ring groove which is matched with the sealing groove of the upper lining sleeve 11 of the end cover 1 and is provided with a sealing ring 4, the bushing component 22 is arranged in the cylindrical body of the kettle body 2, the upper end of the bushing component 22 is fixedly connected with the lower end of the lower lining ring sleeve 21 in a welding way, thus, when the reaction kettle fails due to the damage of the lining assembly 22, only the lining assembly 22 can be replaced, and the structure of the kettle body 2 is not influenced; the reactor is characterized in that a reaction chamber is formed in the lining component 22, the lower end of the lining component 22 is in contact with the upper end of the spherical base 23, the lower end of the spherical base 23 is in contact with the upper end of the lower end socket 25, the lower end socket 25 is screwed in the kettle body 2, the kettle body 2 is made of GH4169 material, the lower lining ring sleeve 21 is made of GH4169 material, and the surface of the lower lining ring sleeve is plated with silver.
The length-diameter ratio of the kettle body 2 is 12: 1, is made by integral forging, thus, the strength of the kettle body 2 can meet the requirements of working conditions at high temperature and high pressure (650 ℃, 80 MPa) and low temperature of minus 50 ℃, and can bear axial tension and radial force.
The outer surface of the kettle body 2 is provided with a plurality of measuring holes for measuring the temperature of the thermocouple, so that the temperature of the kettle body 2 can be monitored in real time to judge the temperature condition in the kettle body 2.
The liner assembly 22 comprises a liner barrel 201 and a support barrel 202, the inner wall of the liner barrel 201 forms the reaction chamber, the liner barrel 201 is made of silver, the liner barrel 201 is arranged in the support barrel 202, and the liner barrel 201 and the support barrel 202 are connected by adopting a pure silver material for hole filling welding, so that the liner barrel 201 cannot be compressed by atmospheric pressure when vacuum is pumped; the lining barrel 201 made of silver mainly plays a role in isolating substances in the kettle body 2, and the corrosion margin is zero. The silver material of the lining barrel 201 has certain extensibility, so that the structure and the shape of the lining barrel 201 have self-adaptive function when the lining barrel is under high pressure or high temperature, and the lining barrel 201 cannot deform to cause failure and fracture to cause gas leakage; the supporting barrel 202 is made of GH4169 nickel-based alloy, has certain rigidity and strength at high temperature and high pressure, and plays a role in supporting the lining barrel 201.
A snap ring table 24 bearing axial force is arranged between the spherical base 23 and the lower end enclosure 25, the bottom of the support barrel 202 is semicircular, the upper surface of the spherical base is attached to the bottom of the support barrel 202, local stress is not generated under the conditions of high temperature and high pressure, the support barrel 202 is only under the action of compressive stress, and the support barrel 202 cannot crack under the condition of the compressive stress; the device is characterized in that the clamp ring table 24 is provided with a step outer edge, the clamp ring table 24 is arranged on the step in the kettle body 2 cylinder and used for blocking components such as the spherical base 23 on the clamp ring table 24 from falling down, a through hole is formed in the middle of the spherical base 23, a through hole is formed in the middle of the clamp ring table 24, the lower seal head 25 is convenient to detach and check whether a leakage phenomenon occurs or not during maintenance, the lower seal head 25 is provided with a saw-toothed external thread section, a saw-toothed internal thread section is formed in the lower portion of the kettle body 2, the lower seal head 25 is connected with the kettle body 2 through saw-toothed threads, the saw-toothed threads can bear axial tension generated by internal pressure, the spherical base 23, the clamp ring table 24 and the lower seal head 25 are all in a hot area but are not in contact with a medium in a reaction chamber, and therefore GH4169 nickel-based alloy material is adopted.
The clamp 3 is a pair of opposite semicircular arches, the inner surfaces of the pair of opposite arches are provided with circumferential grooves which are buckled on the end cover 1 and the flange of the kettle body 2, the pair of opposite arches are provided with bolt through holes 31 which are opposite to each other, and the pair of opposite arches are fastened and connected through tightening bolts and nuts which are arranged in the bolt through holes 21. Therefore, screw through holes and threaded holes are not required to be formed in the end cover 1 and the kettle body 2, the size of the end cover 1 and the kettle body 2 is reduced, the structure of the kettle body 2 is simplified, and integral forging is facilitated.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (8)
1. A hot isostatic pressing ammonothermal reaction kettle is characterized in that: including cauldron body subassembly, kettle cover subassembly and clamp (3), the kettle cover subassembly set up cauldron body subassembly up end, cauldron body subassembly inside open and to have reaction chamber, cauldron body subassembly up end with the kettle cover subassembly under the contact surface of terminal surface between be provided with sealing washer (4), cauldron body subassembly with the kettle cover subassembly through clamp (3) fastening connection and the sealed pretightning force of production that circumference set up, the kettle cover subassembly open and to have the link up that is used for filling the ammonia cauldron body subassembly reaction chamber's air inlet, the kettle cover subassembly cauldron body subassembly sealing washer (4) with clamp (3) adopt nickel base alloy material to make.
2. The hot isostatic ammonothermal reactor of claim 1, wherein: kettle cover subassembly, including end cover (1) and last inside bush (11), end cover (1) be the cylinder that the lower part is provided with the bead, end cover (1) bottom surface open and to have interior concave cavity, interior concave cavity internal stability be equipped with be used for with end cover (1) with kettle body subassembly in acid gas keep apart and sealed last inside bush (11), end cover (1) top surface open and to have the air inlet that is used for filling the ammonia, the air inlet link up end cover (1) with last inside bush (11), the air inlet and ultrahigh pressure joint (13) spiro union that connecting pipe (12) that fill the ammonia are connected, last inside bush (11) lower terminal surface be provided with the installation the sealed recess of sealing washer (4).
3. The hot isostatic ammonothermal reactor of claim 2, wherein: the kettle body assembly comprises a kettle body (2), a lower lining ring sleeve (21), a lining assembly (22), a spherical base (23) and a lower end socket (25), wherein the kettle body (2) is a cylindrical body with a flange at the upper end, the upper end face of the kettle body (2) is provided with a concave cavity, the lower lining ring sleeve (21) is fixedly arranged in the concave cavity through a screw, the upper end face of the lower lining ring sleeve (21) is provided with a concave ring groove matched with a sealing groove of an upper lining sleeve (11) of the end cover (1) to install a sealing ring (4), the cylindrical body of the kettle body (2) is internally provided with the lining assembly (22), the upper end of the lining assembly (22) is fixedly connected with the lower end of the lower lining ring sleeve (21) in a welding way, a reaction chamber is arranged inside the lining assembly (22), the lower end of the lining assembly (22) is contacted with the upper end of the spherical base (23), the lower end of the spherical base (23) is in contact with the upper end of the lower seal head (25), and the lower seal head (25) is screwed in the kettle body (2).
4. A hot isostatic ammonothermal reactor according to any one of claims 1 to 3, wherein: the length-diameter ratio of the kettle body (2) is 12: 1, adopting integral forging to manufacture.
5. The hot isostatic ammonothermal reactor of claim 4, wherein: the outer surface of the kettle body (2) is provided with a plurality of measuring holes for thermocouple temperature measurement.
6. The hot isostatic ammonothermal reactor of claim 5, wherein: the lining assembly (22) comprises a lining barrel (201) and a supporting barrel (202), wherein the inner wall of the lining barrel (201) forms the reaction chamber, the lining barrel (201) is made of silver, the lining barrel (201) is arranged in the supporting barrel (202), and the lining barrel (201) and the supporting barrel (202) are connected by adopting a hole filling welding pure silver material.
7. The hot isostatic ammonothermal reactor of claim 6, wherein: spherical base (23) with low head (25) between set up snap ring platform (24), spherical base (23) upper surface with support bucket (202) bottom laminating, spherical base (23) in the middle of open and to have the through-hole, snap ring platform (24) in the middle of open and to have the through-hole, low head (25) set up zigzag external screw thread section, cauldron body (2) lower part make zigzag internal thread section, low head (25) with cauldron body (2) through zigzag threaded connection.
8. The hot isostatic ammonothermal reactor of claim 7, wherein: the clamp (3) is a pair of opposite semicircular arches, the inner surfaces of the pair of opposite arches are provided with circumferential grooves, the circumferential grooves are buckled on the end cover (1) and the flange of the kettle body (2), the pair of opposite arches are provided with bolt through holes (31) which are opposite to each other, and the pair of opposite arches are fastened and connected through tightening bolts and nuts arranged in the bolt through holes (31).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210740531.9A CN114849590A (en) | 2022-06-28 | 2022-06-28 | Hot isostatic pressing ammonothermal method reation kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210740531.9A CN114849590A (en) | 2022-06-28 | 2022-06-28 | Hot isostatic pressing ammonothermal method reation kettle |
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| Publication Number | Publication Date |
|---|---|
| CN114849590A true CN114849590A (en) | 2022-08-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210740531.9A Pending CN114849590A (en) | 2022-06-28 | 2022-06-28 | Hot isostatic pressing ammonothermal method reation kettle |
Country Status (1)
| Country | Link |
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| CN (1) | CN114849590A (en) |
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-
2022
- 2022-06-28 CN CN202210740531.9A patent/CN114849590A/en active Pending
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