CN220079179U - High temperature and high pressure resistant sealed crucible assembly - Google Patents
High temperature and high pressure resistant sealed crucible assembly Download PDFInfo
- Publication number
- CN220079179U CN220079179U CN202321225983.XU CN202321225983U CN220079179U CN 220079179 U CN220079179 U CN 220079179U CN 202321225983 U CN202321225983 U CN 202321225983U CN 220079179 U CN220079179 U CN 220079179U
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- China
- Prior art keywords
- crucible
- glove box
- joint
- pipeline
- furnace body
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000003860 storage Methods 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 11
- 239000010959 steel Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 238000012544 monitoring process Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 10
- 229910002601 GaN Inorganic materials 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052733 gallium Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- -1 oxides Chemical class 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical group 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model discloses a high-temperature and high-pressure resistant sealed crucible assembly, which relates to the technical field of semiconductor material preparation. Wherein the sealed crucible is arranged in the heating cavity; a reaction chamber is formed in the sealed crucible. The liquid storage tank is arranged in the glove box and is positioned outside the furnace body, and the inlet of the liquid storage tank is communicated with the reaction cavity. The four-way connecting piece is arranged in the glove box and is positioned outside the furnace body, the four-way connecting piece is provided with a first joint, a second joint and a third joint, and the outlet of the liquid storage tank is communicated with the first joint of the four-way connecting piece; the second joint is communicated with the exhaust pipe; the third joint is communicated with a gas storage steel cylinder, and nitrogen is arranged in the gas storage steel cylinder. The method is used for preparing the semiconductor material.
Description
Technical Field
The utility model relates to the technical field of semiconductor material preparation, in particular to a high-temperature and high-pressure resistant sealing crucible assembly.
Background
CVD is a short term of Chemical Vapor Deposition and refers to a method of separating out inorganic materials such as metals, oxides, and carbides by gas phase reaction at high temperature, for example, thermal decomposition of metal halides, organic metals, hydrocarbons, and the like, hydrogen reduction, or chemical reaction of a mixed gas thereof at high temperature.
In the process of manufacturing gallium nitride, a graphite heat-insulating layer is arranged in a reaction container, if nitrogen is directly introduced into the reaction container, the reacted gallium nitride generates impurities which are unfavorable for subsequent use, therefore, the utility model provides the high-temperature and high-pressure resistant sealed crucible which is placed in the reaction container and is completely isolated from the graphite heat-insulating layer, so that nitrogen and gallium sodium mixed solution react in the crucible, and the purity of gallium nitride is further ensured.
Disclosure of Invention
The embodiment of the utility model provides a high-temperature and high-pressure resistant sealed crucible assembly, which ensures that the reaction is carried out in a crucible by arranging a sealed crucible in a reaction container, thereby ensuring the purity of gallium nitride.
In order to achieve the above purpose, the embodiment of the present utility model adopts the following technical scheme:
the embodiment of the utility model provides a high-temperature and high-pressure resistant sealed crucible assembly, which is partially positioned in a glove box, wherein a furnace body is arranged in the glove box, the furnace body is provided with a heating cavity, and the high-temperature and high-pressure resistant sealed crucible assembly comprises:
the sealed crucible is arranged in the heating cavity; a reaction cavity is formed in the sealed crucible;
the liquid storage tank is arranged in the glove box and is positioned outside the furnace body, and the inlet of the liquid storage tank is communicated with the reaction cavity;
the four-way connecting piece is arranged in the glove box and is positioned outside the furnace body, the four-way connecting piece is provided with a first joint, a second joint and a third joint, and the outlet of the liquid storage tank is communicated with the first joint of the four-way connecting piece; the second joint is communicated with the exhaust pipe; the third joint is communicated with a gas storage steel cylinder, and nitrogen is arranged in the gas storage steel cylinder.
Further, the sealed crucible includes:
the crucible comprises a crucible body, wherein a crucible groove is formed above the crucible body;
the crucible cap is covered on the crucible groove;
the octagonal pad is arranged between the crucible cap and the wall of the crucible groove;
the liquid storage tank passes through the crucible cap through a pipeline to be communicated with the reaction cavity.
Further, the wall of the crucible groove is provided with a flange;
the sealed crucible further comprises:
a plurality of screws, one end of which passes through the crucible cap and the flange of the crucible groove;
and a plurality of hexagonal nuts, one of which is connected with one screw, so that the crucible cap is connected with the flange.
Further, the high temperature and high pressure resistant sealed crucible assembly further comprises:
the four-way connecting piece is provided with a fourth joint which is connected with the first pressure gauge and is used for monitoring the pressure in the reaction cavity;
further, the high temperature and high pressure resistant sealed crucible assembly further comprises:
the second pressure gauge is positioned outside the glove box and is arranged on a pipeline between the exhaust pipe and the glove box and used for monitoring pipeline pressure;
the needle valve is positioned outside the glove box and arranged on a pipeline between the exhaust pipe and the glove box and used for adjusting the flow of the pipeline.
Further, the high temperature and high pressure resistant sealed crucible assembly further comprises:
the stop valve is positioned in the glove box and outside the furnace body, is arranged on a pipeline connected with the second joint and is used for communicating or stopping the gas entering the exhaust pipe;
the one-way valve is positioned in the glove box and outside the furnace body, is arranged on a pipeline connected with the third joint and is used for enabling gas of the gas storage steel bottle to flow into the reaction cavity in a single way;
the air inlet valve is positioned outside the glove box and is arranged on an air outlet pipeline of the air storage steel cylinder.
Further, the high temperature and high pressure resistant sealed crucible assembly further comprises:
the ceramic insulating sleeve is connected between the liquid storage tank and the reaction cavity through a stainless steel pipe; the ceramic insulating sleeve is sleeved on a part of the stainless steel pipe.
In summary, due to the adoption of the technical scheme, the beneficial effects of the utility model are as follows:
in the utility model, the sealed crucible is of a sealed structure and can be isolated from the heating cavity of the reaction container, so that the reaction cavity in the sealed crucible is ensured to form a sealed reaction space, and impurities outside the sealed crucible are ensured not to enter the reaction cavity, thereby ensuring the purity of gallium nitride generated by reaction in the reaction cavity. The liquid storage tank can liquefy the gallium and sodium vapor overflowed into the pipeline at low temperature and store the gallium and sodium vapor at the bottom of the liquid storage tank. The glove box is isolated from the external environment, so that the purity of the reacted environment is higher. The ceramic insulating sleeve can isolate the stainless steel tube from the electrode in the furnace body, so that the safety is ensured. The pressure can be monitored through the first pressure gauge and the second pressure gauge, and the whole reaction can be ensured to be carried out through different valve controls.
Drawings
FIG. 1 is a schematic top view of a high temperature and high pressure resistant sealed crucible assembly, a furnace body and a glove box according to an embodiment of the present utility model;
FIG. 2 is a schematic view of a high temperature and high pressure resistant sealed crucible assembly and furnace provided by an embodiment of the present utility model;
FIG. 3 is an enlarged schematic view of the portion A in FIG. 2 according to an embodiment of the present utility model;
fig. 4 is a schematic view of a sealed crucible according to an embodiment of the present utility model.
Detailed Description
Embodiments of the present utility model will be described in detail below with reference to the accompanying drawings.
In the description of the present utility model, it should be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the utility model and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the utility model.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present utility model, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; the two components can be mechanically connected, can be directly connected or can be indirectly connected through an intermediate medium, and can be communicated with each other. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
As shown in fig. 1 to 4, the embodiment of the utility model provides a high temperature and high pressure resistant sealed crucible assembly, which is partially located in a glove box 100, the glove box 100 is internally provided with a furnace body 101, the furnace body 101 is provided with a heating cavity, and the high temperature and high pressure resistant sealed crucible assembly comprises a sealed crucible 201, a liquid storage tank 202 and a four-way connecting piece 203. Wherein the sealed crucible 201 is disposed within the heating chamber; a reaction chamber is formed in the sealed crucible 201. The liquid storage tank 202 is arranged in the glove box 100 and is positioned outside the furnace body 101, and the inlet of the liquid storage tank 202 is communicated with the reaction cavity. The four-way connecting piece 203 is arranged in the glove box 100 and is positioned outside the furnace body 101, the four-way connecting piece 203 is provided with a first joint 2031, a second joint 2032 and a third joint 2033, and the outlet of the liquid storage tank 202 is communicated with the first joint 2031 of the four-way connecting piece 203; the second joint 2032 communicates with the exhaust pipe 400; the third joint 2033 is in communication with the gas storage cylinder 300, and the gas storage cylinder 300 has nitrogen therein.
In this case, as shown in fig. 1 to 3, the four-way joint 203 can supplement nitrogen gas in the sealed crucible 201, and exhaust gas in the sealed crucible 201 can be discharged through the four-way joint 203. The glove box 100 can create a clean environment to prevent impurities in the air from entering the reaction chamber in the sealed crucible 201 to affect the purity of gallium nitride. In addition, the temperature of the liquid storage tank 202 is low, so that the gallium and sodium vapor overflowed into the pipeline can be liquefied at a low temperature and stored in the bottom of the tank.
In addition, metal Na is taken as a solvent, a GaN compound is taken as a solute, the metal Na and the GaN compound are put into a reaction cavity filled with nitrogen, heating is carried out under a certain pressure to a preset temperature range, the metal Na and the GaN compound are dissolved into an ionized intermediate compound, the temperature and the nitrogen pressure in the reaction cavity are controlled, and the ionized intermediate compound grows and is configured on a seed crystal to form a gallium nitride product.
In the following, for example, in some embodiments of the present utility model, the sealed crucible 201 may include a crucible body 2011, a crucible cap 2012 and an octagonal pad 2013, wherein the crucible body 2011 is formed with a crucible groove 20111 above, the crucible cap 2012 is disposed on the crucible groove 20111, and the octagonal pad 2013 is disposed between the crucible cap 2012 and the groove wall of the crucible groove 20111. Wherein the liquid storage tank 202 is communicated with the reaction cavity through a pipeline passing through the crucible cap 2012.
In this way, the gap between the crucible body 2011 and the crucible cap 2012 can be blocked by the octagonal pad 2013, so that the sealing performance of the reaction cavity formed between the crucible groove 20111 and the crucible cap 2012 is better, and impurities in the furnace body 101 are prevented from entering the reaction cavity.
Furthermore, in some embodiments of the utility model, as shown in fig. 4, the walls of the crucible groove 20111 have flanges 20112. Sealed crucible 201 further includes screws 2014, hex nuts 2015, wherein a plurality of screws 2014 pass through crucible cap 2012 and flange 20112 of crucible groove 20111 at one end. A hex nut 2015 is coupled to a screw 2014 to couple the crucible cap 2012 to a flange 20112. In this case, through the cooperation of the screw 2014 and the hexagonal nut 2015 and forming a certain extrusion to the octagonal mat 2013, the connection between the crucible cap 2012 and the crucible body 2011 is tighter, and the flange 20112 can enlarge the contact area with the crucible cap 2012, and can increase the space for accommodating the octagonal mat 2013.
Since nitrogen is required to be continuously charged into the reaction chamber during the reaction process, in order to prevent the pressure from being too high, in some embodiments of the present utility model, as shown in fig. 2 and 3, the high temperature and high pressure resistant sealed crucible assembly further includes a first pressure gauge 204 installed on the glove box 100, and the four-way connector 203 has a fourth connector 2034 connected to the first pressure gauge 204 for monitoring the pressure in the reaction chamber.
In addition, as shown in fig. 1, the high temperature and high pressure resistant sealed crucible assembly further includes: the second pressure gauge 205, which is located outside the glove box 100, is disposed on the pipeline between the exhaust pipe 400 and the glove box 100, and is used for monitoring the pipeline pressure.
In some embodiments of the present utility model, for convenience of user operation, the high temperature and high pressure resistant sealed crucible assembly may further include a plurality of valves, for example, as shown in fig. 1, a needle valve 210, which is located outside the glove box 100, is provided on a pipe between the offgas pipe 400 and the glove box 100, for adjusting a pipe flow. As shown in fig. 2 and 3, a shut-off valve 206, for example, is disposed inside the glove box 100 and outside the furnace body 101, and is mounted on a pipeline connected to the second joint 2032 for communicating or shutting off the gas entering the exhaust pipe 400. As shown in fig. 2 and 3, a check valve 207 is disposed inside the glove box 100 and outside the furnace body 101 and is installed on a pipeline connected to the third joint 2033, so that the gas in the gas storage steel bottle 300 can flow into the reaction chamber in a single way. As shown in fig. 2, an intake valve 208, for example, is located outside the glove box 100 and is mounted on the gas outlet line of the gas storage cylinder 300.
In other embodiments of the present utility model, as shown in fig. 2, the high temperature and high pressure resistant sealed crucible assembly further comprises a ceramic insulating sleeve 209, and the liquid storage tank 202 and the reaction chamber are connected through a stainless steel tube; the ceramic insulating sleeve 209 is sleeved on a part of the stainless steel tube. The ceramic insulating sleeve 209 can isolate the stainless steel tube from the electrode in the furnace body, thereby ensuring safety.
In the description of the present specification, a particular feature, structure, material, or characteristic may be combined in any suitable manner in one or more embodiments or examples.
The foregoing is merely illustrative of the present utility model, and the present utility model is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present utility model. Therefore, the protection scope of the present utility model shall be subject to the protection scope of the claims.
Claims (5)
1. The utility model provides a high temperature high pressure resistant sealed crucible subassembly which characterized in that, partly lie in the glove box, have the furnace body in the glove box, the furnace body has the heating chamber, high temperature high pressure resistant sealed crucible subassembly includes:
the sealed crucible is arranged in the heating cavity; a reaction cavity is formed in the sealed crucible;
the liquid storage tank is arranged in the glove box and is positioned outside the furnace body, and an inlet of the liquid storage tank is communicated with the reaction cavity;
the four-way connecting piece is arranged in the glove box and is positioned outside the furnace body, the four-way connecting piece is provided with a first joint, a second joint and a third joint, and the outlet of the liquid storage tank is communicated with the first joint of the four-way connecting piece; the second joint is communicated with the exhaust pipe; the third joint is communicated with a gas storage steel bottle, and nitrogen is arranged in the gas storage steel bottle;
the ceramic insulating sleeve is connected between the liquid storage tank and the reaction cavity through a stainless steel pipe; the ceramic insulating sleeve is sleeved on a part of the stainless steel pipe;
the sealed crucible includes:
the crucible comprises a crucible body, wherein a crucible groove is formed above the crucible body;
the crucible cap is covered on the crucible groove;
the octagonal pad is arranged between the crucible cap and the wall of the crucible groove;
the liquid storage tank passes through the crucible cap through a pipeline to be communicated with the reaction cavity.
2. The high temperature and pressure resistant sealed crucible assembly of claim 1, wherein the walls of the crucible trough have flanges;
the sealed crucible further comprises:
a plurality of screws, one end of which passes through the crucible cap and the flange of the crucible groove;
and a plurality of hexagonal nuts, one of which is connected with one screw, so that the crucible cap is connected with the flange.
3. The high temperature and high pressure resistant sealed crucible assembly of claim 1 or 2, further comprising:
the first pressure gauge is arranged on the glove box, and the four-way connecting piece is provided with a fourth joint which is connected with the first pressure gauge and used for monitoring the pressure in the reaction cavity.
4. The high temperature and high pressure resistant sealed crucible assembly of claim 3, further comprising:
the second pressure gauge is positioned outside the glove box and is arranged on a pipeline between the exhaust pipe and the glove box and used for monitoring pipeline pressure;
the needle valve is positioned outside the glove box and arranged on a pipeline between the exhaust pipe and the glove box and used for adjusting the flow of the pipeline.
5. The high temperature and high pressure resistant sealed crucible assembly of claim 1 or 2, further comprising:
the stop valve is positioned in the glove box and outside the furnace body, is arranged on a pipeline connected with the second joint and is used for communicating or stopping the gas entering the exhaust pipe;
the one-way valve is positioned in the glove box and outside the furnace body, is arranged on a pipeline connected with the third joint and is used for enabling gas of the gas storage steel bottle to flow into the reaction cavity in a single way;
the air inlet valve is positioned outside the glove box and is arranged on an air outlet pipeline of the air storage steel cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321225983.XU CN220079179U (en) | 2023-05-20 | 2023-05-20 | High temperature and high pressure resistant sealed crucible assembly |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321225983.XU CN220079179U (en) | 2023-05-20 | 2023-05-20 | High temperature and high pressure resistant sealed crucible assembly |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220079179U true CN220079179U (en) | 2023-11-24 |
Family
ID=88821118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202321225983.XU Active CN220079179U (en) | 2023-05-20 | 2023-05-20 | High temperature and high pressure resistant sealed crucible assembly |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220079179U (en) |
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2023
- 2023-05-20 CN CN202321225983.XU patent/CN220079179U/en active Active
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