CN116393044B - Large-particle SiC material synthesis device and process - Google Patents
Large-particle SiC material synthesis device and process Download PDFInfo
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 15
- 239000007770 graphite material Substances 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 230000003647 oxidation Effects 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
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- 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
- C30B29/36—Carbides
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- 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
- B01J19/24—Stationary reactors without moving elements inside
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- 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
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/984—Preparation from elemental silicon
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- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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Abstract
The invention provides a large-particle SiC material synthesis device and a large-particle SiC material synthesis process, which belong to the technical field of SiC preparation and comprise a crucible and a carrier component. The crucible is provided with a cavity for containing silicon powder and carbon powder, the carrier assembly comprises a fixing part and a carrier part, the fixing part is formed by graphite materials, the fixing part is matched with an opening of the crucible, a hole groove is formed in the fixing part along the direction of the cavity, and the carrier part is hung to the hole groove and extends to the silicon powder and the carbon powder in the cavity. The device can be matched with the process to obtain SiC particles (generally not lower than 40%) with the size of more than 6mm, and particularly, under the process condition, the particle size of more than 3mm can be up to 70%, so that the Si/C ratio and the growth speed in the growth atmosphere are effectively influenced by the particle size of SiC powder.
Description
Technical Field
The invention relates to the technical field of SiC preparation, in particular to a large-particle SiC material synthesis device.
Background
SiC, as a third generation semiconductor material, has the advantages of wide band gap, high critical electric field, high thermal conductivity, high drift velocity of saturated carriers, and the like. Compared with the first and second generation semiconductor materials represented by Si and GaAs, siC has great application prospect in high temperature, high frequency, high power, photoelectron and radiation resistance.
The existing growth method of the SiC monocrystal commonly used in industry is a PVT method, the quality of SiC powder used for growth greatly influences the quality of the SiC monocrystal obtained by growth, the purity of the SiC monocrystal is directly influenced by the purity of the powder, the grain size of the powder also has dynamic influence on the SiC growth process, and finally the electrical property, uniformity, defects and the like of the SiC monocrystal are influenced. The SiC powder commonly used for growth is divided into two types: one is an abrasive grade SiC powder; one is a high purity SiC powder synthesized specifically for SiC single crystal growth. In view of impurities, high-purity SiC powder is mainly selected for SiC single crystal growth in production. In the synthesis of high-purity SiC powder, a self-propagating high-temperature combustion method becomes a preferred method for synthesizing industrial high-purity SiC powder due to the advantages of low cost, easy control of the process, high yield and the like.
In the PVT method growth process of SiC single crystal, the grain size of the SiC powder used can influence the Si/C ratio in the growth atmosphere, the growth speed and the like. For reasons of vapor phase evaporation rate and crystal quality, larger particle SiC material is typically selected as the growth source for crystal growth.
Disclosure of Invention
In order to make up for the defects, the invention provides a large-particle SiC material synthesizing device, and aims to solve the problem that the particle size of SiC powder can influence the Si/C ratio in the growth atmosphere and the growth speed so as to synthesize large particles.
The invention is realized in the following way: the invention provides a large-particle SiC material synthesizing device which comprises a crucible and a carrier component.
The crucible is provided with a cavity for containing silicon powder and carbon powder.
The carrier assembly comprises a fixing part made of graphite material and a carrier part made of graphite material, wherein the fixing part is matched with the opening of the crucible, a hole groove is formed in the fixing part along the direction of the cavity, the carrier part is hung to the hole groove and extends to silicon powder and carbon powder in the cavity, and the carrier part is of a strip-shaped structure with the thickness of 0.5-10 mm.
In one embodiment of the present invention, the hole grooves are provided in plurality and uniformly distributed on the fixing portion.
In one embodiment of the invention, the carrier portion top end has a hook member that is suspended into the aperture slot, the hook member extending into the aperture slot as a curved portion.
In one embodiment of the invention, the carrier portion extends between 10cm and 25 cm.
The disclosure also provides a large-particle SiC material synthesis process, which is applicable to a large-particle SiC material synthesis device, and includes the following steps:
uniformly mixing silicon powder with the average grain diameter of 100 mu m and carbon powder with the average grain diameter of 90 mu m according to a certain mass ratio to form powder;
placing powder into a high-purity graphite crucible of a SiC material synthesizing device;
then placing the SiC material synthesizing device in a heating furnace, and vacuumizing to below 1 Pa;
then argon is filled to 2500-3500Pa, and the temperature is heated to 1400 ℃ and kept for 4-5.5h;
maintaining the air pressure in the above steps, further heating to 2300 ℃ and preserving heat for 18-21h;
stopping heating, pouring argon to normal pressure, and naturally cooling to room temperature.
In one embodiment of the invention, the silicon powder and the carbon powder are uniformly mixed according to a mass ratio of 8:4.
In one embodiment of the present invention, after the SiC material is subjected to the synthesis process, the SiC material needs to be purified and separated, which includes the following steps:
step one: opening the crucible, and taking down the carrier component and the powder deposited on the carrier component;
step two: taking the carrier part off the fixing part and putting the carrier part into a tube furnace;
step three: vacuumizing to below 1Pa, and then filling oxygen to normal pressure;
step four: heating to 1000 ℃, oxidizing for 8-10h, and changing gas at a certain flow rate in the oxidation process;
step five: taking out oxidized powder, crushing and sieving to separate, wherein crushing refers to: the agglomerate of particles is broken up from the form of the agglomerate back to the form of individual particles.
In one embodiment of the invention, in step four, the replacement gas is performed at a flow rate of 1000sccm during the oxidation process.
The beneficial effects of the invention are as follows: in the large-particle SiC material synthesizing apparatus according to the present invention, when in use, the plurality of carrier portions 220 and the fixing portions 210 are assembled and placed in the crucible 100 to be subjected to SiC material synthesis, the crucible 100 is put into the synthesizing furnace, and the crucible is heated to the synthesizing temperature and kept for a certain period of time and then cooled, and the carrier portions 220 provide a large specific surface area in the space above the powder material, so that the large-particle SiC material synthesizing apparatus has a large number of nucleation sites. After the high temperature is maintained for a certain time, nucleation and continuous growth can be carried out under the supersaturation condition to obtain larger SiC particles, the device is taken out after synthesis is finished, and graphite parts are removed through oxidation to obtain large-particle SiC materials;
the device can be matched with the process to obtain SiC particles (generally not lower than 40%) with the size of more than 6mm, and particularly, under the process condition, the particle size of more than 3mm can be up to 70%, so that the Si/C ratio and the growth speed in the growth atmosphere are effectively influenced by the particle size of SiC powder.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of a large-particle SiC material synthesizing device provided by an embodiment of the invention;
fig. 2 is a schematic structural view of a fixing part in a large-particle SiC material synthesizing apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic view of a carrier part in a large-particle SiC material synthesizing device according to an embodiment of the present invention;
FIG. 4 is a bar graph of the proportions of powders of different particle sizes according to an embodiment of the present invention.
In the figure: 100-crucible; 110-cavity; 200-a carrier assembly; 210-a fixing part; 211-hole slots; 220-a carrier portion; 221-hooks.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus 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 present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a 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 invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, as well as the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly under and obliquely below the second feature, or simply means that the first feature is less level than the second feature.
Examples
Referring to fig. 1-3, the present invention provides a technical solution: a large particle SiC material synthesizing device comprises a crucible 100 and a carrier assembly 200.
The carrier assembly 200 is mounted on the crucible 100, and carbon powder and silicon powder are contained in the crucible 100, so that the carbon powder and the silicon powder are synthesized on the carrier assembly 200 through conditions of temperature, time and the like to form larger particles.
Referring to fig. 1, a crucible 100 has a cavity 110 for holding silicon powder and carbon powder, and when a carrier assembly 200 is disposed on the crucible 100, a synthesis space is formed by cooperating with the cavity 110, and particles of the synthesis space grow on the carrier assembly 200. Specifically, the carrier 220 extends between 10cm and 25cm, and the distance is adjusted according to the size and structure of the crucible 100, and the graphite strips of the carrier 220 are required to be spaced from the mixed powder at the bottom of the crucible by a certain distance, so that the graphite strips can sublimate at a high temperature, and the growth on the graphite strips is realized.
Referring to fig. 1, 2 and 3, the carrier assembly 200 includes a fixing portion 210 made of graphite material and a carrier portion 220 made of graphite material, the fixing portion 210 is matched with the opening of the crucible 100, a hole slot 211 is formed in the fixing portion 210 along the direction of the cavity 110, and the carrier portion 220 is suspended to the hole slot 211 and extends to silicon powder and carbon powder in the cavity 110 and needs to be spaced a certain distance from the mixture in the crucible 100. Specifically, the carrier part 220 is in a strip structure, the thickness of the carrier part 220 is between 0.5 and 10mm, the carrier part 220 is made into a thin strip shape, so that a larger specific surface area is provided for the silicon powder and carbon powder mixture, more nucleation sites are formed, large-particle materials are formed, and graphite strips are used as disposable consumables, so that carbon dioxide gas is formed after oxidization, and SiC particles are left. The plurality of the hole grooves 211 are provided and uniformly distributed on the fixing portion 210, so that the plurality of the carrier portions 220 can be hung, thereby realizing sufficient synthesis of a large amount of particles. The top end of the carrier portion 220 has a hook 221 that can hang into the slot 211, the hook 221 extending into the slot 211 to a curved portion, the hook 221 being curved at an angle generally between 0 ° and 180 °, and preferably being most stable when hung at 90 °.
Referring to fig. 4, it can be seen from the graph that the particle size of the synthesized SiC particles is at most 2.8mm-3.35mm, so that SiC particles with larger particle size can be prepared to the greatest extent, and generally, the apparatus is matched with the preparation process to obtain SiC particles with particle size of more than 3mm but not less than 40%, and large particles with particle size of more than 6mm can be produced.
The present disclosure also provides a large particle SiC material synthesis process using a large particle SiC material synthesis apparatus, comprising the steps of:
uniformly mixing silicon powder with the average grain diameter of 100 mu m and carbon powder with the average grain diameter of 90 mu m according to the mass ratio of 8:4 to form powder;
placing the materials into a high-purity graphite crucible of a SiC material synthesizing device;
then placing the SiC material synthesizing device in a heating furnace, and vacuumizing to below 1 Pa;
then argon is filled to 2500-3500Pa, and the temperature is heated to 1400 ℃ and kept for 4-5.5h;
maintaining the air pressure in the above steps, further heating to 2300 ℃ and preserving heat for 18-21h;
stopping heating, pouring argon to normal pressure, and naturally cooling to room temperature.
Further, after the SiC material is subjected to the synthesis process, the SiC material needs to be purified and separated, and the method includes the following steps:
step one: opening the crucible, and taking down the carrier component and the powder deposited on the carrier component;
step two: taking the carrier part off the fixing part and putting the carrier part into a tube furnace;
step three: vacuumizing to below 1Pa, and then filling oxygen to normal pressure;
step four: heating to 1000 ℃, oxidizing for 8-10h, changing gas at a flow of 1000sccm in the oxidation process, removing graphite parts by oxidation to obtain large-particle SiC materials, specifically introducing compressed air or oxygen at high temperature, changing graphite strips into carbon dioxide gas after oxidation, and only leaving SiC particles;
step five: taking out oxidized powder, crushing, sieving and separating, and further sieving SiC particles with the diameter of more than 3mm, wherein crushing means: the agglomerate of particles is broken up from the form of the agglomerate back to the form of individual particles.
Note that: large particle SiC material can effectively affect Si/C in the growth atmosphere and affect growth rate as a default background in the art.
Tairov, 1995 and 1983: materials Science and Engineering B29 (1995) 83-89, a study was made of the relationship between Si/C ratio of gas phase generated by decomposition of SiC powder at different particle diameters and the dissociation energy of SiC powder and the average powder particle diameter.
As described herein, larger SiC particles are shown to decompose to produce a gas phase with less Si content and a higher C content.
Larger SiC particles as shown require a higher dissociation energy for decomposition and therefore sublimation of larger particles of powder is slower at the same temperature. In actual production, the powder used for growing crystals is mixed with a plurality of meshes, and the proportion of different meshes can be adjusted according to actual demands, so that the effects of adjusting the generation amount of gas-phase substances and controlling the growth speed are achieved.
The relationship between Si/C in the gas phase and the particle size of the powder, and the relationship between the dissociation energy of SiC and the average particle size of the powder, which are measured under vacuum conditions, are described in the publication.
The ideas of the above-mentioned articles are repeatedly cited in subsequent studies of Shi Erwei, wang Yu, etc., for example, journal 1, influence of raw materials on growth of silicon carbide single crystals, inorganic materials journal, month 7 of 2003, volume 18, 4.
2. Wang Yu, gu Peng, feijun, wang Penggang, lei Pei, yuan Li. The PVT method grows 4H-SiC crystal and the research of polytype inclusion defects progresses [ J/OL ]. Artificial lens school report.
Specifically, the working principle of the large-particle SiC material synthesizing device is as follows: in use, a plurality of carrier parts 220 are assembled with the fixing parts 210 and placed in the crucible 100 ready for SiC material synthesis, the crucible 100 is put into a synthesis furnace, heated to a synthesis temperature and kept for a certain time and cooled, and the carrier parts 220 provide a large specific surface area in the space above the powder, so that the crucible has a large number of nucleation sites. After the high temperature is maintained for a certain time, nucleation and continuous growth can be carried out under the supersaturation condition to obtain larger SiC particles, the device is taken out after synthesis is finished, and graphite parts are removed through oxidation to obtain large-particle SiC materials;
through making carrier portion 220 rectangular structure, and its thickness makes thinly to this regard as disposable consumptive material, this kind of setting not only can make its increase specific surface area, forms more nucleation sites, and also is convenient for oxidize into carbon dioxide gas, leaves the SiC granule, simultaneously, the needs of fixed portion 210 are made thickly, in order to reuse many times.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The large-particle SiC material synthesizing device is characterized by comprising
A crucible (100), wherein the crucible (100) is provided with a cavity (110) for containing silicon powder and carbon powder;
the carrier assembly (200), carrier assembly (200) include fixed part (210) and carrier part (220) that are made by graphite material, fixed part (210) with the opening looks adaptation of crucible (100), just fixed part (210) are followed hole groove (211) has been seted up in the direction of cavity (110), carrier part (220) hang to hole groove (211) to silica flour, the carbon powder in cavity (110) extend, carrier part (220) are the strip structure, and its thickness is between 0.5-10 mm.
2. A large-particle SiC material synthesizing apparatus according to claim 1, characterized in that said hole grooves (211) are provided in plural and uniformly distributed on said fixing portion (210).
3. A large particle SiC material synthesizing apparatus according to claim 2, wherein said carrier portion (220) has a hook member (221) at a top end thereof which is suspended into said hole groove (211), said hook member (221) extending into said hole groove (211) as a curved portion.
4. A large particle SiC material synthesizing apparatus according to claim 1, characterized in that said carrier portion (220) extends between 10cm and 25 cm.
5. A large-particle SiC material synthesizing process, adapted to a large-particle SiC material synthesizing apparatus according to any one of claims 1 to 4, comprising the steps of:
uniformly mixing silicon powder with the average grain diameter of 100 mu m and carbon powder with the average grain diameter of 90 mu m according to a certain mass ratio to form powder;
placing powder into a high-purity graphite crucible of a SiC material synthesizing device;
then placing the SiC material synthesizing device in a heating furnace, and vacuumizing to below 1 Pa;
then argon is filled to 2500-3500Pa, and the temperature is heated to 1400 ℃ and kept for 4-5.5h;
maintaining the air pressure in the above steps, further heating to 2300 ℃ and preserving heat for 18-21h;
stopping heating, pouring argon to normal pressure, and naturally cooling to room temperature.
6. The process for synthesizing large-particle SiC material according to claim 5, wherein the silicon powder and the carbon powder are uniformly mixed according to a mass ratio of 8:4.
7. The process for synthesizing large-particle SiC material according to claim 5, wherein after the SiC material is subjected to the synthesis process, the SiC material is purified and separated, and the process comprises the following steps:
step one: opening the crucible, and taking down the carrier component and the powder deposited on the carrier component;
step two: taking the carrier part off the fixing part and putting the carrier part into a tube furnace;
step three: vacuumizing to below 1Pa, and then filling oxygen to normal pressure;
step four: heating to 1000 ℃, oxidizing for 8-10h, and changing gas at a certain flow rate in the oxidation process;
step five: taking out oxidized powder, crushing, and sieving and separating.
8. The process of claim 7, wherein in step four, the gas is replaced at a flow rate of 1000sccm during the oxidation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310658082.8A CN116393044B (en) | 2023-06-06 | 2023-06-06 | Large-particle SiC material synthesis device and process |
Applications Claiming Priority (1)
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| CN109137076A (en) * | 2018-10-17 | 2019-01-04 | 福建北电新材料科技有限公司 | A kind of fixed device of seed wafer and its application method of growth single-crystal silicon carbide |
| US20190186045A1 (en) * | 2017-12-18 | 2019-06-20 | National Chung Shan Institute Of Science And Technology | Device for growing silicon carbide of specific shape |
| CN110408987A (en) * | 2019-09-06 | 2019-11-05 | 北京北方华创微电子装备有限公司 | Crystal growing furnace |
| CN114368982A (en) * | 2022-01-21 | 2022-04-19 | 巩义市泛锐熠辉复合材料有限公司 | Silicon carbide coating graphite base and preparation method thereof |
| CN116084017A (en) * | 2022-12-22 | 2023-05-09 | 成都中浦科技有限公司 | Crucible structure for preparing silicon carbide single crystal, preparation method and application thereof |
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| US20190186045A1 (en) * | 2017-12-18 | 2019-06-20 | National Chung Shan Institute Of Science And Technology | Device for growing silicon carbide of specific shape |
| CN109137076A (en) * | 2018-10-17 | 2019-01-04 | 福建北电新材料科技有限公司 | A kind of fixed device of seed wafer and its application method of growth single-crystal silicon carbide |
| CN110408987A (en) * | 2019-09-06 | 2019-11-05 | 北京北方华创微电子装备有限公司 | Crystal growing furnace |
| CN114368982A (en) * | 2022-01-21 | 2022-04-19 | 巩义市泛锐熠辉复合材料有限公司 | Silicon carbide coating graphite base and preparation method thereof |
| CN116084017A (en) * | 2022-12-22 | 2023-05-09 | 成都中浦科技有限公司 | Crucible structure for preparing silicon carbide single crystal, preparation method and application thereof |
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