CN111591994A - Preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth - Google Patents
Preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 39
- 239000013078 crystal Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000007789 gas Substances 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- 229910052681 coesite Inorganic materials 0.000 claims description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229910052682 stishovite Inorganic materials 0.000 claims description 16
- 229910052905 tridymite Inorganic materials 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000010812 mixed waste Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005262 decarbonization Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 239000007790 solid phase Substances 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000010795 gaseous waste Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B32/97—Preparation from SiO or SiO2
-
- 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
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of high-purity silicon carbide powder for growing silicon carbide single crystal, which uses CH4High purity SiO as a gas phase carbon source2The powder is a solid silicon source. Under vacuum, re-injecting a gas-phase carbon source, wherein the carbon source is uniformly distributed in the solid silicon source; avoiding unnecessary pollution and improving the purity of the silicon carbide. And the gas phase/solid phase synthesized SiC powder is utilized, and impurities of the gas phase raw material cannot be left in the SiC finished product. Excessive C source is involved in synthesis, and conversion of all Si sources can be ensured, and excessive C is from CH4No impurity exists, and O is introduced under the conditions of dry stillness and high temperature2C of gas oxidation residue becomes gas CO2The C can be easily separated from the powder. Moreover, the raw materials are easy to obtain, and the cost is relatively low. What is needed isTherefore, the preparation cost is low, and the purity of the prepared silicon carbide powder is high.
Description
Technical Field
The invention relates to the field of silicon carbide single crystal growth materials, in particular to a preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth.
Background
In recent years, high-resistivity, high-purity semi-insulating silicon carbide single crystal substrates have been increasingly used for high-frequency, high-power SiC and GaN-based electronic devices. At present, a PVT (physical vapor transport) method is generally adopted to grow high-purity semi-insulating silicon carbide single crystals, and in the PVT method, SiC powder is used as a raw material for growing the single crystals, so that various parameters of the SiC powder directly influence the growth quality and the electrical performance of the high-purity semi-insulating single products.
Commercial SiC powders are generally prepared by the Acheson process, which is a carbothermal reduction process. However, the SiC powder prepared by the method has high impurity content and is not suitable for the growth of SiC single crystals. In addition, the preparation method of the SiC powder further comprises the following steps: sol-gel method, CVD method, self-propagating method, and the like. However, these methods are either costly and not suitable for the batch synthesis of silicon carbide powders; or the purity is not high, so that the method is not suitable for growing the silicon carbide single crystal.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of high-purity silicon carbide powder for growing silicon carbide single crystals, which is low in preparation cost and high in purity of the prepared silicon carbide powder.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing SiO2Putting the powder into a graphite crucible, and then putting the crucible into a vacuum heating furnace;
step 2, vacuumizing the vacuum heating furnace, and then filling CH into the vacuum heating furnace4/N2Mixing the gas;
step 3, turning on a heater to SiO2Heating the powder and standing to obtain silicon carbide powder containing carbon residue and mixed waste gas CO + H2+N2+NH3+H2O；
Step 4, cooling the graphite crucible to room temperature, pumping out mixed waste gas in the vacuum heating furnace, performing electric pulse treatment, and then discharging; injecting air into the vacuum heating furnace to atmospheric pressure, and taking out the graphite crucible;
step 5, taking out the silicon carbide powder containing residual carbon in the graphite crucible, placing the silicon carbide powder in a quartz crucible, and then placing the quartz crucible back to the vacuum heating furnace;
step 6, vacuumizing the vacuum heating furnace; then filling O into the vacuum heating furnace2And N2Heating and standing the mixed gas, and performing decarbonization treatment;
and 7, cooling the quartz crucible, and taking out powder in the quartz crucible to obtain the high-purity SiC powder suitable for single crystal growth.
The SiO2The purity of the powder is more than 99.999%.
The SiO2The particle size of the powder is 50-200 μm.
In the step 2, the vacuum heating furnace is vacuumized to 10 DEG-4Under Pa, pouring CH into the vacuum heating furnace4/N2Mixing the gas until the pressure is 70-90 kPa.
In the step 3, SiO2The heating temperature of the powder is 1800oC~2000oAnd C, standing for more than 3 hours.
In the step 6, the vacuum heating furnace is vacuumized to 10 DEG-4Pa below; filling O into a vacuum heating furnace2And N2Mixed gas (es)The pressure of the mixture is 0.7 to 1MPa, and the heating temperature is 500 to 650oAnd C, standing for more than 1 hour.
After the scheme is adopted, the invention has the following beneficial effects:
in one aspect, the invention uses CH4High purity SiO as a gas phase carbon source2The powder is a solid silicon source. Under vacuum, re-injecting a gas-phase carbon source, wherein the carbon source is uniformly distributed in the solid silicon source; the method can avoid using double solid phase sources, and the unnecessary pollution caused by the uniform premixing of the liquid phase source and the solid phase source or the addition of the activating agent, thereby improving the purity of the silicon carbide. And the gas phase/solid phase synthesized SiC powder is utilized, and impurities of the gas phase raw material cannot be left in the SiC finished product. Excessive C source is involved in synthesis, and conversion of all Si sources can be ensured, and excessive C is from CH4No impurity exists, and O is introduced under the conditions of dry stillness and high temperature2C of gas oxidation residue becomes gas CO2The C can be easily separated from the powder. Therefore, the invention can prepare high-purity silicon carbide powder.
In another aspect, the invention uses high purity SiO2Powder, CH4、N2、O2The raw materials are easily available and relatively low in cost. Only gaseous waste is generated in the production process, and after the waste gas is treated by electric pulses, the final product is all gaseous substances harmless to the environment. Therefore, the invention has low preparation cost, environmental protection and no pollution.
Drawings
FIG. 1 is a schematic reaction scheme of steps 1-4;
FIG. 2 is a schematic diagram of the reaction of steps 5-7.
Description of reference numerals:
a vacuum heating furnace 10; a heater 20; a graphite crucible 30; a quartz crucible 40.
Detailed Description
As shown in FIGS. 1 and 2, the present invention discloses a method for preparing a high purity silicon carbide powder for the growth of a silicon carbide single crystal, comprising the steps of:
step 1, mixing high-purity SiO2(purity of>99.999%) was placed in a graphite crucible 30, and the crucible was then placed in a vacuum heating furnace 10, as shown in fig. 1. SiO 22The powder size is determined according to the required product specification, and the particle size is generally 50-200 μm.
Step 2, vacuumizing the vacuum heating furnace 10 to 10-4Pa below; then, the vacuum heating furnace 10 is started to be charged with CH4/N2Mixing the gas until the pressure is 70-90 kPa. N is a radical of2As shielding and transport gases with catalytic gases, CH4As a gas phase carbon source.
Step 3, using a heater 20 to heat SiO2Heating the powder to 1800oC~2000oAnd C, standing for more than 3 hours. The final product is silicon carbide powder (SiC + C) with carbon residue, and the byproduct is mixed waste gas (CO + H)2+N2+NH3+H2O)。
Step 4, cooling to room temperature, pumping out the mixed waste gas in the reaction furnace, performing electric pulse treatment after passing through a gas collecting tank, and discharging the final mixed gas CO2+N2+H2O+NO2. Then, air is injected into the crucible to atmospheric pressure, and the graphite crucible 30 is taken out.
And 5, taking out the silicon carbide powder (SiC + C) containing carbon residue in the graphite crucible 30, then placing the silicon carbide powder in a quartz crucible 40, and then placing the quartz crucible 40 back to the vacuum heating furnace 10, as shown in figure 2.
Step 6, vacuumizing the vacuum heating furnace 10 to 10-4Pa or less. Then, the vacuum heating furnace 10 is charged with O2/N2Mixing the gas to 0.7-1 MPa, heating to 500-650%oC, standing for more than 1 hour, performing carbon removal process, and reacting C in the powder into CO2。
And 7, cooling and taking out to obtain the high-purity SiC powder suitable for single crystal growth.
The key point of the invention is that the invention uses CH4High purity SiO as a gas phase carbon source2The powder is a solid silicon source. Under vacuum, re-injecting a gas-phase carbon source, wherein the carbon source is uniformly distributed in the solid silicon source; this avoids the use of dual solid phase sources which could cause unwanted contamination when the liquid/solid phase sources are pre-mixed or when the activator is addedAnd (6) dyeing. N is a radical of2When used as a protective and transport gas and a catalytic gas, the catalyst can catalyze the synthesis of C and Si. In addition, in step 3, 1800-2000 is usedoC reaction to suppress nitride generation while suppressing generation of nitrogen compounds by CH4Decomposition of 2H2+ C, then H2The presence of (b) contributes to the reduction of the N concentration in the synthesis of high purity SiC powder.
The gas phase/solid phase is utilized to synthesize SiC powder, and solid impurities mainly come from SiO2Powder, commercial high purity SiO2The powder is easy to obtain and the technology is mature. Impurities of the gas phase feedstock do not remain in the SiC product. Excessive C source is involved in synthesis, and conversion of all Si sources can be ensured, and excessive C is from CH4No impurity exists, and O is introduced under the conditions of dry stillness and high temperature2C of gas oxidation residue becomes gas CO2The C can be easily separated from the powder.
Therefore, the invention patent uses high purity SiO2Powder, CH4、N2、O2The raw materials are easy to obtain and the cost is relatively low. Only gaseous waste is generated in the production process, and after the waste gas is treated by electric pulses, the final product is all gaseous substances harmless to the environment.
The above description is only exemplary of the present invention and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above exemplary embodiments according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (6)
1. A preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing SiO2Putting the powder into a graphite crucible, and then putting the crucible into a vacuum heating furnace;
step 2, vacuumizing the vacuum heating furnace, and then filling CH into the vacuum heating furnace4/N2Mixing the gas;
step 3, turning on a heater to SiO2Heating the powder and standingTo obtain silicon carbide powder containing residual carbon and mixed waste gas CO + H2+N2+NH3+H2O；
Step 4, cooling the graphite crucible to room temperature, pumping out mixed waste gas in the vacuum heating furnace, performing electric pulse treatment, and then discharging; injecting air into the vacuum heating furnace to atmospheric pressure, and taking out the graphite crucible;
step 5, taking out the silicon carbide powder containing residual carbon in the graphite crucible, placing the silicon carbide powder in a quartz crucible, and then placing the quartz crucible back to the vacuum heating furnace;
step 6, vacuumizing the vacuum heating furnace; then filling O into the vacuum heating furnace2And N2Heating and standing the mixed gas, and performing decarbonization treatment;
and 7, cooling the quartz crucible, and taking out powder in the quartz crucible to obtain the high-purity SiC powder suitable for single crystal growth.
2. The method for producing a high purity silicon carbide powder for silicon carbide single crystal growth according to claim 1, characterized in that: the SiO2The purity of the powder is more than 99.999%.
3. The method for producing a high purity silicon carbide powder for silicon carbide single crystal growth according to claim 1, characterized in that: the SiO2The particle size of the powder is 50-200 μm.
4. The method for producing a high purity silicon carbide powder for silicon carbide single crystal growth according to claim 1, characterized in that: in the step 2, the vacuum heating furnace is vacuumized to 10 DEG-4Under Pa, pouring CH into the vacuum heating furnace4/N2Mixing the gas until the pressure is 70-90 kPa.
5. The method for producing a high purity silicon carbide powder for silicon carbide single crystal growth according to claim 1, characterized in that: in the step 3, SiO2The heating temperature of the powder is 1800oC~2000oC, standing for 3 hoursThe above.
6. The method for producing a high purity silicon carbide powder for silicon carbide single crystal growth according to claim 1, characterized in that: in the step 6, the vacuum heating furnace is vacuumized to 10 DEG-4Pa below; filling O into a vacuum heating furnace2And N2Mixing the gas to 0.7-1 MPa, heating to 500-650 deg.CoAnd C, standing for more than 1 hour.
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|---|---|---|---|---|
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2020
- 2020-06-03 CN CN202010494478.XA patent/CN111591994A/en active Pending
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