CN106430212B - A kind of method for industrializing large-scale production silicon carbide powder - Google Patents
A kind of method for industrializing large-scale production silicon carbide powder Download PDFInfo
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Abstract
A kind of method for industrializing large-scale production silicon carbide powder, is related to a kind of industrial-scale production method of high-purity alpha-SiC powder.Present invention selection halosilanes or silane are as original silicon source, using the method for heat stepwise, especially with grinding technics so that mixture mixing is more uniform.The present invention also carries out segregation purification using orientation cohesion to product so that the less pollution of production process；The method that precursor hydrolysis and high temperature cabonization are combined is employed so that silica flour and carbon dust can be mixed uniformly, so as to ensure the preferable homogeneity of final product.
Description
Technical field
The present invention relates to a kind of industrial-scale production method of high-purity alpha-SiC powder.
Background technology
Carborundum from the date of birth, just so that its high rigidity, chemically stable and good corrosion resistance, heat endurance be good, heat is swollen
The many advantages such as swollen coefficient is small, thermal conductivity is high, doping performance height, as noticeable excellent product in inorganic non-metallic material
Kind.Wherein, superfine silicon carbide powder is ranked more due to superior properties such as its higher chemical reactivity and preferable homogeneity
The preferred raw material of the application fields such as structural ceramics, function ceramics, semiconductor components and devices.Silicon carbide ceramics national defence, microelectronics,
The numerous areas such as chemical industry, oil, machinery, metallurgy are all exhibited one's skill to the full.Therefore, industrialization prepares silicon carbide powder right and wrong on a large scale
Often it is necessary and significant.
At present, the method for synthesizing silicon carbide is very more, existing synthesis in solid state, also there is liquid and gas synthesis.Specifically,
Common method has carbon thermal synthesis method, machine-alloying, sol-gel process, self-propagating high-temperature synthetic method, thermal decomposition method, various
Chemical vapour deposition technique etc..Due to the limitation of all many conditions such as cost, technique, equipment, offal treatment complexity, Ke Yishi
Only carbon thermal synthesis method is compared suitable with mechanosynthesis in the method for existing heavy industrialization.But carborundum particle hardness is very
Height, and easily reunite so that mechanosynthesis difficulty or ease prepare the homogeneous silicon carbide powder of high-purity, ultra-fine, property, so that
This method is not well suited on manufacture high-purity silicon carbide powder.And traditional carbon thermal synthesis method has technical process more multiple
Miscellaneous, material purity is difficult to reach big etc. the defect of high purity product standard, heavy contamination and producers' labor intensity.Cause
How this, improve traditional carbon thermal synthesis method so that it can energy-conservation, it is efficient under the conditions of scale produce high-purity carbonization
Silicon powder, the life of silicon carbide ceramics and semiconductor product is produced or even reduces as high purity superfine silicon carbide material industry is solved
Produce the key of cost.
Traditional carbon thermal synthesis method prepares the main component of silicon carbide powder, wherein quartz sand using quartz sand and carbon reaction
SiO2Reacted with carbon C in electric furnace and form SiC.But the purity of its silicon source and carbon source directly limit the purity of product, electric furnace
Reaction condition limit preferable particle diameter distribution.Therefore, follow-up study person is not only improved equipment, and propose
Many new carbon sources, such as carbon black, phenolic resin, starch are used as carbon source；And many new trials, example are have also been made in silicon source
Such as Ludox or silicate.Either production cost is too high and to be not suitable for scale or in life for these silicon sources and carbon source
Very high purity is unable to reach in the range of production cost acceptable, limiting them turns into the powder preparation of industrialization high-purity alpha-SiC
Best option.
The technology that a kind of improved carbothermic method prepares SiC is refer in patent US2014301933., will in the patent
The silicon source of silicic acid matter such as silica, and carbonaceous such as carbon black and oil coke, with C/SiO2Mol ratio 2.5 ~ 4 ratio mixing, so
After be put into 1600 ~ 3000 DEG C of high-temperature process in Acheson stoves and obtain carborundum.This method labor intensity is big, and power consumption is high, operative employee
Sequence is complicated, and needs to use special Special Equipment.
It under the silicon source such as methyl silicate of liquid, normal temperature is liquid to be reported in patent CN 105324332 with being under normal temperature
Carbon source such as phenolic resin and normal temperature under for the catalyst of liquid such as after maleic acid mixes and solidify, in nitrogen or argon gas
Heat 30 ~ 120 minutes and be carbonized at 800 DEG C to 1300 DEG C, then 1350 DEG C to the 2000 DEG C heating 0.5 in nitrogen or argon atmosphere
~ 3 hours synthesizing silicon carbides.The purity of such a method production is higher, it is to avoid because raw material is impure in Acheson method production processes
Only the various impurity elements pollution introduced.It is higher to equipment requirement but this method operating procedure is complicated.
A kind of method of synthesis SiC micro-powders is reported in Chinese patent CN 1636870A.In the method, use
Silicon source of the granularity less than 15 microns, carbon source such as phenolic resin and alcohol are with mass ratio 1：(0.5~2)：2 mixing, through Overheating Treatment,
After cooling, injection pressure, aging, drying process, in 600 ~ 1000 DEG C of high temperature cabonizations 1 ~ 12 hour, 1200 ~ 2000 DEG C of sintering
0.5 ~ 8 hour, obtain sub-micron even nano level silicon carbide powder.This method can cost be low, energy consumption low land prepares SiC powder
Body.But this method needs extra consumption alcohol, is not very economical.
A kind of method of synthesizing silicon carbide powder is reported in the master thesis of University Of Shenyang's Longhai City's ripple.With SiO2With
Activated carbon is initiation material, addition rare earth La or Ce, can obtain silicon carbide powder within 120 ~ 150 minutes in 1500 times insulations.Should
Method significantly reduces energy consumption, alleviates production cost and equipment pressure.However, have very much can for the rare earth element that introduces of this process
The purity of product can be disturbed, and influences the follow-up of powder to use.Therefore, this method is not suitable for industrially preparing on a large scale
High-purity silicon carbide powder.
The content of the invention
For the variety of problems of above-mentioned prior art, it is an object of the invention to provide a kind of industrialized production high-purity silicon carbide
The method of powder.
The present invention comprises the following steps：
1）Silicon source and hydrogen are blended in environment temperature>Reacted under the conditions of 1000 DEG C, obtain purity>4N Si powder；
By high temperature cabonization obtains purity under anaerobic after the carbon source purification with small organic molecule>4N C powder；
2）By the Si powder and C powder with 1: 1 mixed in molar ratio after, add high purity water reaction is hydrolyzed, obtain SiO2
With C homogeneous slurry；
3）By SiO2Be placed in C homogeneous slurry in 150~300 DEG C of temperature environments and carry out granulating and drying, then 600~
Carbonization is pyrolyzed in 800 DEG C of temperature environments, mixture after carbonization is obtained；
4）Mixture after carbonization is placed in pre-burning in 500~600 DEG C of temperature environments, the water for removing mixture remained on surface steams
Gas and air, are placed in 1400~1900 DEG C of temperature environments after then mixture is ground and carry out middle temperature synthesis, obtain carbon
SiClx powder crude product；
5）By silicon carbide powder crude product it is purified after, obtain silicon carbide powder fine work.
The present invention is due to taking above technical scheme, and it has advantages below：
（1）Present invention selection halosilanes or silane select purer small molecular organic compounds to make as original silicon source
For original carbon source.For original silicon source or carbon source, it can be purified using suitable step, the method for purification of small organic molecule
Including but not limited to distillation, rectifying, extraction, absorption etc..This method ensures that purity in raw material level, with final product
Purification is combined, it is ensured that the silicon carbide powder of production is high-purity powder.
（2）The method that this method uses heat stepwise, and the processes such as grinding are added between fragments, reasonably utilize
Heat resource, it is ensured that whole production process power consumption is low.Especially with grinding technics so that mixture mixing is more uniform.
（3）This method has given up the purifying technique that traditional chemical pickling immersion, solvent extraction etc. has pollution, utilizes orientation
Cohesion carries out segregation purification to product so that the less pollution of production process.
（4）This method employs the method that precursor hydrolysis and high temperature cabonization are combined so that silica flour and carbon dust can be uniform
Mixing, so as to ensure the preferable homogeneity of final product.
（5）Silicon carbide powder produced by the invention is characterized in：Carborundum is cubic structure, and its average grain diameter is 1~30
μm, purity is 99.9%（3N）More than, or even 99.999%（5N））, main impurity content：The ppm of nitrogen≤50（Even≤
25 ppm）, the ppm of boron≤1.0（Even≤0.1 ppm）, the ppm of chromium≤0.8（Even≤0.4 ppm）, the ppm of aluminium≤1.0（Very
To≤0.5 ppm）, the ppm of sodium≤0.8（Even≤0.5 ppm）, the ppm of titanium≤1.0（Even≤0.5 ppm）, vanadium≤1.0
ppm（Even≤0.1 ppm）.It is suitable for subsequently manufacturing structural ceramics, function ceramics or semiconductor electronic component etc..
Further, silicon source of the present invention is SiCl4、SiHCl3、SiH2Cl2、SiBr4Or SiI4.These are all can be with
It is used as the halosilanes or silane of original silicon source.Advantage from above-claimed cpd is：
1st, gaseous state is presented in halosilanes or silane at a certain temperature, it is easy to separating-purifying, will not be with the residue in raw material
Deng mixing, so as to ensure that higher purity.
If the 2, do not run out of in gaseous halosilanes or silane reaction, reactant can be left in the form of a vapor
System, so that guarantee system will not be polluted by unnecessary silicon compound.
3rd, there is maturation process in the preparation of such compound so that prepare or buy such compound phase to holding
Easily.
The purer small molecular organic compounds of present invention selection are as original carbon source, and the carbon source is esters such as acetic acid second
Ester, alcohols such as methanol, isopropanol or ethylene glycol, acids such as oleic acid, palmitic acid are used as carbon source raw material using these specific materials
Advantage：
1st, the source of these small organic molecules is quite varied, if esters are common spices and additive, marked down
Ground is largely obtained；Alcohols can be obtained from modes such as stalk fermentation, Soap Factory's soapmaking supernatants；Acids can also be refined by plant
It is extensive easily to prepare；
2nd, their carburizing temperatures are not high so that the cost of carbonisation is in controllable scope；
3rd, they all only have carbon, hydrogen, three kinds of elements of oxygen, and hydrogen-oxygen can be run away in the form of water, will not be in final product
Middle introducing impurity element pollution.
Step 3 of the present invention）The preferable temperature environment of middle granulating and drying is 180~280 DEG C, preferred temperature environment
For 200~250 DEG C.The preferable temperature environment is to the dry mechanism of action and accessible special excellent results：
The silica flour and carbon dust prepared as described above is all simple substance element inorganic matter, therefore, and they only can be with absorption shape
The water of formula, rather than chemical bonding water.Therefore, and high temperature it can just need not go out these moisture very much, certainly, they must
Must than water vapour pressure（100℃）It is higher by certain scope so that whole process is occurred near chemical balance, but
Some position away from chemical balance occurs.But, this temperature can not be too high, and otherwise watch crystal can occur for silicon powder surface
Change or partially sinter and influence following process, carbon dust is also faced with generates CO or CO with oxygen reaction2And cause unnecessary
Loss.In summary, in the case where ensureing that obvious loss does not occur for carbon dust silica flour, some water for adsorption of fully going out
Point.Temperature range more than, can ensure the surface texture and reactivity of the nanoscale carbon dust silica flour to greatest extent, together
When remove influence subsequent reactions absorption water.
The step 4）Described in grind nitrogen protect in the case of carry out.It is preferred that effect machine of the nitrogen protection to grinding
Reason and accessible special excellent results：
As described above, carbon dust easily and air in oxygen reaction bring unnecessary loss, therefore, the present invention selectionization
Learn inert nitrogen protection and grind.Nitrogen will not generally react with Si and C（Within rational temperature range）, while can be with
The method separated by air is inexpensively prepared, therefore selection nitrogen is used as chemoproection gas.Meanwhile, the atmosphere of nitrogen can subtract
The bulk density of small solid state powder, the nitrogen being passed through can partly fluidized bulk powder so that grinding and mixing
Cheng Gengwei is fully and effective.
The method that the present invention is refined to the silicon carbide powder crude product of acquirement has following three kinds：
The step 5）Middle silicon carbide powder crude product is placed under the conditions of 1900~2200 DEG C is evaporated in vacuo, and obtains carbon
SiClx powder fine work.Process for purification is in technologic advantage and accessible special excellent results：
The sublimation temperature of carborundum is higher, and up to 270 DEG C, following danger is faced at these high temperatures：(i) SiC in itself can
There is a certain degree of decomposition；(ii) requirement for equipment is too high, easily causes danger.And being evaporated in vacuo can be steamed by reducing
The method of air pressure, at relatively low temperature steams SiC, so as to alleviate facility load, adds whole technological process
Safety coefficient.The explosion danger that the moment malleation of a large amount of air accumulations generations is brought is not had simultaneously.
The step 5）In it is optional by silicon carbide powder crude product it is oriented condensation segregation purification, obtain silicon carbide powder essence
Product.The process for purification is in technologic advantage and accessible special excellent results：Orientation condensation segregation purification is to utilize mixing
Thing is different in the composition of solid-state and liquid, thus they have a solid liquid phase distribution coefficient.Pass through solid-liquid distribution coefficient
Difference, by sacrificing the controllable liquid region, can complete whole solid phase by the impurity enriched in solid a to liquid regions
Material purity is substantially improved.This method and other method such as electrolysis etc. are compared, and are compared in terms of the purity of solid matter is improved
It is more effective.In the preparation of many materials, such as the preparation of rafifinal, orientation condensation segregation purification can cause the purity of material
Reach 5N.Therefore, this method is good candidate for preparing high-purity alpha-SiC material.
Embodiment
The present invention is described in detail with reference to specific example, but the present invention is not limited to act set forth below
Example.
Embodiment 1：
By SiCl4With H2With 1: 2.2 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1200 DEG C；Ethylene glycol is existed
N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.By Si powder and C powder mixed hydrolysis with disposed slurry in 200 DEG C of granulations
Dry, well mixed SiO is obtained in 600 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 1900 DEG C of high-temperature vacuum distillation removal of impurities after terminating.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（4N）, remaining impurity content：The ppm of nitrogen≤50, boron
≤ 1.0 ppm, the ppm of chromium≤0.8, the ppm of aluminium≤1.0, the ppm of sodium≤0.8, the ppm of titanium≤1.0, the ppm of vanadium≤1.0.
Embodiment 2：
By SiHCl3With H2With 1: 1.2 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1100 DEG C；Methanol is existed
N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.By Si powder and C powder mixed hydrolysis with disposed slurry in 240 DEG C of granulations
Dry, well mixed SiO is obtained in 600 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 2000 DEG C of high-temperature vacuum distillation removal of impurities after terminating.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（4N）, remaining impurity content：The ppm of nitrogen≤50, boron
≤ 1.0 ppm, the ppm of chromium≤0.8, the ppm of aluminium≤1.0, the ppm of sodium≤0.8, the ppm of titanium≤1.0, the ppm of vanadium≤1.0.
Embodiment 3：
By SiI4With H2With 1: 2.2 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1200 DEG C；By ethyl acetate
In N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.Si powder and C powder mixed hydrolysis are made with disposed slurry at 250 DEG C
Grain is dried, and well mixed SiO is obtained in 550 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 2100 DEG C of high-temperature vacuum distillation removal of impurities after terminating,
Finally it is oriented condensation segregation purification.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（5N）, remaining impurity content：The ppm of nitrogen≤25, boron
≤ 0.1 ppm, the ppm of chromium≤0.4, the ppm of aluminium≤0.5, the ppm of sodium≤0.5, the ppm of titanium≤0.5, the ppm of vanadium≤0.1.
Embodiment 4：By SiBr4With H2With 1: 2.2 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1150 DEG C；Will
Oleic acid is in N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.By Si powder and C powder mixed hydrolysis with disposed slurry 250
DEG C granulating and drying, well mixed SiO is obtained in 550 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 2100 DEG C of high-temperature vacuum distillation removal of impurities after terminating,
Finally it is oriented condensation segregation purification.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（5N）, remaining impurity content：The ppm of nitrogen≤27, boron
≤ 0.2 ppm, the ppm of chromium≤0.5, the ppm of aluminium≤0.7, the ppm of sodium≤0.6, the ppm of titanium≤0.6, the ppm of vanadium≤0.2.
Embodiment 5：
By SiH2Cl2With H2With 1: 1.5 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1200 DEG C；By isopropanol
In N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.Si powder and C powder mixed hydrolysis are made with disposed slurry at 240 DEG C
Grain is dried, and well mixed SiO is obtained in 600 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 2000 DEG C of high-temperature vacuum distillation removal of impurities after terminating.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（4N）, remaining impurity content：The ppm of nitrogen≤30, boron
≤ 0.7 ppm, the ppm of chromium≤0.8, the ppm of aluminium≤0.5, the ppm of sodium≤0.6, the ppm of titanium≤0.9, the ppm of vanadium≤0.9.
Embodiment 6：By SiBr4With H2With 1: 2.2 mixed in molar ratio, reaction obtains 4N high-purity Si powder at 1150 DEG C；Will
Palmitic acid is in N2High temperature cabonization obtains 4N high-purity C powder under conditions of protection.Si powder and C powder mixed hydrolysis are existed with disposed slurry
250 DEG C of granulating and dryings, well mixed SiO is obtained in 550 DEG C of carbonizations2With C powder mixtures.
Being down to instrument with 500~600 DEG C of pre-burning to water vapour contents in high temperature furnace can not detect, then in N2Under protection
Grinding is uniform.Then middle temperature synthesis is carried out at 1400~1900 DEG C.Reaction uses 2100 DEG C of high-temperature vacuum distillation removal of impurities after terminating,
Finally it is oriented condensation segregation purification.
Obtained product progress carries out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4~20 μm.Use ICP-
MS carries out Si contents in elementary analysis, high-purity Si powder and reaches 99.99%（5N）, remaining impurity content：The ppm of nitrogen≤27, boron
≤ 0.2 ppm, the ppm of chromium≤0.5, the ppm of aluminium≤0.7, the ppm of sodium≤0.6, the ppm of titanium≤0.6, the ppm of vanadium≤0.2.
Claims (9)
1. a kind of method for industrializing large-scale production silicon carbide powder, it is characterised in that comprise the following steps：
1）Silicon source and hydrogen are blended in environment temperature>Reacted under the conditions of 1000 DEG C, obtain purity>4N Si powder；To have small
High temperature cabonization obtains purity under anaerobic after the carbon source purification of molecular organic>4N C powder；The silicon source be halosilanes or
Person's silane；
2）By the Si powder and C powder with 1: 1 mixed in molar ratio after, add high purity water reaction is hydrolyzed, obtain SiO2With C's
Homogeneous slurry；
3）By SiO2It is placed in C homogeneous slurry in 150~300 DEG C of temperature environments and carries out granulating and drying, then at 600~800 DEG C
Carbonization is pyrolyzed in temperature environment, mixture after carbonization is obtained；
4）Mixture after carbonization is placed in pre-burning in 500~600 DEG C of temperature environments, remove mixture remained on surface vapor and
Air, is placed in 1400~1900 DEG C of temperature environments after then mixture is ground and carries out middle temperature synthesis, obtain carborundum
Powder crude product；
5）By silicon carbide powder crude product it is purified after, obtain silicon carbide powder fine work.
2. the method for industrialization large-scale production silicon carbide powder according to claim 1, it is characterised in that the silicon source is
SiCl4、SiHCl3、SiH2Cl2、SiBr4Or SiI4。
3. the method for industrialization large-scale production silicon carbide powder according to claim 1, it is characterised in that the carbon source is
Ethyl acetate, methanol, isopropanol, ethylene glycol, oleic acid or palmitic acid.
4. the method that industrialization mass produces silicon carbide powder according to claim 1, it is characterised in that the step 3）
The temperature environment of middle granulating and drying is 180~280 DEG C.
5. the method that industrialization mass produces silicon carbide powder according to claim 4, it is characterised in that the step 3）
The temperature environment of middle granulating and drying is 200~250 DEG C.
6. the method that industrialization mass produces silicon carbide powder according to claim 1, it is characterised in that the step 4）
Described in grind nitrogen protect in the case of carry out.
7. the method for industrialization large-scale production silicon carbide powder, its feature according to claim 1 or 2 or 3 or 4 or 5 or 6
It is the step 5）Middle silicon carbide powder crude product is placed under the conditions of 1900~2200 DEG C is evaporated in vacuo, and obtains carborundum
Powder fine work.
8. the method for industrialization large-scale production silicon carbide powder, its feature according to claim 1 or 2 or 3 or 4 or 5 or 6
It is the step 5）Middle silicon carbide powder crude product is first placed under the conditions of 1900~2200 DEG C is evaporated in vacuo, then oriented
Segregation purification is condensed, silicon carbide powder fine work is obtained.
9. the method for industrialization large-scale production silicon carbide powder, its feature according to claim 1 or 2 or 3 or 4 or 5 or 6
It is the step 5）It is middle to purify the oriented condensation segregation of silicon carbide powder crude product, obtain silicon carbide powder fine work.
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| CN107902658B (en) * | 2017-11-13 | 2020-07-31 | 宁夏工商职业技术学院（宁夏化工技工学校、宁夏机电工程学校、宁夏农业机械化学校） | Carborundum powder midbody apparatus for producing |
| CN112522788A (en) * | 2020-10-30 | 2021-03-19 | 山东天岳先进科技股份有限公司 | Nitrogen-rich silicon carbide powder and preparation method and application thereof |
| CN113501525A (en) * | 2021-08-20 | 2021-10-15 | 中电化合物半导体有限公司 | Synthesis method of silicon carbide powder |
| CN113896201B (en) * | 2021-10-29 | 2022-07-19 | 连云港市沃鑫高新材料有限公司 | Preparation method of silicon carbide powder for electronic packaging |
| CN114835123B (en) * | 2022-05-24 | 2023-11-28 | 内蒙古海特华材科技有限公司 | Preparation method of cubic phase silicon carbide micron particles |
| CN117003244B (en) * | 2023-07-11 | 2024-04-26 | 温州宏丰电工合金股份有限公司 | High-purity silicon carbide powder and preparation method thereof |
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| CN101857439A (en) * | 2010-06-18 | 2010-10-13 | 北京科技大学 | Method for synthesizing SiC powder by utilizing gold mine tailings |
| CN102674355A (en) * | 2012-05-11 | 2012-09-19 | 南京工业大学 | Alpha crystal phase mesoporous silicon carbide material and preparation method thereof |
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