CN106430212A - Method for industrialized mass production of silicon carbide powder - Google Patents
Method for industrialized mass production of silicon carbide powder Download PDFInfo
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Abstract
The invention discloses a method for industrialized mass production of silicon carbide powder, and relates to industrialized mass production of high-purity SiC powder. According to the method for the industrialized mass production of the silicon carbide powder, halogenosilane or silane is used as an original silicon resource, and mixture is blended more uniformly through the adoption of an incremental heating method and particularly a grinding process. Besides, directional coagulation is adopted to conduct segregation and purification on a product, so that pollution during the production process is lesser; a method combining precursor hydrolyzation with high temperature carbonization is adopted so that silicon powder and carbon powder can be mixed uniformly, thus guaranteeing good homogeneity of a 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 little, thermal conductivity is high, doping performance height, become noticeable excellent product in Inorganic Non-metallic Materials
Kind.Wherein, superfine silicon carbide powder, more due to superior properties such as its higher chemical reactivity and preferable homogeneity, ranks
The preferred raw material of the applications 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, silicon carbide powder right and wrong are prepared in industrialization on a large scale
Often it is necessary and significant.
At present, the method for synthesizing silicon carbide is very many, existing synthesis in solid state, also has liquid and gas to synthesize.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 restriction of all many condition such as cost, technique, equipment, offal treatment complexity, Ke Yishi
Carbon thermal synthesis method is only had to compare with mechanosynthesis in the method for existing heavy industrialization suitable.But carborundum particle hardness is very
Height, and easily reunite so that mechanosynthesis difficulty or ease prepare silicon carbide powder high-purity, ultra-fine, that property is homogeneous, so that
This method is not well suited on manufacturing high-purity silicon carbide powder.And traditional carbon thermal synthesis method has technical process more multiple
Miscellaneous, material purity difficult to reach high purity product standard, heavy contamination and producers' high labor intensive etc. defect.Cause
This, how to improve traditional carbon thermal synthesis method so that it can energy-conservation, efficient under the conditions of scale produce high-purity carbonization
Silicon powder, becomes the life solving that high purity superfine silicon carbide material industry produces or even reduces silicon carbide ceramics and semiconductor product
Produce the key of cost.
Traditional carbon thermal synthesis method prepares silicon carbide powder, the wherein main component of quartz sand using quartz sand and carbon reaction
SiO2React formation SiC with carbon C in electric furnace.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.For this reason, follow-up study person is not only improved to equipment, and propose
Many new carbon sources, such as carbon black, phenolic resin, starch etc. is as carbon source；And many new trials, example be have also been made on silicon source
As Ludox or silicate etc..These silicon sources and carbon source or production cost are too high and to be not suitable for scale, or are giving birth to
Produce and be unable to reach very high purity in the range of cost acceptable, limiting them becomes industrialization high-purity alpha-SiC powder preparation
Best option.
Refer to the technology that a kind of improved carbothermic method prepares SiC in patent US2014301933.In this patent, will
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 put into 1600 ~ 3000 DEG C of high-temperature process in Acheson stove and obtain carborundum.The method high labor intensive, power consumption is high, operative employee
Sequence is complicated, and needs using special Special Equipment.
Patent CN 105324332 reports with normal temperature be liquid silicon source such as methyl silicate, be liquid under normal temperature
Carbon source such as phenolic resin and normal temperature under for liquid catalyst such as maleic acid mix and solidify after, in nitrogen or argon gas
Heat carbonization in 30 ~ 120 minutes, then 1350 DEG C to 2000 DEG C heating 0.5 in nitrogen or argon atmosphere at 800 DEG C to 1300 DEG C
~ 3 hours synthesizing silicon carbides.The purity that this kind of method produces is higher, it is to avoid because raw material is impure in Acheson method production process
The net various impurity element pollutions introducing.But this method operating procedure is complicated, higher to equipment requirement.
A kind of method of synthesis SiC micro-powder is reported in Chinese patent CN 1636870A.In the method, use
Granularity is less than 15 microns of silicon source, carbon source such as phenolic resin and alcohol is with mass ratio 1：(0.5~2)：2 mixing, through Overheating Treatment,
Cooling, injection pressure, after aging, dried 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.The method being capable of low cost, energy consumption low land preparation 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, adds 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, the rare earth element that introduces of this process have very much can
The purity of product can be disturbed, and affect the follow-up use of powder.Therefore, the method is not suitable for industrially preparing on a large scale
High-purity silicon carbide powder.
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>React under the conditions of 1000 DEG C, obtain purity>The Si powder of 4N；
After the carbon source with small organic molecule is purified, high temperature cabonization obtains purity under anaerobic>The C powder of 4N；
2）By described Si powder and C powder with 1: 1 mixed in molar ratio after, add high purity water to be hydrolyzed reaction, obtain SiO2With C's
Homogeneous slurry；
3）By SiO2It is placed in 150～300 DEG C of temperature environments with the homogeneous slurry of C and carries out granulating and drying, then 600～800
It is pyrolyzed carbonization in DEG C temperature environment, obtain mixture after carbonization；
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 after being then ground mixture in 1400～1900 DEG C of temperature environments and carries out middle temperature synthesis, obtain carborundum
Powder crude product；
5）After purified for silicon carbide powder crude product, obtain silicon carbide powder fine work.
Due to taking above technical scheme, it has advantages below to the present invention：
（1）The present invention selects halosilanes or silane as original silicon source, selects purer small molecular organic compounds as former
Beginning carbon source.For original silicon source or carbon source, can be included using suitable step purification, the method for purification of small organic molecule
But it is not limited to distillation, rectifying, extraction, absorption etc..This method ensures that purity in raw material level, the purification with final product
Combine it is ensured that the silicon carbide powder producing is high-purity powder.
（2）The method that this method adopts heat stepwise, and add the operations such as grinding between fragments, reasonably utilize
Heat resource is 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 traditional chemical pickling immersion, solvent extraction etc. the purifying technique of pollution, using orientation
Cohesion carries out segregation purification to product so that the less pollution of production process.
（4）The method that this method employs precursor hydrolysis and high temperature cabonization combines is so that silica flour and carbon dust can be uniform
Mixing, thus ensure the preferable homogeneity of final product.
（5）The feature of silicon carbide powder that the present invention produces is：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：Nitrogen≤50 ppm（Even≤
25 ppm）, boron≤1.0 ppm（Even≤0.1 ppm）, chromium≤0.8 ppm（Even≤0.4 ppm）, aluminium≤1.0 ppm（Very
To≤0.5 ppm）, sodium≤0.8 ppm（Even≤0.5 ppm）, titanium≤1.0 ppm（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 permissible
Halosilanes as original silicon source or silane.Advantage from above-claimed cpd is：
1st, halosilanes or silane assumes gaseous state at a certain temperature it is easy to separating-purifying, will not be mixed with the residue in raw material etc.
Close, thus 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, thus guarantee system will not be polluted by unnecessary silicon compound.
3rd, there is maturation process so that preparing or buying such compound phase to appearance in the preparation of such compound
Easily.
The present invention selects purer small molecular organic compounds as original carbon source, and described carbon source is esters such as acetic acid second
Ester, alcohols such as methyl alcohol, isopropanol or ethylene glycol, acids such as oleic acid, palmitic acid, these concrete materials are used as carbon source raw material
Advantage：
1st, the source of these small organic molecules is quite varied, and such as esters are common spices and additive, and marked down ground is big
Amount obtains；Alcohols can obtain from modes such as stalk fermentation, Soap Factory's soapmaking supernatants；Acids can also be refined easily by plant
Ground is extensive to be prepared；
2nd, their carburizing temperatures not high so that the cost of carbonisation is in controlled 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 draw in final product
Enter 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.This preferable temperature environment is to the mechanism of action being dried and accessible special excellent results：
The silica flour of preparation as above and carbon dust are all simple substance element inorganic matters, and therefore, they only can carry adsorption form
Water, rather than chemical bonding water.Therefore, too high temperature is not needed just can to go out these moisture, certainly, they must compare
The vapour pressure of water（100℃）Exceed certain scope so that whole process be not near chemical balance occur, but away from
Certain position of chemical balance occurs.But, this temperature nor too high, otherwise silicon powder surface can occur surface vitrification or
Person partially sinters and affects following process, and carbon dust is also faced with and generates CO or CO with oxygen reaction2And cause unnecessary loss.
In sum, in the case of ensureing that carbon dust silica flour does not occur obvious loss, some moisture of adsorption of fully going out.?
Above temperature range, can ensure surface texture and the reactivity of this nanoscale carbon dust silica flour to greatest extent, remove simultaneously
Go to affect the absorption water of subsequent reactions.
Described step 4）Described in grind nitrogen protection in the case of carry out.Preferably nitrogen protection is to the effect machine grinding
Reason and accessible special excellent results：
As described above, easy and in the air the oxygen reaction of carbon dust brings unnecessary loss, therefore, the present invention selects chemistry lazy
Property nitrogen protection and grind.Nitrogen generally will not be reacted with Si and C（Within rational temperature range）, can pass through simultaneously
The detached method of air is prepared at a low price, therefore selects nitrogen as chemoproection gas.Meanwhile, the atmosphere of nitrogen can reduce admittedly
The bulk density of state powder, the nitrogen being passed through can partly fluidized bulk powder so that grind and mixed process more
For abundant and effective.
The present invention carries out refined method to the silicon carbide powder crude product obtaining following three kinds：
Described step 5）Middle silicon carbide powder crude product is placed in 1900～2200 DEG C under the conditions of carry out vacuum distillation, obtain carborundum
Powder fine work.Process for purification is in technologic advantage and accessible special excellent results：
The sublimation temperature of carborundum is higher, up to 270 DEG C, faces following danger at these high temperatures：I () SiC has one in itself
Determine the decomposition of degree；(ii) requirement for equipment is too high, is susceptible to danger.And vacuum distillation can be by reducing vapour pressure
Method, at relatively low temperature SiC being steamed, thus alleviating facility load, increased the peace of whole technological process
Overall coefficient.Do not have the explosion danger that the moment malleation of a large amount of air accumulations generations is brought simultaneously.
Described step 5）In optional by oriented for silicon carbide powder crude product condensation segregation purification, obtain silicon carbide powder essence
Product.This process for purification is in technologic advantage and accessible special excellent results：Orientation condensation segregation purification is using mixing
Thing is different in the composition of solid-state and liquid, thus they have a solid liquid phase distribution coefficient.By solid-liquid distribution coefficient
Impurity enriched in solid to liquid regions by sacrificing this controllable liquid region, can be completed whole solid phase by difference
Being substantially improved of material purity.The method and additive method such as electrolysis etc. are compared, ratio in terms of improving the purity of solid matter
More effective.In the preparation of many materials, the preparation of such as rafifinal, orientation condensation segregation purification is so that the purity of material
Reach 5N.Therefore, the method is good candidate for preparing high-purity alpha-SiC material.
Specific embodiment
With reference to specific example, the present invention is described in detail, 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 at 1200 DEG C obtains the high-purity Si powder of 4N；By ethylene glycol in N2Protect
Under conditions of shield, high temperature cabonization obtains high-purity C powder of 4N.By Si powder and C powder mixed hydrolysis with disposed slurry in 200 DEG C of granulating and dryings,
The SiO being uniformly mixed in 600 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 1900 DEG C of high-temperature vacuum distillation removal of impurities.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（4N）, remaining impurity content：Nitrogen≤50 ppm, boron
≤ 1.0 ppm, chromium≤0.8 ppm, aluminium≤1.0 ppm, sodium≤0.8 ppm, titanium≤1.0 ppm, vanadium≤1.0 ppm.
Embodiment 2：
By SiHCl3With H2With 1: 1.2 mixed in molar ratio, reaction at 1100 DEG C obtains the high-purity Si powder of 4N；By methyl alcohol in N2Protect
Under conditions of shield, high temperature cabonization obtains high-purity C powder of 4N.By Si powder and C powder mixed hydrolysis with disposed slurry in 240 DEG C of granulating and dryings,
The SiO being uniformly mixed in 600 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 2000 DEG C of high-temperature vacuum distillation removal of impurities.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（4N）, remaining impurity content：Nitrogen≤50 ppm, boron
≤ 1.0 ppm, chromium≤0.8 ppm, aluminium≤1.0 ppm, sodium≤0.8 ppm, titanium≤1.0 ppm, vanadium≤1.0 ppm.
Embodiment 3：
By SiI4With H2With 1: 2.2 mixed in molar ratio, reaction at 1200 DEG C obtains the high-purity Si powder of 4N；By ethyl acetate in N2
Under conditions of protection, high temperature cabonization obtains high-purity C powder of 4N.Will be dry in 250 DEG C of granulations with disposed slurry to Si powder and C powder mixed hydrolysis
SiO that is dry, being uniformly mixed in 550 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 2100 DEG C of high-temperature vacuum distillation removal of impurities,
Finally it is oriented condensation segregation purification.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（5N）, remaining impurity content：Nitrogen≤25 ppm, boron
≤ 0.1 ppm, chromium≤0.4 ppm, aluminium≤0.5 ppm, sodium≤0.5 ppm, titanium≤0.5 ppm, vanadium≤0.1 ppm.
Embodiment 4：By SiBr4With H2With 1: 2.2 mixed in molar ratio, reaction at 1150 DEG C obtains the high-purity Si powder of 4N；Will
Oleic acid is in N2Under conditions of protection, high temperature cabonization obtains high-purity C powder of 4N.By Si powder and C powder mixed hydrolysis with disposed slurry 250
DEG C granulating and drying, the SiO being uniformly mixed in 550 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 2100 DEG C of high-temperature vacuum distillation removal of impurities,
Finally it is oriented condensation segregation purification.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（5N）, remaining impurity content：Nitrogen≤27 ppm, boron
≤ 0.2 ppm, chromium≤0.5 ppm, aluminium≤0.7 ppm, sodium≤0.6 ppm, titanium≤0.6 ppm, vanadium≤0.2 ppm.
Embodiment 5：
By SiH2Cl2With H2With 1: 1.5 mixed in molar ratio, reaction at 1200 DEG C obtains the high-purity Si powder of 4N；By isopropanol in N2
Under conditions of protection, high temperature cabonization obtains high-purity C powder of 4N.Will be dry in 240 DEG C of granulations with disposed slurry to Si powder and C powder mixed hydrolysis
SiO that is dry, being uniformly mixed in 600 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 2000 DEG C of high-temperature vacuum distillation removal of impurities.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（4N）, remaining impurity content：Nitrogen≤30 ppm, boron
≤ 0.7 ppm, chromium≤0.8 ppm, aluminium≤0.5 ppm, sodium≤0.6 ppm, titanium≤0.9 ppm, vanadium≤0.9 ppm.
Embodiment 6：By SiBr4With H2With 1: 2.2 mixed in molar ratio, reaction at 1150 DEG C obtains the high-purity Si powder of 4N；Will
Palmitic acid is in N2Under conditions of protection, high temperature cabonization obtains high-purity C powder of 4N.Si powder and C powder mixed hydrolysis are existed with disposed slurry
250 DEG C of granulating and dryings, the SiO being uniformly mixed in 550 DEG C of carbonizations2With C powder mixture.
It is down to instrument with 500～600 DEG C of pre-burning to water vapour contents in high temperature furnace cannot detect, then in N2Under protection
Grind uniformly.Then carry out middle temperature synthesis at 1400～1900 DEG C.React after terminating using 2100 DEG C of high-temperature vacuum distillation removal of impurities,
Finally it is oriented condensation segregation purification.
The product obtaining carries out carrying out grain size analysis, particle mean size d with laser particle analyzer50It is distributed in 4～20 μm.Use ICP-
MS carries out elementary analysis, and in high-purity Si powder, Si content reaches 99.99%（5N）, remaining impurity content：Nitrogen≤27 ppm, boron
≤ 0.2 ppm, chromium≤0.5 ppm, aluminium≤0.7 ppm, sodium≤0.6 ppm, titanium≤0.6 ppm, vanadium≤0.2 ppm.
Claims (9)
1. a kind of method of industrialization large-scale production silicon carbide powder is it is characterised in that comprise the following steps：
1）Silicon source and hydrogen are blended in environment temperature>React under the conditions of 1000 DEG C, obtain purity>The Si powder of 4N；To have little
After the carbon source purification of molecular organic, high temperature cabonization obtains purity under anaerobic>The C powder of 4N；
2）By described Si powder and C powder with 1: 1 mixed in molar ratio after, add high purity water to be hydrolyzed reaction, obtain SiO2With C's
Homogeneous slurry；
3）By SiO2It is placed in 150～300 DEG C of temperature environments with the homogeneous slurry of C and carries out granulating and drying, then at 600～800 DEG C
It is pyrolyzed carbonization in temperature environment, obtain mixture after carbonization；
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 after being then ground mixture in 1400～1900 DEG C of temperature environments and carries out middle temperature synthesis, obtain carborundum
Powder crude product；
5）After purified for silicon carbide powder crude product, obtain silicon carbide powder fine work.
2. industrialization mass produces the method for silicon carbide powder it is characterised in that described silicon source is according to claim 1
SiCl4、SiHCl3、SiH2Cl2、SiBr4Or SiI4.
3. industrialization mass produces the method for silicon carbide powder it is characterised in that described carbon source is according to claim 1
Ethyl acetate, methyl alcohol, isopropanol, ethylene glycol, oleic acid or palmitic acid.
4. according to claim 1 the method for industrialization large-scale production silicon carbide powder it is characterised in that described step 3）
The temperature environment of middle granulating and drying is 180～280 DEG C.
5. according to claim 4 the method for industrialization large-scale production silicon carbide powder it is characterised in that described step 3）
The temperature environment of middle granulating and drying is 200～250 DEG C.
6. according to claim 1 the method for industrialization large-scale production silicon carbide powder it is characterised in that described step 4）
Described in grind nitrogen protection in the case of carry out.
7. the method that industrialization according to claim 1 or 2 or 3 or 4 or 5 or 6 mass produces silicon carbide powder, its feature
It is described step 5）Middle silicon carbide powder crude product is placed in 1900～2200 DEG C under the conditions of carry out vacuum distillation, obtain carborundum
Powder fine work.
8. the method that industrialization according to claim 1 or 2 or 3 or 4 or 5 or 6 mass produces silicon carbide powder, its feature
It is described step 5）Middle silicon carbide powder crude product is first placed in 1900～2200 DEG C under the conditions of carry out vacuum distillation, more oriented
Condensation segregation purification, obtains silicon carbide powder fine work.
9. the method that industrialization according to claim 1 or 2 or 3 or 4 or 5 or 6 mass produces silicon carbide powder, its feature
It is described step 5）Middle by oriented for silicon carbide powder crude product condensation segregation purification, obtain silicon carbide powder fine work.
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| CN107902658A (en) * | 2017-11-13 | 2018-04-13 | 毛涛 | A kind of silicon carbide powder intermediate process units |
| 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 |
| CN113896201A (en) * | 2021-10-29 | 2022-01-07 | 连云港秉文科技有限公司 | Preparation method of silicon carbide powder for electronic packaging |
| CN114835123A (en) * | 2022-05-24 | 2022-08-02 | 内蒙古海特华材科技有限公司 | Preparation method of cubic phase silicon carbide microparticles |
| CN117003244A (en) * | 2023-07-11 | 2023-11-07 | 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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| 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 |
| CN113896201A (en) * | 2021-10-29 | 2022-01-07 | 连云港秉文科技有限公司 | Preparation method of silicon carbide powder for electronic packaging |
| 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 |
| CN114835123A (en) * | 2022-05-24 | 2022-08-02 | 内蒙古海特华材科技有限公司 | Preparation method of cubic phase silicon carbide microparticles |
| 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 |
| CN117003244A (en) * | 2023-07-11 | 2023-11-07 | 温州宏丰电工合金股份有限公司 | High-purity silicon carbide powder and preparation method thereof |
| 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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