CN114835124A - Preparation method of nano silicon carbide particles based on ferric nitrate shape regulator - Google Patents
Preparation method of nano silicon carbide particles based on ferric nitrate shape regulator Download PDFInfo
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- CN114835124A CN114835124A CN202210570209.6A CN202210570209A CN114835124A CN 114835124 A CN114835124 A CN 114835124A CN 202210570209 A CN202210570209 A CN 202210570209A CN 114835124 A CN114835124 A CN 114835124A
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 title claims abstract description 86
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 44
- 239000002245 particle Substances 0.000 title claims abstract description 41
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000007833 carbon precursor Substances 0.000 claims description 12
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 12
- -1 polydimethylsiloxane Polymers 0.000 claims description 12
- 239000012686 silicon precursor Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 7
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 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
- C01B32/977—Preparation from organic compounds containing silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
A preparation method of nano silicon carbide particles based on a ferric nitrate shape regulator belongs to the technical field of silicon carbide powder preparation and aims to solve the problems of complex preparation process, low yield, and uneven appearance and granularity of the existing silicon carbide powder. The method comprises the following steps: firstly, preparing precursor powder of silicon and carbon; and secondly, sintering and removing impurities to obtain the nano silicon carbide particles based on the ferric nitrate shape regulator. According to the invention, ferric nitrate is used as a shape regulator, and the prepared nano silicon carbide particles based on the ferric nitrate shape regulator have uniform particle size distribution. Solvent components such as water and the like are not introduced in the whole preparation process, reactants are introduced in a solid form, the reaction process is easy to control, the product purity is high, the process is simple, the yield is improved, and the method is suitable for industrial production. The unique combination of the carbon source, the silicon source precursor and the ferric nitrate provides a material basis for the micro-morphology adjustment of the silicon carbide. The method is suitable for preparing the nano silicon carbide particles based on the ferric nitrate shape regulator.
Description
Technical Field
The invention belongs to the technical field of silicon carbide powder preparation, and particularly relates to a preparation method of nano silicon carbide particles based on a ferric nitrate shape regulator.
Background
The ceramic material becomes a non-replaceable material in many fields due to excellent mechanical property and high-temperature stability, wherein the innovation of the preparation technology of the ceramic powder has important significance for the development of the ceramic material. The silicon carbide has the excellent characteristics of light weight, high hardness, high strength, acid and alkali resistance, high temperature resistance and the like. The particle reinforced ceramic is a reinforced or toughened ceramic matrix composite material obtained by introducing particles serving as a second phase reinforcing phase into a ceramic matrix, uniformly dispersing and distributing the particles and compounding the particles with the matrix, and the adopted silicon carbide particles are required to have the characteristics of uniform size and regular shape. The preparation of the silicon carbide particle powder with uniform size has the problems of low product purity, reduced yield, unstable product size, uneven particle size distribution and the like. Therefore, the method has great significance for the research on the preparation of the nano silicon carbide particle powder.
Disclosure of Invention
The invention aims to solve the problems of complex preparation process, low yield and uneven morphology and granularity of the existing silicon carbide powder, and provides a preparation method of nano silicon carbide particles based on ferric nitrate shape regulator.
A preparation method of nano silicon carbide particles based on ferric nitrate shape regulator is realized by the following steps:
firstly, preparing silicon and carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, carbonizing, and adding the carbonized product, phenolic resin powder and ferric nitrate powder into a high-speed mixer for processing to obtain silicon and carbon precursor powder;
II, sintering and impurity removal:
putting the silicon and carbon precursor powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 h to obtain an initial product, and removing impurities to obtain nano silicon carbide particles based on the ferric nitrate shape regulator, thus completing the preparation method;
the mass ratio of the polydimethylsiloxane to the curing agent is 9: 1;
and (3) carbonizing treatment: heating to 800 ℃ at the speed of 1-3.5 ℃/min, and keeping the temperature for 2-5 h;
the mass ratio of the carbonized product to the phenolic resin powder to the ferric nitrate powder is (1-50): 1;
the parameters of the high-speed mixer are as follows: mixing for 5-10 h at the rotating speed of 60-100 r/min under the power of 1-20 Hz;
the purity of the argon is 99.99 percent;
in the high-temperature sintering furnace, firstly heating to 800 ℃ at the speed of 1-3.5 ℃/min, preserving heat for 2-5 h, then continuously heating to 1250-1600 ℃ at the speed of 2-5 ℃/min, preserving heat for 5-10 h, and keeping the temperature reduction speed and the temperature rise speed the same after finishing;
performing impurity removal treatment; and (3) placing the primary product in a muffle furnace, heating to 600-800 ℃ in the air, and firing for 1-6 h.
The reaction principle of the invention is as follows: a novel carbon source and silicon source combination and double-carbon-source reaction system are adopted. Under the combined action of the ferric nitrate powder, the novel carbon source and the silicon source precursor, the reaction of the carbon source and the silicon source is controlled under the molten state to realize the growth of the low-size nanowire silicon carbide particles. Due to the existence of the shape regulator metal salt, the present growth of the silicon carbide crystal grains is inhibited in the growth process, so that the spheroidal morphology is formed.
The invention has the beneficial effects that: the nano silicon carbide particles based on the ferric nitrate shape regulator are prepared by adopting ferric nitrate as the shape regulator, the particle size distribution is uniform, and the average size is nano. In the whole preparation process of the invention, solvent components such as water and the like are not introduced, reactants are introduced in a solid form, the reaction process is easy to control, the product purity is high, the preparation process is simple, the yield is improved, and the preparation method is suitable for industrial production. The unique combination of the carbon source, the silicon source precursor and the ferric nitrate in the invention provides a material basis for the micro-morphology adjustment of the silicon carbide.
The method is suitable for preparing the nano silicon carbide particles based on the ferric nitrate shape regulator.
Drawings
FIG. 1 is an XRD spectrum of nano silicon carbide particles based on ferric nitrate shape modifier prepared in example;
fig. 2 is a TEM image of nano-sized silicon carbide particles based on a shape-modifying agent of iron nitrate prepared in the example.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment provides a preparation method of nano silicon carbide particles based on a ferric nitrate shape regulator, which is realized by the following steps:
firstly, preparing silicon and carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, carbonizing, and adding the carbonized product, phenolic resin powder and ferric nitrate powder into a high-speed mixer for processing to obtain silicon and carbon precursor powder;
II, sintering and impurity removal:
and putting the silicon and carbon precursor powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 h to obtain an initial product, and removing impurities to obtain the nano silicon carbide particles based on the ferric nitrate shape regulator, thus completing the preparation method.
In the first step of this embodiment, the polydimethylsiloxane and the curing agent are commercially available, and the specific curing conditions are based on the specifications of the commercial products.
In the first step of the present embodiment, the treatment is performed in a high-speed mixer, in which the blocks are pulverized and ground and uniformly mixed with the powder.
In the second step of the present embodiment, the carbon removal treatment is directly performed in the impurity removal treatment, because it is ensured that carbon components are excessive in the reaction process, a dual carbon source reaction system is adopted in the raw material ratio of the first step, and it is ensured that the initial product is excessive carbon after the reaction time.
In the first step of the present embodiment, the polydimethylsiloxane serves as a carbon source and a silicon source, and the phenolic resin serves as a supplementary carbon source.
The second embodiment is as follows: the difference between the present embodiment and the first embodiment is that the mass ratio of the polydimethylsiloxane to the curing agent in the first step is 9: 1. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: in this embodiment, the carbonization treatment in the first step is different from the carbonization treatment in the first or second embodiment: heating to 800 ℃ at the speed of 1-3.5 ℃/min, and preserving heat for 2-5 h. Other steps and parameters are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between the embodiment and one of the first to third embodiments is that the mass ratio of the carbonized product, the phenolic resin powder and the ferric nitrate powder in the step one is (1-50): 1. Other steps and parameters are the same as those in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to the fourth embodiments is that the parameters of the high-speed mixer in the first step: mixing for 5-10 h at a rotation speed of 60-100 r/min under the power of 1-20 Hz. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: this embodiment differs from one of the first to fifth embodiments in that the purity of the argon gas in the second step is 99.99%. Other steps and parameters are the same as those in one of the first to fifth embodiments.
The seventh embodiment: the difference between the first embodiment and the sixth embodiment is that, in the second step, the temperature in the high-temperature sintering furnace is first raised to 800 ℃ at a rate of 1-3.5 ℃/min, the temperature is maintained for 2-5 h, then the temperature is continuously raised to 1250-1600 ℃ at a rate of 2-5 ℃/min, the temperature is maintained for 5-10 h, and the temperature lowering rate and the temperature raising rate after the completion are kept the same. Other steps and parameters are the same as those in one of the first to sixth embodiments.
In the embodiment, the heat preservation at 800 ℃ is carried out for 2-5 h, so that the organic carbon component is carbonized, and the generated simple substance carbon participates in the subsequent generation of silicon carbide.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is that the impurity removal treatment in the second step; and (3) placing the initial product in a muffle furnace, heating to 600-800 ℃ in the air, and firing for 1-6 h. Other steps and parameters are the same as those in one of the first to seventh embodiments.
The beneficial effects of the present invention are demonstrated by the following examples:
example (b):
a preparation method of nano silicon carbide particles based on ferric nitrate shape regulator is realized by the following steps:
firstly, preparing silicon and carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, and then carrying out carbonization treatment, and adding the carbonized product, phenolic resin powder and ferric nitrate powder into a high-speed mixer together for treatment to obtain silicon and carbon precursor powder;
II, sintering and impurity removal:
putting the silicon and carbon precursor powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 h to obtain an initial product, and removing impurities to obtain nano silicon carbide particles based on the ferric nitrate shape regulator, thus completing the preparation method;
the mass ratio of the polydimethylsiloxane to the curing agent is 9: 1;
and (3) carbonizing treatment: heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 3 h;
the mass ratio of the carbonized product to the phenolic resin powder to the ferric nitrate powder is 20:10: 1;
the parameters of the high-speed mixer are as follows: mixing for 8 hours at the rotating speed of 100r/min under the power of 20 Hz;
the purity of the argon is 99.99 percent;
in the high-temperature sintering furnace, firstly heating to 800 ℃ at a speed of ℃/min, preserving heat for 4h, then continuously heating to 1500 ℃ at a speed of 2.5 ℃/min, preserving heat for 5h, and keeping the temperature reduction speed and the temperature rise speed the same after finishing; wherein the purpose of keeping the temperature at 800 ℃ for 4h is to carbonize the organic carbon component to generate simple substance carbon which participates in the subsequent generation of silicon carbide;
performing impurity removal treatment; placing the primary product in a muffle furnace, heating to 700 ℃ in air, and burning for 4 h; the decarbonization treatment is directly carried out in the impurity removal treatment, because the excess of carbon components is ensured in the reaction process, a double-carbon-source reaction system is adopted in the raw material proportion in the step one, and the carbon excess is ensured as an initial product after the reaction time.
In the first step of this embodiment, the polydimethylsiloxane and the curing agent are commercially available, and the specific curing conditions are based on the specifications of the commercial products.
In the first step of this embodiment, the block is ground and uniformly mixed with the powder in a high-speed mixer.
In the first step of this example, the polydimethylsiloxane is used as a unified body of the carbon source and the silicon source, and the phenolic resin is used as a supplementary carbon source. In order to ensure the growth of the silicon carbide particles with the nanometer morphology and effectively inhibit the supersaturated linear growth of the silicon carbide, ferric nitrate is introduced as a shape regulator.
In this example, the carbon source and the silicon source react at high temperature under the action of ferric nitrate to form silicon carbide. Wherein, the carbon source and the silicon source have complex systems, so the reaction is carried out by taking ferric nitrate as the leading factor. The ferric nitrate is beneficial to promoting the reaction of a silicon source and a carbon source in a molten state, and the existing growth of silicon carbide crystal grains is inhibited in the growth process due to the existence of the shape regulator metal salt, so that the spheroidal morphology is formed.
The nano silicon carbide particles based on the ferric nitrate shape modifier prepared in the embodiment have an X-ray diffraction (XRD) spectrum as shown in figure 1, and diffraction peaks at 35.7 degrees, 41.4 degrees, 60.0 degrees, 71.8 degrees and 75.4 degrees in the figure are respectively corresponding to (111), (200), (220), (311) and (222) crystal faces of beta-SiC; no impurity peak was found, indicating that the method of this example successfully produced a β -SiC material and the product purity was high.
The micro-morphology of the nano silicon carbide particles based on the ferric nitrate shape regulator prepared in the embodiment is shown in fig. 2, and the silicon carbide particles prepared based on the method of the invention in the embodiment are nano spherical-like micro-morphologies, and the morphology and the particle size distribution are uniform.
Claims (8)
1. A preparation method of nano silicon carbide particles based on a ferric nitrate shape regulator is characterized by comprising the following steps:
firstly, preparing silicon and carbon precursor powder:
uniformly mixing polydimethylsiloxane and a curing agent, curing, carbonizing, and adding the carbonized product, phenolic resin powder and ferric nitrate powder into a high-speed mixer for processing to obtain silicon and carbon precursor powder;
II, sintering and impurity removal:
and putting the silicon and carbon precursor powder into a graphite crucible, putting the graphite crucible into a high-temperature sintering furnace under the protection of argon, heating to 1250-1600 ℃, reacting for 5-10 h to obtain an initial product, and removing impurities to obtain the nano silicon carbide particles based on the ferric nitrate shape regulator, thus completing the preparation method.
2. The method for preparing nano silicon carbide particles based on ferric nitrate shape modifier as claimed in claim 1, wherein the mass ratio of polydimethylsiloxane to curing agent in step one is 9: 1.
3. The method for preparing nano silicon carbide particles based on ferric nitrate shape modifier as claimed in claim 1, wherein the carbonization treatment in step one: heating to 800 ℃ at the speed of 1-3.5 ℃/min, and preserving heat for 2-5 h.
4. The method as claimed in claim 1, wherein the mass ratio of the carbonized product, the phenolic resin powder and the ferric nitrate powder in the step one is (1-50): 1.
5. The method for preparing nano silicon carbide particles based on ferric nitrate shape modifier as claimed in claim 1, wherein the parameters of the high speed mixer in step one are as follows: mixing for 5-10 h at a rotation speed of 60-100 r/min under the power of 1-20 Hz.
6. The method as claimed in claim 1, wherein the purity of argon gas in step two is 99.99%.
7. The method for preparing nano silicon carbide particles based on the ferric nitrate shape modifier according to claim 1, wherein in the second step, the temperature in the high-temperature sintering furnace is increased to 800 ℃ at a rate of 1-3.5 ℃/min, the temperature is maintained for 2-5 h, then the temperature is increased to 1250-1600 ℃ at a rate of 2-5 ℃/min, the temperature is maintained for 5-10 h, and the temperature reduction rate and the temperature increase rate after the temperature is reduced are kept the same.
8. The method for preparing nano silicon carbide particles based on ferric nitrate shape modifier as claimed in claim 1, wherein the impurity removing treatment in step two; and (3) placing the initial product in a muffle furnace, heating to 600-800 ℃ in the air, and firing for 1-6 h.
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| CN114132929A (en) * | 2020-09-04 | 2022-03-04 | 比亚迪股份有限公司 | Preparation method of silicon carbide powder and silicon carbide powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117658145A (en) * | 2023-12-28 | 2024-03-08 | 扎赉诺尔煤业有限责任公司 | Method for preparing SiC nano particles by efficiently utilizing lignite |
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