KR101641839B1 - Preparation method of Si/SiC composite nanoparticles by fusion process of solid phase reaction and plasma decomposition - Google Patents
Preparation method of Si/SiC composite nanoparticles by fusion process of solid phase reaction and plasma decomposition Download PDFInfo
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- 238000003746 solid phase reaction Methods 0.000 title claims abstract description 27
- 239000002105 nanoparticle Substances 0.000 title abstract description 12
- 239000002131 composite material Substances 0.000 title abstract description 6
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000000354 decomposition reaction Methods 0.000 title description 2
- 238000007499 fusion processing Methods 0.000 title 1
- 239000000843 powder Substances 0.000 claims abstract description 105
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 17
- 238000000197 pyrolysis Methods 0.000 claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
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- 238000004519 manufacturing process Methods 0.000 claims description 18
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 9
- 239000006188 syrup Substances 0.000 claims description 2
- 235000020357 syrup Nutrition 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 33
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 185
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
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- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
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- 238000003917 TEM image Methods 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- 238000010574 gas phase reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical group C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
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- C01B31/36—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
Description
The present invention relates to a method for producing a Si / SiC nanocomposite powder by a solid-phase reaction and a thermal plasma pyrolysis process, and more particularly, to a method for producing a Si / SiC nanocomposite powder, SiC nanocomposite powder using a solid-phase reaction and a thermal plasma pyrolysis process capable of producing Si / SiC nanocomposite powder at a high cost, uniformity and low cost.
SiC (silicon carbide) is generally physically / chemically stable and has high heat stability and high temperature strength because it has high heat resistance and thermal conductivity. It has high abrasion resistance and is used as a high temperature material for gas turbine structural materials, It can be used mainly for manufacturing semiconductor fixtures, wear resistant materials, automobile parts, corrosion resistance or chemical resistance parts and electronic parts of chemical plants.
SiC based products are manufactured by the sintering method because of the high melting point of SiC (over 2400 ℃) and sintering additives are used to lower the sintering temperature. When the sintering additive is added, the sintering temperature can be lowered to around 2000 ℃. As the sintering aid for the SiC powder, B (boron), Al 2 O 3 (alumina), C (carbon) and the like are used. On the other hand, in order to use the SiC sintered product for the semiconductor wafer manufacturing process and the facing material of the fusion reactor, high purity is essential. However, sintering aids used in the sintering of SiC powders may act as impurities.
In order to solve this problem, nano-sized SiC can be used as a sintering auxiliary agent. The effect of the nano-sized SiC powder on the sintering of the micro-sized SiC powder is as follows. As the particle size becomes smaller, the surface energy is increased. As a result, the melting point of the nano-sized SiC powder is lowered and the sintering phenomenon occurs. . That is, the sintering method using nanopowder can be called liquid phase sintering or partial liquid sintering method. In this case, since a homogeneous material is used as the sintering aid, there is an advantage that the concern about a decrease in the purity of the sintered body of SiC, which occurs when the hetero-oxide is used as a sintering aid, can be minimized. However, even if a nano-sized SiC powder is used as a sintering aid, a high sintering temperature of 2000 ° C or more is required. Therefore, in order to lower the sintering temperature and the impurity concentration of the SiC sintered body simultaneously, it is required to develop a new sintering auxiliary agent.
On the other hand, there is a liquid reaction sintering method for producing a SiC sintered body at a relatively low sintering temperature. In this method, SiC powder and C (carbon) powder are mixed with an organic binder (10-20 wt% The Si is evaporated or infiltrated into the SiC compact in a high-temperature vacuum of 1500-1700 ° C to react with carbon in the SiC compact to obtain a sintered compact. However, in this method, there is a problem that unreacted Si remains in the SiC sintered body because the silicon metal infiltrates into the SiC molded body after melting or requires infiltration after evaporation.
Therefore, it is necessary to develop a sintering additive capable of simultaneously exhibiting the effect of sintering assistant nanoparticles and the sintering of liquid phase reaction in order to reduce the mixing of impurities by the sintering aid in the production of high-purity SiC sintered body and at the same time lower the sintering temperature. The Si / SiC nanocomposite powder is a sintering aid material suitable for this demand.
According to conventional studies, SiC nano powder was synthesized by gas phase reaction or pyrolysis. The new material research group of the new technology research institute in Japan synthesized SiC nano powder of 30 ~ 50 nm size by using RF thermal plasma. Ethylene (C 2 H 4 ) gas was used as carbon source and SiH 4 gas was used. SiC nano powder having a size of several tens of nanometers, which is excellent in dispersibility, is produced, but the operation cost of raw material and RF plasma is expensive. Also, Professor of UC Santa Barbara, USA. Eric McFarland produced SiC nano powders with 10 nm size by thermal plasma decomposition of tetramethylsilane (TMS) at a high vacuum of 0.001 ~ 0.02 Torr using a low pressure plasma reactor. Silane pyrolysis is a process used to produce ultrafine β-SiC by pyrolysis of silane in a graphite reactor. The synthesis reaction is [CH 3 SiH 3 = SiC + 3H 2 ]. Since expensive raw materials are used to produce SiC nano powder, there is a problem that the price of SiC nano powder becomes expensive. Si / SiC nanocomposite powders also require a higher manufacturing cost because they use a similar process as SiC nano powder.
On the other hand, the inventor of the present invention has proposed a method of manufacturing silicon carbide nanotubes using thermal plasma as Patent Document No. 0001. Patent Literature 0001 discloses a method for manufacturing a microcrystalline silicon carbide composite material which comprises mixing a silicon fine powder and a carbon source followed by firing to synthesize silicon microcrystalline silicon powder and treating the microcrystalline silicon with thermal plasma to produce silicon carbide, But the uniformity was not good due to the mixing of large particles of 200 nm or more and small nano particles of about 20 to 30 nm.
The present invention relates to a solid-state reaction and thermal plasma which can attain both the nano-effect of a sintering aid and the sintering effect of a liquid phase reaction, and can produce a Si / SiC nanocomposite powder with high dispersibility and specific surface area, uniform particle size, And a method for producing Si / SiC nanocomposite powder using a pyrolysis process.
According to an aspect of the present invention,
a) mixing silicon powder and carbon powder homogeneously and synthesizing SiC fine powder through solid phase reaction in a state where argon is charged;
and b) preparing a Si / SiC nanocomposite powder by treating the SiC fine powder with a thermal plasma to provide a Si / SiC nanocomposite powder using the solid phase reaction and thermal plasma pyrolysis process do.
Particularly, the solid state reaction in step a) is preferably carried out at 1300 ° C in a state where argon is introduced. Further, the solid state reaction in step a) is preferably performed at 1300 ° C in a state where a mixed gas of argon and hydrogen is introduced.
In the step b), it is preferable that the SiC fine powder is treated with a thermal plasma in a state where argon syrup and hydrogen gas are supplied, and the thermal plasma treatment is preferably performed at a current of 50 to 300 A and a voltage of 5 to 50 V. Particularly, it is preferable that the thermal plasma treatment is performed at a current of 300A and a voltage of 45V.
Hereinafter, the method for producing Si / SiC nanocomposite powder using solid-state reaction and thermal plasma pyrolysis process of the present invention will be described in detail.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a process flow chart showing a method of producing the Si / SiC nanocomposite powder of the present invention.
The method of producing the Si / SiC nanocomposite powder of the present invention mainly includes the step of synthesizing the SiC fine powder and the step of producing the Si / SiC nanocomposite powder.
First, in the step of synthesizing the SiC fine powder, the silicon powder and the carbon powder are homogeneously mixed, and the solid phase reaction is performed to synthesize the SiC fine powder in a state where argon is introduced.
Although the kind and the particle diameter of the silicon powder and the carbon powder are not particularly limited, it is preferable to use a powder having a particle size of 100 μm or less for activation of the solid-phase reaction. Meanwhile, in the embodiment of the present invention, the silicon powder was pulverized into a powder having a particle size of 10 to 50 탆, and a carbon powder having a particle size of 5 to 50 탆 was used.
The silicon powder and the carbon powder are uniformly mixed using a ball mill which can be uniformly pulverized and mixed.
The solid phase reaction is preferably carried out at 1300 占 폚 at a high temperature while argon is introduced. When firing in the state of argon is fired, it is possible to prevent the oxidation of silicon, and at the same time, the carbon component diffuses and penetrates into the silicon crystal to form new crystals of SiC. In this process, And the SiC fine powder is synthesized.
Particularly, it is more preferable to sinter at a high temperature at 1300 캜 in a state where a mixed gas of argon and hydrogen is added. This is because the hydrogen introduced with argon can increase the brittleness of SiC crystals in the process of producing SiC crystals and can further promote the atomization of SiC crystals, thereby making it possible to synthesize uniform SiC particulate powders having a particle size of 0.2 to 2.5 μm have.
As the SiC crystal is atomized, the SiC powder is easily nanoized by the thermal plasma treatment, and the SiC thermally decomposing reaction can be easily performed. Therefore, the Si / SiC nanocomposite powder production rate can be improved.
Next, in the step of preparing the Si / SiC nanocomposite powder, the SiC fine powder is treated with a thermal plasma to produce a Si / SiC nanocomposite powder.
At this time, the thermal plasma converts the SiC particulate powder into the Si / SiC nanocomposite powder by applying the non-transfer plasma. When the SiC fine powder is injected into the flame of the non-transfer type arc plasma through the quantitative feeder, the SiC fine powder is temporarily melted in the plasma space. At this time, the molten SiC powder The SiC nano powder is separated into Si and C and adhered to other SiC nano powder to form Si / SiC nanocomposite powder.
In order to effectively form the Si / SiC nanocomposite powder, the thermal plasma treatment is preferably performed at a current of 300 A and a voltage of 45 V.
delete
Since the method of producing Si / SiC nanocomposite powder of the present invention uses silicon powder in solid state and carbon powder as raw materials, it is economical to produce Si / SiC nanocomposite powder at low cost and has a dispersing property and a specific surface area SiC / SiC nanocomposite powder having a high grain size and uniform particle size can be produced. Especially, when the Si / SiC nanocomposite powder is used as a sintering aid for SiC, the effect of SiC nano- It is expected that a high-density SiC sintered body can be manufactured at 2000 DEG C or less.
BRIEF DESCRIPTION OF DRAWINGS FIG. 1 is a process flow chart schematically showing a method of producing a Si / SiC nanocomposite powder of the present invention.
2 is a scanning electron microscope (SEM) image of a metal silicon powder used in Example 1 of the present invention,
3 is a scanning electron microscope (SEM) image of the activated carbon used in Example 1 of the present invention.
4 is an XRD result of the SiC fine powder synthesized by solid state reaction in Example 1,
5 is a scanning electron microscope (SEM) image of the SiC fine powder synthesized by the solid state reaction of Example 1,
FIG. 6 is a transmission electron microscope photograph showing the characteristics of the SiC fine powder synthesized by solid state reaction in Example 1. FIG.
7 is an XRD result of the SiC fine powder synthesized by solid state reaction in Example 2,
8 is a scanning electron microscope (SEM) image of the SiC fine powder synthesized by the solid state reaction of Example 2,
Fig. 9 is a transmission electron microscope image of the characteristics of the SiC fine powder synthesized by solid state reaction in Example 2. Fig.
10 is an XRD result of the Si / SiC nanocomposite powder produced by the thermal plasma treatment of Example 3. Fig.
11 is a scanning electron microscope (SEM) image of the Si / SiC nanocomposite powder prepared by the thermal plasma treatment of Example 3,
FIG. 12 is a transmission electron microscope (SEM) image of the Si / SiC nanocomposite powder prepared by the thermal plasma treatment of Example 3. FIG.
13 is a high-resolution transmission electron micrograph showing the characteristics of the Si / SiC nanocomposite powder produced by the thermal plasma treatment of Example 3. Fig.
14 is an XRD result of the Si / SiC nanocomposite powder produced by the thermal plasma treatment of Example 4. Fig.
FIG. 15 is a transmission electron microscope image of the characteristics of the Si / SiC nanocomposite powder produced by the thermal plasma treatment of Example 4. FIG.
Hereinafter, the method for producing the Si / SiC nanocomposite powder using the solid-phase reaction and thermal plasma pyrolysis process of the present invention will be described in more detail. The scope of the present invention is not limited to the following examples.
[Example 1] Production of SiC fine powder: In the argon gas,
Silicon powders and carbon powders were used to prepare mixed samples. A metal silicon powder was used as the silicon powder, and a scanning electron microscope photograph showing the characteristics thereof is shown in Fig. Activated carbon was used as a carbon powder, and a scanning electron microscope photograph showing the characteristics thereof is shown in FIG.
The mixing ratio of Si: C in the mixture of the silicon powder and the carbon powder was 1.5 mol based on the Si 1 mole of the silicon powder. The weighed silicon powder and the carbon powder were mixed in a plastic container of 200 mL filled with zirconia balls in a volume of 1/3 volume for 12 hours. The mixed samples were calcined at 1300 ° C for 2 hours using a vertical tubular electric furnace. In order to prevent the oxidation of Si during the firing process, firing was carried out while flowing argon gas at a flow rate of 1 L / min into the firing furnace. After the calcination, the synthesized SiC powder was subjected to ultrasonic cleaning once to remove unreacted carbon and stored in an oven at 80 ° C for 12 hours for drying.
XRD analysis was carried out to investigate the degree of SiC synthesis and the crystal structure of the SiC fine powder thus obtained, and the results are shown in FIG. XRD analysis showed that unreacted Si other than SiC was not detected and pure SiC was formed. The crystal structure of synthesized SiC showed mostly β - phase SiC and very small amount of α - phase SiC.
5 and 6 are a scanning electron microscope and a transmission electron microscope photograph taken to confirm the shape and particle diameter of the synthesized SiC fine particle powder. The shape of the SiC fine powder synthesized from the scanning electron microscope photograph of FIG. 5 was amorphous, and the grain size was in the range of 0.5 to 4 μm, which was about 10 times smaller than the grain size of the raw material sample. The transmission electron microscope image of FIG. 6 shows that one large SiC powder was formed by coalescence of small particles (primary particles), and the primary SiC particles had a particle size of 30 to 50 nm. BET analysis was performed to determine the specific surface area of the synthesized SiC fine powder, and the specific surface area was 23.6 m 2 / g.
[Example 2] Production of SiC fine powder: In the argon / hydrogen mixed gas,
A vertical tubular electric furnace was calcined at 1300 ° C. for 2 hours and a mixed tube of the same silicon powder and carbon powder as in Example 1 was treated with argon / hydrogen The mixed sample was sintered in a state of supplying the mixed gas to synthesize the SiC fine powder of Example 2. At this time, argon / hydrogen mixed gas was supplied into the calcination furnace at a flow rate of 1 L / min with 5 vol% H 2 mixed argon gas.
After the calcination, the synthesized SiC powder was subjected to ultrasonic cleaning once to remove unreacted carbon and stored in an oven at 80 ° C for 12 hours for drying.
The results of XRD analysis of the SiC fine powder of Example 2 synthesized above are shown in FIG. 7, and it can be confirmed that the same SiC crystals as the SiC fine powder obtained in Example 1 were synthesized.
8 and 9 are a scanning electron microscope and a transmission electron micrograph showing the shape and particle diameter of the synthesized SiC fine powder of Example 2. Fig. It can be seen that the shape of the SiC fine powder synthesized from the scanning electron microscope photograph of FIG. 8 is amorphous and the particle diameter is smaller than the particle size of the SiC fine powder obtained in Example 1 in the range of 0.2 to 2.5 μm. Also, in the transmission electron microscope photograph of FIG. 9, the particle size of the primary SiC particles is 20 to 30 nm, which is smaller than the particle size of the primary SiC particles of Example 1 and excellent in dispersibility.
The specific surface area by BET analysis was investigated to confirm the dispersibility of the synthesized SiC fine powder, and the specific surface area was found to be 40.6 m 2 / g. This is 1.7 times higher than the specific surface area of the SiC fine powder obtained in Example 1. [
That is, it can be seen from the experimental results of Example 1 and Example 2 that the addition of the hydrogen gas led to the refinement of the SiC powder. In the course of the SiC crystal formation, hydrogen was added to increase the brittleness of the SiC crystal, and it was judged that the atomization of SiC proceeded further. In the solid phase reaction of Si and the carbon powder, a mixed gas of argon and hydrogen Is preferable for atomization of the SiC powder.
[Example 3] Production of Si / SiC nanocomposite powder
SiC fine powder synthesized in Example 2 was supplied to a non-transfer type DC thermal plasma reactor to prepare Si / SiC nanocomposite powder. At this time, the sample feed rate was 0.45 g / min and the flow rate of the powder transport gas was set to 1 L / min. In addition, the output condition of the power source of the arc thermal plasma generator was a current of 200 A and a voltage of 40 V, and argon gas and hydrogen gas were used as gas for plasma flame formation.
XRD analysis was performed to observe the phase change and crystal structure change of the SiC fine powder after the thermal plasma treatment, and the results are shown in FIG. From the XRD analysis, it was found that β-phase and a small amount of α-phase SiC were observed, and Si / SiC nanocomposite powder was formed due to addition of Si phase.
11 and 12 show photographs of a scanning electron microscope and a transmission electron microscope after plasma treatment of the synthesized SiC fine powder of Example 2. Fig. From the photograph of the scanning electron microscope of FIG. 11, it can be seen that Si / SiC nanocomposite powder of 100 nm or less is formed in a very uniform state. The transmission electron microscope image of FIG. 12 also shows that the Si / SiC nanocomposite powder was also formed within the range of 20 to 80 nm.
13 shows a high-resolution transmission electron microscope photograph taken to observe the presence and shape of the Si / SiC nanocomposite powder. In Fig. 13, the (111) plane of the SiC crystal and the (111) plane of the Si crystal were observed, and the plane spacing was 0.214 nm and 0.306 nm, respectively. From these results, it can be seen that metal Si is adhered on the surface of SiC at a size of about 10 nm.
[Example 4] Production of Si / SiC nanocomposite powder
Si / SiC nanocomposite powder was produced under the same conditions as in Example 3 by raising the output condition of the power supply of the arc thermal plasma generator to a current of 300 A and a voltage of 45 V.
XRD analysis was performed to observe the phase change and the crystal structure change of the SiC fine powder after thermal plasma treatment, and the results are shown in Fig. It can be seen that the X-ray diffraction intensity of the Si phase is greatly increased as compared with the XRD analysis result of Example 3. This is because the generation of the Si phase is increased due to the activation of the pyrolysis reaction of the SiC powder as the output of the thermal plasma increases.
Fig. 15 is a photograph of a transmission electron microscope. It can be seen that the particle diameter of the Si / SiC nano powder was within the range of 10 to 50 nm, and the particle diameter was smaller than that of Example 3.
Claims (6)
b) treating the SiC fine powder with a thermal plasma to produce a Si / SiC nanocomposite powder,
The solid phase reaction in step a) is carried out at 1300 캜 for 2 hours in a state where a mixed gas of argon and hydrogen is introduced,
Wherein the thermal plasma process in the step b) is performed at a current of 300 A and a voltage of 45 V. The method for producing Si / SiC nanocomposite powder using the solid-phase reaction and thermal plasma pyrolysis process.
Wherein the step b) comprises treating the Si / SiC nanocomposite powder with a thermal plasma in the state where argon syrup and hydrogen gas are introduced.
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Cited By (2)
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CN109607539A (en) * | 2019-01-31 | 2019-04-12 | 杭州致德新材料有限公司 | High-dispersion nano silicon carbide and preparation method thereof |
KR20200142734A (en) * | 2019-06-13 | 2020-12-23 | 주식회사 카보넥스 | Fabrication method of sintered SiC and sintered SiC using thereof |
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JP2006001779A (en) | 2004-06-16 | 2006-01-05 | National Institute For Materials Science | Method for producing sic nanoparticles by nitrogen plasma |
KR20110112223A (en) * | 2010-04-06 | 2011-10-12 | 다카시 도미타 | Method and system for manufacturing silicon and silicon carbide |
KR20120121109A (en) | 2011-04-26 | 2012-11-05 | (주)네오플랜트 | Production method for nano-sized silicone carbide using thermal plasma |
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CN109607539A (en) * | 2019-01-31 | 2019-04-12 | 杭州致德新材料有限公司 | High-dispersion nano silicon carbide and preparation method thereof |
CN109607539B (en) * | 2019-01-31 | 2020-01-24 | 杭州致德新材料有限公司 | High-dispersion nano silicon carbide and preparation method thereof |
KR20200142734A (en) * | 2019-06-13 | 2020-12-23 | 주식회사 카보넥스 | Fabrication method of sintered SiC and sintered SiC using thereof |
KR102281102B1 (en) | 2019-06-13 | 2021-07-23 | 주식회사 카보넥스 | Fabrication method of sintered SiC and sintered SiC using thereof |
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