WO2023167387A1 - Méthode de synthèse de poudre de carbure de silicium - Google Patents

Méthode de synthèse de poudre de carbure de silicium Download PDF

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Publication number
WO2023167387A1
WO2023167387A1 PCT/KR2022/017961 KR2022017961W WO2023167387A1 WO 2023167387 A1 WO2023167387 A1 WO 2023167387A1 KR 2022017961 W KR2022017961 W KR 2022017961W WO 2023167387 A1 WO2023167387 A1 WO 2023167387A1
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powder
silicon carbide
crucible
carbide powder
temperature
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PCT/KR2022/017961
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English (en)
Korean (ko)
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서태일
최규채
김동훈
이가형
전구식
서민혁
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주식회사 에스티아이
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Publication of WO2023167387A1 publication Critical patent/WO2023167387A1/fr

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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/97—Preparation from SiO or SiO2

Definitions

  • the present invention relates to a method for synthesizing silicon carbide powder, and more particularly, by synthesizing using a crucible having an inner wall uniformly coated with silicon carbide powder, the yield of the synthesized silicon carbide powder is improved, and in the synthesis process It relates to a method for synthesizing silicon carbide powder in which the average particle size of the silicon carbide powder can be easily controlled by appropriately adjusting the temperature difference between the upper and lower parts of the crucible so that the particle size distribution of the silicon carbide powder is formed narrowly.
  • Silicon carbide (SiC) is physically and chemically stable, has good heat resistance and thermal conductivity, and has excellent high-temperature stability, high-temperature strength and wear resistance. Accordingly, silicon carbide powder is widely used in the manufacture of high-temperature materials, high-temperature semiconductors, wear-resistant materials, automobile parts, and the like.
  • the above silicon carbide powder can be synthesized by mixing powder raw materials such as silicon source and carbon source and then applying heat and pressure. In the synthesis step, the synthesis yield and purity of the synthesized silicon carbide powder are increased, It is a very important task to easily adjust the average particle size by narrowing the particle size distribution of the silicon powder.
  • the step of synthesizing the silicon carbide powder by applying heat and pressure to the mixed silicon source and carbon source is very important.
  • a method of increasing the synthesis yield and purity of silicon carbide powder synthesized by changing the method has been proposed.
  • Korean Patent Publication No. 10-2012-0012345 proposes a technique for improving the purity of silicon carbide powder by limiting the molar ratio of the carbon source to the silicon source.
  • Korean Patent Registration No. 10-1601282 has a problem in that the cost of manufacturing the device increases due to the need to change the structure of the crucible, and Korean Patent Publication No. 10-2012-0012345 simply synthesizes silicon carbide There is a problem in that the average particle size cannot be adjusted by narrowing the particle size distribution of the synthesized silicon carbide powder, only improving the purity of the powder.
  • An object of the present invention is to solve the above problems, and an object of the present invention is not only to improve the yield of synthesized silicon carbide powder by synthesizing using a crucible with silicon carbide powder uniformly coated on the inner wall, An object of the present invention is to provide a method for synthesizing silicon carbide powder in which the average particle size of the silicon carbide powder can be easily controlled by appropriately adjusting the temperature difference of the upper and lower parts of the crucible in the synthesis process so that the particle size distribution of the silicon carbide powder is formed narrowly.
  • the step of preparing a mixed powder by mixing silica (SiO 2 ) powder and carbon (C) powder at a predetermined ratio, and putting the prepared mixed powder into a crucible at 1550 to 1900 ° C.
  • a method for synthesizing silicon carbide powder comprising the step of synthesizing silicon carbide powder by heat treatment at a synthesis temperature of ⁇ 2350 ° C.
  • the mixed powder prepared in the mixed powder preparation step and the mixed powder re-preparation step is mixed at a weight ratio of silica (SiO 2 ) powder and carbon (C) powder in a ratio of 1: 0.3 to 1: 1.3. do.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at 90 to 150 ° C.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at -20 to 50 ° C.
  • the crucible on which the coating step has been completed is cooled at a natural cooling rate of 3 ° C. / min while maintaining an inert gas atmosphere of 400 to 750 torr. do.
  • the step of synthesizing the silicon carbide powder after raising the temperature to the synthesis temperature at a heating rate of 5 to 12 ° C / min in an inert gas atmosphere of 400 to 750 torr, it is characterized in that heat treatment for 0.5 to 3 hours.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at 50 to 100 ° C.
  • the silica (SiO 2 ) powder has a purity of 99.999% or more and an average particle size of 50 to 300 nm
  • the carbon (C) powder has a purity of 99.99% or more and an average particle size of 1 to 10 ⁇ m.
  • the yield of the synthesized silicon carbide powder is improved as the synthesis is performed using a crucible in which the silicon carbide powder is uniformly coated on the inner wall.
  • the present invention can easily control the average particle size of the silicon carbide powder by appropriately adjusting the temperature difference between the upper and lower parts of the crucible during the synthesis process to narrow the particle size distribution of the silicon carbide powder.
  • FIG. 1 shows a process flow chart of a method for synthesizing silicon carbide powder according to an embodiment of the present invention.
  • Figure 2 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Example 1 of the present invention.
  • Figure 3 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Example 2 of the present invention.
  • Figure 4 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Example 3 of the present invention.
  • FIG. 1 is a process flow diagram of a method for synthesizing silicon carbide powder according to an embodiment of the present invention.
  • the method for synthesizing silicon carbide powder includes a mixed powder preparation step (S1), a silicon carbide powder coating step (S2), a silicon carbide powder and unreacted mixed powder removal step ( S3), a mixed powder re-preparation step (S4), a silicon carbide powder synthesis step (S5), and a carbon removal step (S6).
  • silica (SiO2) powder with a purity of 99.999% or more and an average particle size of 50 to 300 nm and carbon (C) powder with a purity of 99.99% or more and an average particle size of 1 to 10 ⁇ m are mixed in a ratio of 1:0.3 to 1:1.3. to prepare a mixed powder.
  • the mixed powder is uniformly mixed using a ball mill, but a high-purity synthetic quartz ball and tube are used to prevent impurities from entering.
  • the prepared mixed powder is put into a carbon material crucible and heated to a synthesis temperature of 1550 to 1900 ° C at a heating rate of 4 to 9 ° C / min in an inert gas atmosphere of 400 to 750 torr.
  • a heating rate of 4 to 9 ° C / min in an inert gas atmosphere of 400 to 750 torr.
  • the inner wall of the crucible is coated with silicon carbide (SiC) powder.
  • argon gas may be used as the inert gas, but the present invention is not limited thereto.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at 90 to 150 ° C.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at -20 to 50 ° C.
  • the reason for maintaining the temperature difference between the lower outer wall of the crucible and the upper outer wall of the crucible at 90 to 150 ° C in the process of raising the temperature to the synthesis temperature is to ensure that the silicon carbide powder synthesized inside the crucible is uniformly applied to the inner wall of the crucible as a whole. am.
  • the temperature difference between the lower part of the outer wall of the crucible and the upper part of the outer wall of the crucible is 90 ° C or less
  • the diffusion and convection of the synthesized vapor phase silicon carbide is not performed smoothly because the width of the temperature change is not large. This is because it is difficult to uniformly coat the vapor phase silicon carbide on the inner wall of the crucible made of carbon material.
  • the reason why the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at -20 to 50 ° C during the heat treatment process is that the temperature deviation of the upper and lower parts of the crucible is reduced and the temperature of the entire crucible is maintained uniformly, so that the gas phase synthesized inside the crucible is maintained. This is to ensure that the silicon carbide is uniformly convected and diffused inside the crucible so that the silicon carbide powder is uniformly applied to the entire inner wall of the crucible.
  • silicon (Si) generated from silica (SiO2) does not react with carbon (C) of the crucible material in the step of synthesizing silicon carbide powder, which will be described later.
  • the crucible on which the coating step has been completed is cooled at a natural cooling rate of 3°C/min while maintaining an inert gas atmosphere of 400 to 750 torr, and then synthesized inside the crucible and then applied to the inner wall of the crucible. Uncoated silicon carbide powder and unreacted mixed powder are removed.
  • argon gas may be used as the inert gas, but the present invention is not limited thereto.
  • the reason for cooling the crucible for which the coating step has been completed in this step at a natural cooling rate of 3°C/min is that the silicon carbide powder applied to the inner wall of the crucible made of carbon material is separated from the inner wall of the crucible due to shrinkage or thermal stress caused by rapid cooling. This is to prevent (S3)
  • silica (SiO2) powder with a purity of 99.999% or more and an average particle size of 50 to 300 nm and carbon (C) powder with a purity of 99.999% or more and an average particle size of 1 to 10 ⁇ m are mixed at a ratio of 1:0.3 to 1:1.3. Mix to re-prepare the mixed powder.
  • the mixed powder is uniformly mixed using a ball mill, but a high-purity synthetic quartz ball and tube are used to prevent impurities from entering the mixed powder.
  • the prepared mixed powder is put into a crucible coated with silicon carbide powder and heated to a synthesis temperature of 1850 to 2350 ° C at a heating rate of 5 to 12 ° C / min in an argon atmosphere of 400 to 750 torr, Silicon carbide (SiC) powder is synthesized inside the crucible by heat treatment for 0.5 to 3 hours.
  • SiC Silicon carbide
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible is maintained at 50 to 100 ° C.
  • the reason why the temperature difference between the lower outer wall of the crucible and the upper part of the outer wall of the crucible is maintained at 50 to 100 ° C is that the average particle size of the silicon carbide powder is easily controlled by narrowing the particle size distribution of the synthesized silicon carbide powder. is to do
  • the overall temperature of the crucible becomes similar, so that the synthesis of silicon carbide powder does not take place primarily at the bottom of the crucible, but partially moves to the upper part of the crucible.
  • the desired average particle size of the synthesized silicon carbide powder because the particle size of the silicon carbide powder decreases and the particle size distribution widens at the same time as the amount of the silicon carbide powder synthesized to a small particle size increases.
  • carbon is removed by heat treatment in an air atmosphere of 700 to 950 ° C. for 0.5 to 5 hours.
  • a mixed powder was prepared by mixing 400 g of silica (SiO2) powder having a purity of 99.999% or more and an average particle size of 50 to 300 nm and 200 g of carbon (C) powder having a purity of 99.99% or more and an average particle size of 1 to 10 ⁇ m.
  • the mixed powder was uniformly mixed using a ball mill, but a high-purity synthetic quartz ball and tube were used to prevent impurities from entering.
  • the prepared mixed powder was put into a carbon material crucible, heated to a synthesis temperature of 1800 ° C at a heating rate of 7 ° C / min in an argon atmosphere of 700 torr, and then heat-treated for 3 hours to uniformly coat the inside of the crucible with silicon carbide powder. .
  • the difference between the lower temperature of the outer wall and the upper temperature of the outer wall of the crucible is maintained at 120 °C, and in the heat treatment process, the difference between the lower temperature of the outer wall and the upper temperature of the outer wall of the crucible is maintained at 20 °C did
  • the crucible coated with the silicon carbide powder was cooled at a natural cooling rate of 3° C./min while maintaining an argon atmosphere of 700 torr, and then the uncoated silicon carbide powder and unreacted mixed powder were removed from the inner wall of the crucible.
  • a mixed powder was prepared by mixing 400 g of silica (SiO2) powder having a purity of 99.999% or more and an average particle size of 50 to 300 nm and 200 g of carbon (C) powder having a purity of 99.99% or more and an average particle size of 1 to 10 ⁇ m.
  • the mixed powder was uniformly mixed using a ball mill, but a high-purity synthetic quartz ball and tube were used to prevent impurities from entering.
  • the difference between the lower temperature of the outer wall of the crucible and the upper temperature of the outer wall of the crucible was maintained at 70 ° C.
  • Example 2 is different from Example 1 only in that the synthesis temperature for synthesizing the silicon carbide powder is lowered to 2150 ° C., and the rest is the same as Example 1, so a detailed description thereof will be omitted.
  • Example 3 is different from Example 1 only in that the synthesis temperature for synthesizing the silicon carbide powder is lowered to 1850 ° C., and the rest is the same as Example 1, so a detailed description thereof will be omitted.
  • Comparative Example 1 only the coating step of the silicon carbide powder in Example 1 was performed, and a detailed description thereof will be omitted.
  • Comparative Example 2 was performed only after the re-preparation step of the mixed powder in Example 1, and a detailed description thereof will be omitted.
  • Example 3 the only difference is that the mixed powder prepared in Example 1 is mixed with 240 g of silica (SiO2) powder and 360 g of carbon (C) powder, and the rest is the same as Example 1, so a detailed description thereof should be omitted.
  • SiO2 silica
  • C carbon
  • Examples 1 to 3 synthesized according to an embodiment of the present invention had an average yield of 37% and an impurity content of about 6.9 ppm, compared to Comparative Examples 1 to 3. It was confirmed that the synthesis yield of the silicon carbide powder was improved and the purity was high due to the low impurity content.
  • Comparative Example 1 the yield of silicon carbide powder was lowered as silicon (Si) generated from silica (SiO2) during the synthesis process was applied to the inside of the carbon material crucible, and unreacted carbon due to lack of silicon (Si) The purity was lowered due to the influence of (C).
  • Comparative Example 2 As in Comparative Example 1, the yield of silicon carbide powder was lowered as silicon (Si) generated from silica (SiO2) in the synthesis process was applied to the inside of the carbon material crucible, but compared to Comparative Example 1, the upper and lower parts of the crucible Since the temperature deviation of is large, silicon (Si) generated from silica (SiO2) is applied only to the upper and lower parts of the inside of the carbon material crucible, resulting in an increased synthesis yield compared to Comparative Example 1, and unreacted carbon due to lack of silicon (Si) ( C) and the influence of carbon introduced from the inner wall of the crucible to which silicon (Si) is not applied, the purity is lower than that of Comparative Example 1.
  • Comparative Example 3 an excessive amount of carbon (C) was added compared to silica (SiO 2 ), resulting in a low synthesis yield of silicon carbide powder and a relatively large amount of carbon, resulting in low purity.
  • Comparative Examples 1 to 3 all of Comparative Examples 1 to 3 had an excess of carbon, and the excess of carbon affected the synthesis process of silicon carbide, resulting in a low synthesis yield of silicon carbide powder, and inappropriate time and conditions in the carbon removal step. Therefore, it can be inferred that the carbon not sufficiently removed has an effect on the purity.
  • Figure 2 is a graph showing the particle size distribution of silicon carbide powder synthesized according to Example 1 of the present invention
  • Figure 3 is a graph showing the particle size distribution of silicon carbide powder synthesized according to Example 2 of the present invention
  • Figure 4 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Example 3 of the present invention
  • FIG. 5 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Comparative Example 1
  • FIG. 7 is a graph showing the particle size distribution of the silicon carbide powder synthesized according to Comparative Example 3.
  • the X-axis of the graph represents the particle size of the synthesized silicon carbide powder in units of ⁇ m
  • the Y-axis of the graph represents the number of particles
  • the silicon carbide powders of Examples 1 to 3 synthesized according to the synthesis method according to an embodiment of the present invention are concentrated in a narrow particle size range. It was confirmed that the particle size distribution was formed narrowly.
  • the synthesis method according to an embodiment of the present invention can more easily control the average particle size of the synthesized silicon carbide powders.
  • Examples 1 to 3 synthesized according to the synthesis method according to an embodiment of the present invention adjust the synthesis temperature at which silicon carbide powder is synthesized to obtain a particle size of 5 to 280 ⁇ m. It was confirmed that silicon carbide powders having various average particle sizes could be obtained.
  • the silicon carbide powders synthesized according to the synthesis method according to Comparative Examples 1 to 3 are dispersed within a wide particle size range, resulting in a particle size distribution. It was found that it was widely formed.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne une méthode de synthèse de poudre de carbure de silicium, la méthode comprenant : une étape de préparation de poudre mélangée par mélange de poudre de silice (SiO2) et de poudre de carbone (C) à un rapport constant ; une étape de revêtement de la paroi interne d'un creuset avec de la poudre de carbure de silicium (SiC) par ajout de la poudre mélangée préparée dans le creuset et traitement thermique de celle-ci à une température de synthèse de 1550 à 1900°C ; après refroidissement du creuset ayant subi l'étape de revêtement, une étape d'élimination de la poudre de carbure de silicium synthétisée et de la poudre mélangée n'ayant pas réagi de l'intérieur du creuset ; une étape de re-préparation de poudre mélangée par mélange de poudre de silice (SiO2) et de poudre de carbone (C) à un rapport constant ; et une étape de synthèse de poudre de carbure de silicium par ajout de la poudre mélangée repréparée dans le creuset avec de la poudre de carbure de silicium revêtue sur la paroi interne et traitement thermique de celle-ci à une température de synthèse de 1850 à 2350°C. Selon l'invention telle que décrite ci-dessus, à mesure que la synthèse est effectuée à l'aide du creuset avec de la poudre de carbure de silicium uniformément revêtue sur la paroi interne, le rendement de poudre de carbure de silicium synthétisée peut être amélioré. De plus, dans le procédé de synthèse de la présente invention, la distribution de taille de particule de poudre de carbure de silicium est rétrécie par ajustement approprié d'une variation de température entre les parties supérieure et inférieure du creuset, et par conséquent, la taille moyenne de particule de poudre de carbure de silicium peut être facilement contrôlée.
PCT/KR2022/017961 2022-03-04 2022-11-15 Méthode de synthèse de poudre de carbure de silicium WO2023167387A1 (fr)

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KR102407043B1 (ko) * 2022-03-04 2022-06-10 주식회사 에스티아이 탄화규소 분말의 합성방법
KR102581526B1 (ko) * 2022-08-22 2023-09-20 주식회사 쎄닉 탄화규소 분말, 이의 제조방법 및 이를 이용하여 탄화규소 잉곳을 제조하는 방법

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