WO2013055016A1 - Procédé de production pour poudre de carbure de silicium et poudre de carbure de silicium ainsi produite - Google Patents

Procédé de production pour poudre de carbure de silicium et poudre de carbure de silicium ainsi produite Download PDF

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WO2013055016A1
WO2013055016A1 PCT/KR2012/005671 KR2012005671W WO2013055016A1 WO 2013055016 A1 WO2013055016 A1 WO 2013055016A1 KR 2012005671 W KR2012005671 W KR 2012005671W WO 2013055016 A1 WO2013055016 A1 WO 2013055016A1
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silicon carbide
carbide powder
formula
powder
heat treatment
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PCT/KR2012/005671
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English (en)
Korean (ko)
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김영희
김수룡
권우택
이윤주
정은진
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한국세라믹기술원
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Priority claimed from KR1020110105550A external-priority patent/KR101356971B1/ko
Priority claimed from KR1020120028369A external-priority patent/KR101322796B1/ko
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Publication of WO2013055016A1 publication Critical patent/WO2013055016A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth

Definitions

  • the present invention relates to a method for producing silicon carbide powder, and more particularly, to a method for producing silicon carbide powder capable of obtaining high purity beta phase crystal silicon carbide powder in high yield and a silicon carbide powder produced thereby. .
  • Silicon carbide has high temperature stability, high thermal shock resistance, good abrasion resistance and self-lubricating activity, and is chemically excellent in acid resistance and corrosion resistance, and thus is used as abrasives, bearings, various nozzles, and high temperature structural materials.
  • abrasives bearings, various nozzles, and high temperature structural materials.
  • precise control of a high temperature process is required, and it has attracted the spotlight as a material which replaces quartz and alumina.
  • Representative methods for producing silicon carbide powder include the Acheson method, the carbon reduction method (carbothermal reduction method), the synthesis method using a gas phase reaction, liquid polymer reaction method and the like.
  • the Acheson method is a representative industrial mass production method suitable for the production of alpha-phase silicon carbide ( ⁇ -SiC), and it is used as a starting material for quartz carbide and coke as a starting material.
  • thermocarbon reduction method gas phase reaction method and liquid polymer reaction method are suitable for producing stable beta-phase silicon carbide ( ⁇ -SiC) at low temperature range, but there is a disadvantage that mass production is difficult except for thermal carbon reduction method.
  • the thermal carbon reduction method is a method of producing silicon carbide by mixing silica and carbon at a predetermined ratio and heat treatment in an inert gas atmosphere. The thermal carbon reduction method can obtain a high purity powder having a uniform particle size, and can produce silicon carbide having excellent sintered body properties.
  • Carbothermal reduction method is a method of producing silicon carbide by heat-treating silica mixed with carbon in argon atmosphere.Since the silica reacts with carbon during the heat treatment process, oxygen in the silica is formed as carbon monoxide (CO) gas and disappeared. The remaining silicon reacts with the carbon to form silicon carbide.
  • the scheme is as follows.
  • the technical problem to be solved by the present invention is that in the production of silicon carbide by thermal carbon reduction reaction, it is possible to form silicon carbide by the reaction of silicon and carbon elements uniformly, and does not require modification of existing process equipment It is possible to provide a high purity silicon carbide powder without having to provide a method for producing beta-phase silicon carbide powder having a high yield.
  • the present invention to solve the above technical problem
  • silicon carbide precursor Heat treating the silicon carbide precursor at 1,400-2,200 ° C. under a gas atmosphere selected from vacuum or helium, neon, and argon to produce silicon carbide powder, wherein the silicon carbide precursor is a high carbon silica powder mixed with silica and carbon; ; Or a siloxane polymer, a silsesquioxane polymer, and a mixture of two or more of these polymers.
  • the high-carbon silica powder composed of the siloxane polymer, the silsesquioxane polymer and a mixture of two or more of these polymers includes two or more of the silicon-alkoxides represented by the following [Formula 1] to [Formula 3].
  • the reaction mixture is characterized in that it is prepared by sol-gel reaction.
  • R is a methyl group or an ethyl group, and R 'and R "are each independently an alkyl group having 5 to 20 carbon atoms.
  • the reaction mixture is characterized in that at least any one selected from the above [Formula 2] and [Formula 3] at least 50 mol% to less than 100 mol% in the reaction mixture.
  • the high-carbon silica powder mixed with the silica and carbon is characterized in that the mixture of more than one selected from carbon black, pitch, phenolic resin and polystyrene resin.
  • the heat treatment step (a) a first heat treatment step for the carbonization reduction reaction of the silicon carbide precursor at 1,400-1,600 °C; And (b) a second heat treatment step of inducing crystallization at 1,800-1,900 ° C. after the first heat treatment, wherein the first heat treatment step starts a carbonization reduction reaction at 1,400-1,600 ° C. to 5-7 Characterized in that it is maintained for a time, the second heat treatment step is characterized in that after the first heat treatment to induce crystallization at 1,800-1,900 °C for 2-3 hours to obtain a high crystalline silicon carbide powder.
  • the step of performing a decarburization process of the silicon carbide powder prepared at 600-1000 °C under an atmosphere is performed.
  • Silicon carbide powder prepared according to the above method, wherein the purity of the beta phase crystals of silicon carbide is 99.0-99.9%, and the average particle size of the silicon carbide powder is 0.01-25 ⁇ m, and the same. To provide a silicon carbide single crystal produced.
  • beta phase silicon carbide powder can be produced at a high temperature by suppressing grain growth of silicon carbide powder, having good crystallinity, good reactivity and low particle size.
  • the heat treatment step to control the production rate of the SiO gas generated as the reaction intermediate, it is possible to produce a high purity beta-phase silicon carbide powder in a high yield by minimizing the loss of SiO gas.
  • it is possible to manufacture a high yield, high purity silicon carbide powder without changing the process equipment by the existing thermal carbon reduction reaction is excellent in process efficiency.
  • thermogravimetric analysis performed in Preparation Example 1 of the present invention.
  • Example 2 is an X-ray diffraction analysis of the silicon carbide powder prepared in Example 1, Example 2 of the present invention. (a) Example 1, (b) Example 2
  • Figure 3 is a scanning electron micrograph of the silicon carbide powder prepared in Example 1, Example 2 of the present invention.
  • (a) Example 1 (b) Example 2
  • Figure 4 is an X-ray diffraction analysis of the silicon carbide powder prepared in Example 3 of the present invention.
  • Example 5 is a scanning electron micrograph of the silicon carbide powder prepared in Example 3 of the present invention.
  • Example 6 is an X-ray diffraction analysis result of the silicon carbide powder subjected to the decarburization process prepared in Example 3 of the present invention.
  • Example 7 is a transmission electron microscope photograph of the silicon carbide powder subjected to the decarburization process prepared in Example 3 of the present invention.
  • Example 8 is an X-ray diffraction analysis of the silicon carbide powder prepared in Example 4 of the present invention.
  • Example 9 is a result of FE-SEM analysis of the silicon carbide powder prepared in Example 4 of the present invention.
  • 13a and 13b are scanning electron micrographs of the silicon carbide powder prepared in Examples 5 and 6 of the present invention.
  • (a) Example 1 (b) Example 2
  • FIG. 16 is 29 Si-NMR of an intermediate subjected to pyrolysis on a high carbon silica powder prepared from silicon-alkoxide.
  • 17 is a 29 Si MAS NMR of an intermediate subjected to pyrolysis of silica sol-resin powder prepared according to Preparation Example 2 of the present invention.
  • Method for producing a silicon carbide powder according to the invention is characterized in that the silicon carbide precursor is prepared by heat treatment at 1,400-2,200 °C in a gas atmosphere selected from vacuum or helium, neon and argon, the silicon carbide precursor is silica and carbon It is characterized by being a mixed high carbon silica powder, or a siloxane polymer, a silsesquioxane polymer and a mixture of two or more of these polymers.
  • the heat treatment step is a first heat treatment step for starting the reaction in the temperature range of 1,400-1,600 °C, the temperature at which the silicon carbide precursor begins to thermal carbon reduction, at the same time the silicon carbide starts to form, and 1,800 Comprising a second heat treatment step to complete the crystallization reaction in the range of -1,900 °C for 2-3 hours to form a high purity crystalline silicon carbide powder.
  • the beta phase silicon carbide powder In order to manufacture the beta phase silicon carbide powder by the thermal carbon reduction method using the silicon carbide precursor, it is generally reacted by heat treatment at high temperature.
  • the reaction of [Formula 2-1] occurs explosively in the range of 1,400-1,600 ° C.
  • the reaction of [Formula 2-1] is faster than the reaction of [Formula 2-2], when the heat treatment is performed in the range of 1,600-1,800 ° C., the loss of SiO gas is very large.
  • reaction temperature 1,800 ° C. or more is required, so a second heat treatment step in the range of 1,800-1,900 ° C. is required, thereby increasing the yield of about 20%. It is possible to obtain silicon carbide in the phase.
  • the first heat treatment step temperature is preferably performed in the range of 1,400 ° C. to 1,600 ° C.
  • Silicon carbide can be produced only by the first heat treatment step, but the silicon carbide obtained in the first heat treatment step forms small particles having a low crystallinity of 1 ⁇ m or less, so that 1,900 ° C. to 1,900 ° C. can be used to prepare high crystalline and high purity powder.
  • a step is required to complete the reaction in the range of.
  • the step of calcining the silicon carbide precursor at 800-1,000 °C prior to the first heat treatment step may be further included.
  • the present invention is carried out a decarburization process at 600-1000 °C the silicon carbide powder prepared under an atmospheric atmosphere
  • the method may further include performing the step.
  • All of the above heat treatment process may be carried out in an inert atmosphere or a vacuum state of helium (He), neon (Ne), argon (Ar), and the like, preferably in an argon atmosphere.
  • silicon carbide precursor used in the production of the silicon carbide powder according to the present invention not only a mixed powder in which silica and carbon are most widely used, but also a silica sol-resin mixture and a silicon-based siloxane polymer may be used. . More preferably, in the pyrolysis process, silicon oxycarbide (SiOC) having a C-Si-O network may be formed in an intermediate step, and a high carbon silica powder or siloxane polymer prepared from silicon-alkoxide may be used. Can be.
  • SiOC silicon oxycarbide
  • the high carbon silica powder is prepared by sol-gel reaction of a reaction mixture containing two or more of the silicon-alkoxides represented by the following [Formula 1] to [Formula 3]. It is done.
  • R is a methyl group or an ethyl group, and R 'and R "are each independently an alkyl group having 5 to 20 carbon atoms.
  • the silicon-alkoxide is carried out in two or more kinds of the silicon-alkoxides represented by the above [Formula 1] to [Formula 3], preferably selected from [Formula 2] or [Formula 3] in the reaction mixture At least one or more must be included.
  • the reaction mixture forms a silica powder including R ′ or R ′′ by a sol-gel reaction.
  • R 'or R is pyrolyzed to leave carbon, and thus may be supplied with carbon required for SiC manufacturing.
  • At least one or more selected from the above [Formula 2] or [Formula 3] is preferably contained in the reaction mixture in more than 50 mol% or less than 100 mol%.
  • the reaction mixture includes at least any one or more selected from [Formula 2] or [Formula 3] as the content, the higher the number of R ′ or R ′′ participating in the reaction, the greater the amount of carbon and silicon carbide
  • the excess carbon that does not participate in the formation has the effect of obtaining high-crystalline silicon carbide while controlling the growth of the silicon carbide formed at the heat treatment temperature of the present invention.
  • the silicon atom includes at least one carbon as a neighboring element.
  • silicon oxycarbide having a C-Si-O network it is more effective to control the rate of SiO gas generation in the range of 1,400-1,600 ° C. as compared with the case where the silica and the carbon element are physically mixed.
  • the improved total yield is difficult to show more than 70% with respect to the yield improvement.
  • the basic yield is higher than that of the silica, and the yield may be about 80% or more by the heat treatment step according to the present invention.
  • Precursors capable of forming silicon oxycarbide (SiOC) having a C-Si-O network include polyphenyl siloxane, polymethylphenyl siloxane, polyvinylsiloxane, and polyvinylsiloxane.
  • Siloxane-based polymers such as polymethylphenyl hydroxysilane, polysilsesquioxane, polymethylsilsesquioxanes, polyphenylmethylsilsesquioxane, methylsilsesquioxane silsesquioxane family of polymers including methylsilsesquioxane, polyvinylsilsesquioxane, methylphenyl silsesquioxane, polyhedralorganosilsesquioxane and the like Silicone polymer such as silica sol by gel process and two or more kinds of horns It may be to contain water.
  • Synthetic starting material of the high carbon silica powder is a silicon-oxide compound corresponding to [Formula 1], and tetra-ethyl-ortho-silicate (TEOS) and phenyl-tri-methoxysilane (PTMS) corresponding to [Formula 2].
  • the reaction mixture was prepared by mixing as described in the following [Table 1]. 200 mL of ethanol was used as a solvent, and the reaction mixtures were each added and stirred. While maintaining the stirring state, the temperature was gradually raised to 50 ° C, and when the temperature was kept stable, 5% ammonia solution was added to make the pH 10. Ammonia was added to form a precipitate, which was reacted for at least 12 hours while maintaining stirring. The slurry after the reaction was washed with water, centrifuged and dried. The structure of the high carbon silica powder thus prepared is as shown in [Formula 1].
  • Tetra-ethyl-ortho-silicate was used as a starting material for the synthesis of silica sol, and novolac, a phenolic resin, was used as a carbon raw material.
  • 100 mL of TEOS was dissolved in 66 mL of ethanol, followed by the addition of 25 g of novolac having a carbon yield of 60%.
  • Oxalic acid was added to the TEOS-novolak mixed solution to bring the pH to 4-5.
  • Hexamethylenetetramine (HMTA) was added as a curing agent for novolac, and then reacted at 60 ° C. for 24 hours, and then cured at 80 ° C.
  • the structure of the silica sol-resin mixed powder thus prepared is shown in [Formula 2] below.
  • the high carbon silica powder synthesized in Preparation Example 1 was subjected to thermogravimetric analysis under a nitrogen atmosphere at room temperature from -1,000 ° C., at which time the temperature rising condition was 5 ° C./min.
  • Thermogravimetric analysis of the silica powder synthesized in Preparation Example 1 is shown in FIG. 1.
  • Thermogravimetric analysis showed that the high-carbon silica powder synthesized in Preparation Example 1 was pyrolyzed and the amount of inorganic matter remaining was about 80%.
  • the high carbon silica powder synthesized in Preparation Example 1 was pyrolyzed at 1,000 ° C. under a nitrogen atmosphere.
  • the pyrolyzed powder was subjected to elemental analysis to confirm that the weight content of silicon atoms in the remaining inorganic material was 69.4%.
  • silica 1 (silica powder) synthesized in Preparation Example 1 was heat-treated at 1,800 ° C. for 1 hour in an argon atmosphere to prepare silicon carbide powder. Formation of silicon carbide was measured using an X-ray diffraction analyzer and the results are shown in FIG. 2 (a), and the shape of the particles was confirmed by scanning electron microscope (FIG. 3 a).
  • silica 3 (silica powder) synthesized in Preparation Example 1 was heat-treated at 1,800 ° C. for 1 hour under an argon atmosphere to prepare silicon carbide powder. Formation of silicon carbide was measured using an X-ray diffraction analyzer and the results are shown in FIG. 2 (b), and the shape of the particles was confirmed by scanning electron microscope (FIG. 3 b).
  • beta phase silicon carbide was produced by heat-treating the silica powder having a molar ratio of PTMS of 50% in the reaction mixture.
  • the average particle size of the silicon carbide powder confirmed by the scanning electron microscope was 10 ⁇ m. It was confirmed that it was formed.
  • silica 2 (silica powder) synthesized in Preparation Example 1 was calcined at 1,000 ° C. for 4 hours under an argon atmosphere.
  • the calcined silica powder was heat-treated at 1,800 ° C. for 1 hour under argon atmosphere to prepare silicon carbide powder.
  • Formation of silicon carbide was measured using an X-ray diffraction analyzer and the results are shown in FIG. 4, and the shape of the particles was confirmed by scanning electron microscopy (FIG. 5).
  • silica 4 (silica powder) synthesized in Preparation Example 1 was heat-treated at 1,800 ° C. for 1 hour in an argon atmosphere to prepare silicon carbide powder. Formation of silicon carbide was measured using an X-ray diffraction analyzer and the results are shown in FIG. 8, and the shape of the particles was confirmed by scanning electron microscopy (FIG. 9).
  • silica 2 (silica powder) synthesized in Preparation Example 1 was heat-treated at 1,600 ° C. for 1 hour in an argon atmosphere to prepare silicon carbide powder. Formation of silicon carbide was measured using an X-ray diffraction analyzer and the results are shown in FIG. 10, and the shape of the particles was confirmed by scanning electron microscopy (FIG. 11).
  • Example 1 When comparing the results of Example 1 and Example 2 with Example 4, when the content of PTMS in the reaction mixture is less than 50 mol% silicon is formed with silicon carbide, it can be confirmed that the synthesis is inefficient there was.
  • Example 2 when comparing the results of Example 1 with Example 2, the condition that the content of PTMS content of 60 mol% in the reaction mixture is higher than the condition that the content of PTMS 50 mol%, the amount of carbon, the same temperature It was confirmed that the growth of the particles under the conditions can be stably formed fine powder silicon carbide.
  • silica 3 (silica powder) synthesized in Preparation Example 1 was maintained at 1,550 ° C. for 6 hours in an argon atmosphere, and then heated to 1,800 ° C. for 2 hours to prepare silicon carbide.
  • the manufactured silicon carbide was obtained 3.1 g, the formation of silicon carbide was confirmed by using an X-ray diffraction analyzer and the results are shown in Figure 12a below, the shape of the particles was confirmed by a scanning electron microscope (see Figure 13a below) ).
  • the prepared silicon carbide was subjected to purity analysis according to the Korean Industrial Standard (KS L1612) (Table 2).
  • the silicon carbide prepared in Example 5 showed a yield of 84.8%.
  • the particles confirmed by the scanning electron microscope were formed into particles having a size of about 23 ⁇ m.
  • the purity of the beta phase silicon carbide was confirmed to be 99.8%.
  • Example 5 by performing a two-step heat treatment as in Example 5 when compared with Example 2, it can be seen that the silicon carbide powder is more excellent in crystallinity and uniform particle size.
  • the silicon carbide prepared in Example 2 was found to be a yield of 67%, the purity was found to be 99.7%.
  • the silicon carbide produced by Comparative Example 2 was found to have a yield of 62%, and the purity was confirmed to be 99.7%. As a result of comparison with Example 5, it was confirmed that the yield of the silicon carbide powder obtained in Example 5 was about 22% higher than in Comparative Example 1.
  • the silicon carbide prepared by Comparative Example 3 was found to have a yield of 49%, and the purity was found to be 98.4%. In Example 6, the purity was higher and the yield was about 18% higher than that of Comparative Example 3. However, when compared to Example 5, the purity of silicon carbide was similar to that of Example 6 compared to the conditions of Example 6. At the same time, the yield of the powder was about 17% higher.
  • the production method according to the present invention by controlling the heat-treatment step to control the production rate of the SiO gas produced as the reaction intermediate to minimize the loss of SiO gas, it is possible to produce high purity beta-phase silicon carbide powder in high yield, It is possible to manufacture silicon carbide powder of high yield and high purity with excellent process efficiency without changing the process equipment by the existing thermal carbon reduction reaction.
  • the silicon carbide powder prepared according to the present invention has good reactivity, uniform particle size, and has an excellent beta phase crystal phase, which may be molded into a silicon carbide single crystal and a silicon carbide substrate and used in various fields.

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Abstract

La présente invention concerne un procédé de production de poudre de carbure de silicium. De la poudre de carbure de silicium cristalline et exceptionnellement réactive peut être produite et un procédé de traitement thermique est divisé en deux étapes de manière à améliorer encore la cristallinité du carbure de silicium produit. Il est également possible de produire une poudre de carbure de silicium cristalline de phase bêta avec un rendement et une pureté élevés.
PCT/KR2012/005671 2011-10-14 2012-07-16 Procédé de production pour poudre de carbure de silicium et poudre de carbure de silicium ainsi produite WO2013055016A1 (fr)

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KR1020110105550A KR101356971B1 (ko) 2011-10-14 2011-10-14 탄화규소 분말의 제조방법，이의 탄화규소 분말，이의 성형물 및 이의 탄화규소 단결정
KR10-2011-0105550 2011-10-14
KR1020120028369A KR101322796B1 (ko) 2012-03-20 2012-03-20 열탄소환원법에 의한 수율이 향상된 탄화규소 분말의 제조방법 및 이에 의해서 제조된 탄화규소 분말
KR10-2012-0028369 2012-03-20

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CN103834988A (zh) * 2014-03-24 2014-06-04 中国科学院山西煤炭化学研究所 一种制备纳米碳化硅晶须的方法
KR101538021B1 (ko) * 2013-06-03 2015-07-22 한국세라믹기술원 직접탄화법을 이용한 고순도 탄화규소 분말의 합성방법 및 이에 의하여 제조된 고순도 탄화규소 분말
US20160207782A1 (en) * 2013-05-02 2016-07-21 Melior Innovations, Inc. Polysilocarb based silicon carbide materials, applications and devices
CN115087620A (zh) * 2020-01-31 2022-09-20 弗劳恩霍夫应用研究促进协会 用于从碳化硅中分离杂质的方法以及经温度处理和净化处理的碳化硅粉末
US12030819B2 (en) 2013-05-02 2024-07-09 Pallidus, Inc. Doped SiC and SiOC compositions and Methods

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
US20160207782A1 (en) * 2013-05-02 2016-07-21 Melior Innovations, Inc. Polysilocarb based silicon carbide materials, applications and devices
US11091370B2 (en) 2013-05-02 2021-08-17 Pallidus, Inc. Polysilocarb based silicon carbide materials, applications and devices
US12030819B2 (en) 2013-05-02 2024-07-09 Pallidus, Inc. Doped SiC and SiOC compositions and Methods
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CN115087620B (zh) * 2020-01-31 2024-05-07 弗劳恩霍夫应用研究促进协会 用于从碳化硅中分离杂质的方法以及经温度处理和净化处理的碳化硅粉末

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