KR102649189B1 - Method for manufacturing of porous sic molded body for single crystal growth - Google Patents
Method for manufacturing of porous sic molded body for single crystal growth Download PDFInfo
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- KR102649189B1 KR102649189B1 KR1020200179375A KR20200179375A KR102649189B1 KR 102649189 B1 KR102649189 B1 KR 102649189B1 KR 1020200179375 A KR1020200179375 A KR 1020200179375A KR 20200179375 A KR20200179375 A KR 20200179375A KR 102649189 B1 KR102649189 B1 KR 102649189B1
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 22
- 239000013078 crystal Substances 0.000 title description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 61
- 239000000843 powder Substances 0.000 claims abstract description 57
- 238000002156 mixing Methods 0.000 claims abstract description 49
- 239000008187 granular material Substances 0.000 claims abstract description 45
- 229920000642 polymer Polymers 0.000 claims abstract description 45
- 239000000126 substance Substances 0.000 claims abstract description 41
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 239000000701 coagulant Substances 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 17
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 8
- -1 polypropylene Polymers 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 230000015271 coagulation Effects 0.000 description 7
- 238000005345 coagulation Methods 0.000 description 7
- 239000012670 alkaline solution Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000002706 hydrostatic effect Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012154 double-distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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Abstract
본 발명은 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계; 상기 혼합용액에 알칼리 물질을 혼합하는 단계; 상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계; 상기 슬러리를 성형하여 성형체를 제조하는 단계; 및 상기 성형체를 하소시키는 단계;를 포함하는, SiC 성형체 제조방법에 관한 것이다.The present invention includes the steps of mixing and dispersing a dispersant, SiC powder, and polymer granules in a solvent to prepare a mixed solution; Mixing an alkaline substance into the mixed solution; Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances; Manufacturing the slurry into a molded body; and calcining the molded body. It relates to a method of manufacturing a SiC molded body, including.
Description
본 발명은 SiC 단결정 성장시 원료로 사용되는 SiC 성형체 제조방법에 관한 것이다. 구체적으로 본 발명은 다공성 SiC 성형체에 관한 것이다.The present invention relates to a method of manufacturing a SiC molded body used as a raw material when growing a SiC single crystal. Specifically, the present invention relates to porous SiC molded bodies.
기존 SiC 단결정 성장 방법은 원료물질인 SiC 분말 일정량을 칭량하여 탄소도가니 내부에 장입 후 상부의 Seed의 위치로부터 일정한 거리를 맞추어 주기 위하여 도가니 내 원료 분말의 높이를 기계적인 방법으로 눌러 주어 맞추는 방법을 사용하고 있다.The existing SiC single crystal growth method uses a method of weighing a certain amount of SiC powder as a raw material, charging it into a carbon crucible, and then mechanically pressing and adjusting the height of the raw material powder in the crucible to set a certain distance from the position of the seed at the top. I'm doing it.
그러나 원료 분말이 대부분 미분말이므로 기존의 누르는 방법은 원료 장입 시 그리고 기계적 압력을 가해줄 때 미분이 휘산되어 도가니 내벽에 들러 붙을 수 있다. 또한 기계적 압력장치와 탄소도가니 내벽의 마찰에 의해 발생하는 미세한 탄소 가루에 의한 원료분말의 오염이 발생하기도 한다. 또한 들러 붙은 미분을 도가니 내벽으로부터 제거하기 위하여 진공흡입기를 이용해야 하는 등, 기존 방법은 공정상의 어려움이 있었다.However, since the raw material powder is mostly fine powder, the existing pressing method may cause the fine powder to volatilize and stick to the inner wall of the crucible when charging the raw material and applying mechanical pressure. In addition, contamination of the raw material powder may occur due to fine carbon powder generated by friction between the mechanical pressure device and the inner wall of the carbon crucible. In addition, the existing method had process difficulties, such as having to use a vacuum suction device to remove stuck fine powder from the inner wall of the crucible.
따라서, SiC 원료 분말의 탄소도가니 내 장입 시 원료 분말의 오염을 피하면서도 용이하게 원료를 장입하는 방법이 필요하다.Therefore, when charging SiC raw material powder into a carbon crucible, a method is needed to easily charge the raw material while avoiding contamination of the raw material powder.
이에, 단순한 SiC 성형체를 제조하는 방법으로 스틸몰드를 이용한 프레스 법이나 정수압성형을 이용한 방법이 제안되었다. 그러나 스틸몰드를 이용한 프레스법은 프레스 공정시 스틸몰드의 마찰에 의해 성형체 외부에 오염이 발생하게 되며, 정수압성형법의 경우 정확한 형상 제어가 힘들어 추가로 정확한 형상 가공을 필요로 하기 때문에 원료 분말의 손실이 많다는 단점이 있다. Accordingly, a method using a press method using a steel mold or a method using hydrostatic pressure forming has been proposed as a method of manufacturing a simple SiC molded body. However, in the pressing method using a steel mold, contamination occurs on the outside of the molded body due to friction of the steel mold during the pressing process, and in the case of the hydrostatic forming method, accurate shape control is difficult and additional accurate shape processing is required, resulting in loss of raw material powder. There are many disadvantages.
또한 기존 성형방법으로 제조된 SiC 성형체는 성형체 내에 기공이 거의 형성되어 있지 않은바, SiC 단결정 성장공정 진행 중의 SiC 원료 분말 내부에서 발생하는 기상 화합물종(Si, Si2C, SiC2 등)이 원료 분말 내에서 나와 단결정 성장부로 원활하게 이동하지 못하는 단점이 있다. In addition, the SiC molded body manufactured by the existing molding method has almost no pores formed in the molded body, and the gaseous compound species (Si, Si 2 C, SiC 2 , etc.) generated inside the SiC raw material powder during the SiC single crystal growth process are the raw material. It has the disadvantage of not being able to come out of the powder and move smoothly to the single crystal growth area.
이에, 상기 단점들을 보완하는 SiC 성형체 제조방법 제공에 대한 필요성이 있다.Accordingly, there is a need to provide a SiC molded body manufacturing method that complements the above shortcomings.
본 발명은 SiC 단결정 성장시 사용하는 탄소 도가니 내에 원료 물질인 SiC를 분말형으로 장입하는 경우 발생하는 문제를 해결하기 위하여, SiC 성형체를 제조하는 방법을 제공하고자 한다.The present invention seeks to provide a method of manufacturing a SiC molded body in order to solve problems that occur when charging SiC, a raw material, in powder form into a carbon crucible used when growing a SiC single crystal.
보다 구체적으로 본 발명은 미분의 SiC 분말을 탄소도가니 내에 분말형태로 투입하지 않고, 단결정 성장용 도가니 내부의 모양에 맞는 일정한 형태의 SiC 분말 성형체로 만드는 방법을 제공하고자 한다.More specifically, the present invention seeks to provide a method of making a SiC powder molded body of a certain shape that fits the shape of the inside of a crucible for single crystal growth, without putting fine SiC powder in powder form into a carbon crucible.
본 발명 일 구현예에 따른 SiC 성형체 제조방법은 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계; 상기 혼합용액에 알칼리 물질을 혼합하는 단계; 상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계; 상기 슬러리를 성형하여 성형체를 제조하는 단계; 및 상기 성형체를 하소시키는 단계;를 포함한다.A method for manufacturing a SiC molded body according to an embodiment of the present invention includes the steps of mixing and dispersing a dispersant, SiC powder, and polymer granules in a solvent to prepare a mixed solution; mixing an alkaline substance into the mixed solution; Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances; Manufacturing the slurry into a molded body; and calcining the molded body.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서, SiC 분말은 직경이 10㎛ 이하이다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, the SiC powder has a diameter of 10㎛ or less.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 고분자 과립은 직경이 SiC 분말 직경의 1배 내지 10배이다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, the polymer granules have a diameter 1 to 10 times the diameter of the SiC powder.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 고분자 과립은 폴리프로필렌(Polypropylene), 폴리에틸렌(Polyethylene) 또는 이들의 혼합물이다.In the step of preparing a mixed solution by mixing and dispersing a dispersant, SiC powder, and polymer granules in a solvent, the polymer granules are polypropylene, polyethylene, or a mixture thereof.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 고분자 과립은 SiC 분말 총 중량 대비 5 내지 50중량% 포함된다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, the polymer granules are included in an amount of 5 to 50% by weight based on the total weight of the SiC powder.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서 알칼리 물질은 암모니아, NaOH, 및 TMAH (Tetramethylammonium hydroxide)로 이루어진 군 중에서 선택된 1종 이상이다.In the step of mixing an alkaline substance into the mixed solution, the alkaline substance is at least one selected from the group consisting of ammonia, NaOH, and TMAH (Tetramethylammonium hydroxide).
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서 알칼리 물질이 혼합된 혼합용액의 pH는 10 이상이다.In the step of mixing an alkaline substance into the mixed solution, the pH of the mixed solution containing the alkaline substance is 10 or more.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서 알칼리 물질은 혼합용액 전체 중량에 대하여 2 중량% 이하로 첨가된다.In the step of mixing an alkaline substance with the mixed solution, the alkaline substance is added in an amount of 2% by weight or less based on the total weight of the mixed solution.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;는 혼합용액에 알칼리 물질을 혼합한 후 용액을 에이징 하고 탈포하는 단계를 더 포함한다.The step of mixing an alkaline substance into the mixed solution further includes mixing the alkaline substance into the mixed solution and then aging and degassing the solution.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서 응고제는 염산, 불산 및 포름산메틸(Methyl formate)로 이루어진 군 중에서 선택된 1종 이상이다.In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the coagulant is at least one selected from the group consisting of hydrochloric acid, hydrofluoric acid, and methyl formate.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서 응고제는 알칼리 물질에 대하여 당량비로 1.2 내지 1.4 당량으로 첨가된다.In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the coagulant is added in an equivalent ratio of 1.2 to 1.4 based on the alkaline substance.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서 응고제가 투입된 슬러리는 pH가 6 내지 9이다.In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the slurry to which the coagulant is added has a pH of 6 to 9.
상기 슬러리를 성형하여 성형체를 제조하는 단계;는 성형체를 상온에서 건조하는 단계; 및 상온 건조된 성형체를 건조 오븐에서 추가 건조하는 단계; 를 더 포함한다.Manufacturing the molded body by molding the slurry; drying the molded body at room temperature; and additionally drying the molded body dried at room temperature in a drying oven; It further includes.
상기 성형체를 하소시키는 단계;는 온도 700℃ 이상에서 5시간 이상 성형체를 하소시키는 단계이다.The step of calcining the molded body is a step of calcining the molded body at a temperature of 700° C. or higher for 5 hours or more.
상기 성형체를 하소시키는 단계;는 고분자 과립을 산화시켜 다공질 조직을 형성하는 단계이다.The step of calcining the molded body is a step of forming a porous structure by oxidizing the polymer granules.
본 발명 일 구현예에 따른 SiC 성형체 제조방법에 따르면, SiC 성형체를 기계적인 프레스 공정없이 원하는 형상으로 제조할 수 있다.According to the SiC molded body manufacturing method according to one embodiment of the present invention, the SiC molded body can be manufactured into a desired shape without a mechanical press process.
또한, 본 발명 일 구현예에 따른 방법으로 제조된 SiC 성형체는 주변을 오염시키지 않고 용이하게 SiC 단결정 성장용 탄소 도가니 내에 장입될 수 있다.In addition, the SiC molded body manufactured by the method according to one embodiment of the present invention can be easily inserted into a carbon crucible for SiC single crystal growth without contaminating the surrounding area.
또한, 본 발명 일 구현예에 따른 방법으로 제조된 SiC 성형체는 다공성인바, 원료 물질인 SiC 성형체 내부에서 발생하는 기상 화합물종(Si, Si2C, SiC2 등)이 빠져나와 단결정 성장부로 이동하는 것이 용이하다.In addition, the SiC molded body manufactured by the method according to one embodiment of the present invention is porous, so gaseous compound species (Si, Si 2 C, SiC 2, etc.) generated inside the SiC molded body, which is a raw material, escape and move to the single crystal growth zone. It is easy.
제1, 제2 및 제3 등의 용어들은 다양한 부분, 성분, 영역, 층 및/또는 섹션들을 설명하기 위해 사용되나 이들에 한정되지 않는다. 이들 용어들은 어느 부분, 성분, 영역, 층 또는 섹션을 다른 부분, 성분, 영역, 층 또는 섹션과 구별하기 위해서만 사용된다. 따라서, 이하에서 서술하는 제1 부분, 성분, 영역, 층 또는 섹션은 본 발명의 범위를 벗어나지 않는 범위 내에서 제2 부분, 성분, 영역, 층 또는 섹션으로 언급될 수 있다.Terms such as first, second, and third are used to describe, but are not limited to, various parts, components, regions, layers, and/or sections. These terms are used only to distinguish one part, component, region, layer or section from another part, component, region, layer or section. Accordingly, the first part, component, region, layer or section described below may be referred to as the second part, component, region, layer or section without departing from the scope of the present invention.
여기서 사용되는 전문 용어는 단지 특정 실시예를 언급하기 위한 것이며, 본 발명을 한정하는 것을 의도하지 않는다. 여기서 사용되는 단수 형태들은 문구들이 이와 명백히 반대의 의미를 나타내지 않는 한 복수 형태들도 포함한다. 명세서에서 사용되는 "포함하는"의 의미는 특정 특성, 영역, 정수, 단계, 동작, 요소 및/또는 성분을 구체화하며, 다른 특성, 영역, 정수, 단계, 동작, 요소 및/또는 성분의 존재나 부가를 제외시키는 것은 아니다.The terminology used herein is only intended to refer to specific embodiments and is not intended to limit the invention. As used herein, singular forms include plural forms unless phrases clearly indicate the contrary. As used in the specification, the meaning of "comprising" refers to specifying a particular characteristic, area, integer, step, operation, element and/or ingredient, and the presence or presence of another characteristic, area, integer, step, operation, element and/or ingredient. This does not exclude addition.
어느 부분이 다른 부분의 "위에" 또는 "상에" 있다고 언급하는 경우, 이는 바로 다른 부분의 위에 또는 상에 있을 수 있거나 그 사이에 다른 부분이 수반될 수 있다. 대조적으로 어느 부분이 다른 부분의 "바로 위에" 있다고 언급하는 경우, 그 사이에 다른 부분이 개재되지 않는다.When a part is referred to as being “on” or “on” another part, it may be directly on or on the other part or may be accompanied by another part in between. In contrast, when a part is said to be "directly on top" of another part, there is no intervening part between them.
또한, 특별히 언급하지 않는 한 %는 중량%를 의미하며, 1ppm 은 0.0001중량%이다.Additionally, unless specifically stated, % means weight%, and 1ppm is 0.0001% by weight.
다르게 정의하지는 않았지만, 여기에 사용되는 기술용어 및 과학용어를 포함하는 모든 용어들은 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 일반적으로 이해하는 의미와 동일한 의미를 가진다. 보통 사용되는 사전에 정의된 용어들은 관련기술문헌과 현재 개시된 내용에 부합하는 의미를 가지는 것으로 추가 해석되고, 정의되지 않는 한 이상적이거나 매우 공식적인 의미로 해석되지 않는다.Although not defined differently, all terms including technical and scientific terms used herein have the same meaning as those generally understood by those skilled in the art in the technical field to which the present invention pertains. Terms defined in commonly used dictionaries are further interpreted as having meanings consistent with related technical literature and currently disclosed content, and are not interpreted in ideal or very formal meanings unless defined.
이하, 본 발명의 실시예에 대하여 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 상세히 설명한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며 여기에서 설명하는 실시예에 한정되지 않는다.Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily implement the present invention. However, the present invention may be implemented in many different forms and is not limited to the embodiments described herein.
본 발명은 단결정 성장용 SiC 분말 성형체를 제조하기 위하여, 일정량의 SiC 분말을 적당량의 물에 분산하고, 분산제를 투입한 후 중화제를 첨가하여 경화시키는 솔-젤 (Sol-gel) 방법을 이용한다. 이때 성형체 내부에 기공을 형성하기 위하여 원료 물질 중에 고분자를 혼합하고, 이것을 산화시켜 기공을 형성시키는 하소 단계를 더 포함한다.In order to produce a SiC powder molded body for single crystal growth, the present invention uses a sol-gel method in which a certain amount of SiC powder is dispersed in an appropriate amount of water, a dispersant is added, and a neutralizing agent is added to cure the SiC powder. At this time, in order to form pores inside the molded body, a calcination step of mixing polymers among the raw materials and oxidizing them to form pores is further included.
이하, 각 단계에 대하여 구체적으로 살펴본다.Below, we will look at each step in detail.
본 발명 일 구현예에 따른 SiC 성형체 제조방법은 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계; 상기 혼합용액에 알칼리 물질을 혼합하는 단계; 상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계; 상기 슬러리를 성형하여 성형체를 제조하는 단계; 및 상기 성형체를 하소시키는 단계;를 포함한다.A method for manufacturing a SiC molded body according to an embodiment of the present invention includes the steps of mixing and dispersing a dispersant, SiC powder, and polymer granules in a solvent to prepare a mixed solution; Mixing an alkaline substance into the mixed solution; Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances; Manufacturing the slurry into a molded body; and calcining the molded body.
상기 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 용매는 증류수 일 수 있고, 구체적으로는 2차 증류수일 수 있다. 상기 증류수는 가급적이면 2차 이상의 증류수를 사용하는 것이 바람직하다. SiC 성형체 제작의 최종 목적은 단결정 성장용 원료로 사용하기 위한 것이므로, 순도를 중요시하는 단결정 성장용 원료로서 원치 않는 불순물의 혼입 가능성을 최소화하기 위함이다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in the solvent, the solvent may be distilled water, and specifically, may be double distilled water. It is desirable to use secondary or higher distilled water if possible. The final purpose of producing a SiC molded body is to use it as a raw material for single crystal growth, and as a raw material for single crystal growth where purity is important, the purpose is to minimize the possibility of unwanted impurities being mixed in.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 SiC 분말은 직경이 10㎛ 이하이다. 구체적으로 SiC 분말 직경은 1㎛ 내지 10㎛, 보다 구체적으로 5㎛ 내지 10㎛이다. SiC 분말의 입도가 너무 크면 침전이 일어나 균일한 분산을 하기가 어렵고, 입도가 너무 작으면 분산은 잘 되지만, 덩치가 커져서 최종 성형체의 충전밀도가 양호하지 않게 되어 많은 양을 넣을 수 없다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, the SiC powder has a diameter of 10㎛ or less. Specifically, the SiC powder diameter is 1㎛ to 10㎛, more specifically 5㎛ to 10㎛. If the particle size of SiC powder is too large, precipitation occurs, making it difficult to disperse uniformly. If the particle size is too small, dispersion is good, but the size becomes large, so the packing density of the final molded body is not good, so a large amount cannot be added.
또한, 본 발명에서 원료 물질로서 사용되는 SiC는 고순도 SiC 분말, 구체적으로 순도 약 99% 이상인 고순도 SiC 분말을 사용한다.In addition, SiC used as a raw material in the present invention is high-purity SiC powder, specifically, high-purity SiC powder with a purity of about 99% or more.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 고분자 과립(bead)은 직경이 SiC 분말 직경의 1배 내지 10배일 수 있다. 구체적으로 고분자 과립은 직경이 SiC 분말 직경의 3 내지 5배일 수 있다. 즉, SiC 분말 직경이 10㎛이면 고분자 과립의 직경은 10㎛ 내지 100㎛, 구체적으로는 30㎛ 내지 50㎛일 수 있다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, the diameter of the polymer granules (beads) may be 1 to 10 times the diameter of the SiC powder. Specifically, the polymer granules may have a diameter 3 to 5 times the diameter of the SiC powder. That is, if the SiC powder diameter is 10㎛, the polymer granule diameter may be 10㎛ to 100㎛, specifically 30㎛ to 50㎛.
상기 고분자 과립은 하소 단계에서 산화 및 기화 되어 기공을 형성할 수 있는 것이면 제한이 없으나, 예를 들어 폴리프로필렌(Polypropylene), 폴리에틸렌(Polyethylene) 또는 이들의 혼합물일 수 있다.The polymer granules are not limited as long as they can be oxidized and vaporized in the calcination step to form pores, but may be, for example, polypropylene, polyethylene, or a mixture thereof.
상기 고분자 과립은 SiC 분말 총 중량 대비 5 내지 50중량% 포함될 수 있다. 구체적으로 고분자 과립은 SiC 분말 총 중량 대비 10 내지 30중량% 또는 20 내지 30중량% 포함될 수 있다.The polymer granules may be included in an amount of 5 to 50% by weight based on the total weight of SiC powder. Specifically, the polymer granules may be included in an amount of 10 to 30% by weight or 20 to 30% by weight based on the total weight of the SiC powder.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서, 상기 분산제로서는 수용성 폴리머 제품을 사용할 수 있다. 분산제는 용액내에서 SiC 분말 및 고분자 과립의 분산을 도와주는 역할을 한다. 예로서, 아크릴, 비닐, 또는 알릴 단량체와 아크릴산의 수용성 공중합체를 들 수 있다. 상기 분산제는 증류수 100 중량부당 0.1 내지 0.5 중량부로 포함될 수 있다. 상기 분산제가 너무 많거나 적으면 효과적인 분산제의 역할을 하지 못할 수 있다.In the step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent, a water-soluble polymer product can be used as the dispersant. The dispersant serves to help disperse SiC powder and polymer granules in the solution. Examples include water-soluble copolymers of acrylic acid with acrylic, vinyl, or allyl monomers. The dispersant may be included in an amount of 0.1 to 0.5 parts by weight per 100 parts by weight of distilled water. If the dispersant is too much or too little, it may not function as an effective dispersant.
상기 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;는 교반기를 이용하여 고르게 분산시키는 단계이다.The step of preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in the solvent is a step of dispersing evenly using a stirrer.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서, 상기 알칼리 물질은 암모니아, NaOH, 및 TMAH (Tetramethylammonium hydroxide)로 이루어진 군 중에서 선택된 1종 이상으로, 강알칼리성 용액일 수 있다. In the step of mixing an alkaline substance into the mixed solution, the alkaline substance is one or more selected from the group consisting of ammonia, NaOH, and TMAH (Tetramethylammonium hydroxide), and may be a strongly alkaline solution.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서, 알칼리 물질이 혼합된 혼합용액의 pH는 10 이상일 수 있다. 구체적으로 혼합용액의 pH는 11 이상일 수 있다.In the step of mixing an alkaline substance into the mixed solution, the pH of the mixed solution containing the alkaline substance may be 10 or more. Specifically, the pH of the mixed solution may be 11 or higher.
상기 알칼리 물질로 강알칼리성 용액을 사용하는 이유는 SiC 분말의 표면을 덮는 미량의 SiO2 표면층의 전하특성을 이용하기 위함이다. 강알칼리성 용액의 양은 SiC 슬러리의 pH가 10이상이 되도록 하는 양이다.The reason for using a strong alkaline solution as the alkaline material is to utilize the charge characteristics of a trace amount of SiO 2 surface layer covering the surface of SiC powder. The amount of strongly alkaline solution is such that the pH of the SiC slurry is 10 or more.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서, 알칼리 물질은 혼합용액 전체 중량에 대하여 2 중량% 이하로 첨가될 수 있다. 구체적으로 강알칼리성 용액은 혼합용액 전체 중량에 대하여 0.1 내지 2 중량%, 보다 구체적으로 0.1 내지 1.5중량%로 첨가될 수 있다. 알칼리성 용액의 양이 적으면 원하는 pH에 도달하지 못하고 너무 많으면 비경제적이다.In the step of mixing an alkaline substance with the mixed solution, the alkaline substance may be added in an amount of 2% by weight or less based on the total weight of the mixed solution. Specifically, the strong alkaline solution may be added in an amount of 0.1 to 2% by weight, more specifically 0.1 to 1.5% by weight, based on the total weight of the mixed solution. If the amount of alkaline solution is small, the desired pH cannot be reached, and if it is too much, it is uneconomical.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;는, 혼합용액에 알칼리 물질을 혼합한 후 용액을 에이징 하고 탈포하는 단계를 더 포함할 수 있다. 상기 에이징 시간은 24시간 이상일 수 있다.The step of mixing an alkaline substance into the mixed solution may further include mixing the alkaline substance into the mixed solution and then aging and defoaming the solution. The aging time may be 24 hours or more.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서, 응고제는 pH 강하제이면 제한이 없고, 예컨대 염산(HCl), 불산(HF) 및 포름산메틸(Methyl formate)로 이루어진 군 중에서 선택된 1종 이상일 수 있다. In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the coagulant is not limited as long as it is a pH lowering agent, for example, a group consisting of hydrochloric acid (HCl), hydrofluoric acid (HF), and methyl formate. There may be one or more types selected from among.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서, 응고제는 알칼리 물질에 대하여 당량비로 1.2 내지 1.4 당량으로 첨가될 수 있다. pH 강하 효과를 나타내는 응고제의 함량이 너무 적으면 pH가 낮아지지 않아 응고가 일어나지 않을 수 있고, 응고제의 함량이 너무 많으면 응고가 급속하게 일어나 성형공정 제어가 곤란한 문제가 있을 수 있다. In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the coagulant may be added in an equivalent ratio of 1.2 to 1.4 based on the alkaline substance. If the content of the coagulant, which has a pH-lowering effect, is too small, the pH may not be lowered and coagulation may not occur. If the content of the coagulant is too high, coagulation may occur rapidly, making it difficult to control the molding process.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서 응고제가 투입된 슬러리는 pH가 6 내지 9일 수 있다. 즉 슬러리가 pH 6 내지 9 범위에서 SiC 응고가 이루어진다. 슬러리의 pH가 6 내지 9 범위에서 응고가 시작되는바, 아직 유동성이 있는 상태에서 슬러리를 원하는 형상의 몰드내에 부어 응고 시켜 성형체를 제조한다. In the step of preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances, the slurry to which the coagulant is added may have a pH of 6 to 9. That is, SiC solidification occurs in the slurry pH range of 6 to 9. Solidification begins when the pH of the slurry is in the range of 6 to 9, and the slurry is poured into a mold of the desired shape while still fluid and solidified to produce a molded body.
상기 슬러리를 성형하여 성형체를 제조하는 단계;는 슬러리를 몰드에 넣고 응고 시켜 몰드 형상의 성형체를 수득하는 단계일 수 있다. 응고 반응이 완결되기까지의 시간은 고형분의 양과 응고 촉진제 양에 영향을 받지만, 통상적으로 응고 시간은 5 내지 10분일 수 있다. The step of manufacturing a molded body by molding the slurry may be a step of putting the slurry into a mold and solidifying it to obtain a molded body. The time until the coagulation reaction is completed is affected by the amount of solids and the amount of coagulation accelerator, but typically the coagulation time can be 5 to 10 minutes.
상기 슬러리를 성형하여 성형체를 제조하는 단계;는 성형체를 상온에서 건조하는 단계; 및 상온 건조된 성형체를 건조 오븐에서 추가 건조하는 단계;를 더 포함할 수 있다. 상기 상온에서 건조시키는 단계는 24시간 이상 진행될 수 있고, 건조 오븐에서 추가 건조 하는 단계는 온도가 100 내지 150℃일 수 있다. Manufacturing the molded body by molding the slurry; drying the molded body at room temperature; and additionally drying the molded body dried at room temperature in a drying oven. The drying step at room temperature may be performed for more than 24 hours, and the additional drying step in a drying oven may have a temperature of 100 to 150°C.
응고된 SiC 슬러리는 겔 상태로 몰드로부터 수득된다. 이것을 상온에서 건조시키고, 다시 건조오븐에서 건조시키는 단계를 거친다.The solidified SiC slurry is obtained from the mold in a gel state. This is dried at room temperature and then dried again in a drying oven.
상기 성형체를 하소시키는 단계;는 온도 700℃ 이상에서 5시간 이상 성형체를 하소시키는 단계일 수 있다. 구체적으로 하소 온도는 700 내지 1000℃이고, 하소 시간은 5시간 내지 7시간일 수 있다. 구체적으로 상기 성형체를 하소시키는 단계;는 고분자 과립을 산화시켜 다공질 조직을 형성하는 단계일 수 있다. 성형체 내에 존재하던 고분자 과립은 하소 단계에서 산화되어 그 차지하고 있던 부피 만큼 기공을 형성할 수 있다.The step of calcining the molded body may be a step of calcining the molded body at a temperature of 700° C. or higher for 5 hours or more. Specifically, the calcination temperature may be 700 to 1000° C., and the calcination time may be 5 to 7 hours. Specifically, the step of calcining the molded body may be a step of oxidizing the polymer granules to form a porous structure. The polymer granules present in the molded body may be oxidized during the calcination step, forming pores corresponding to the volume they occupied.
이하 본 발명의 실시예에 대하여 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 용이하게 실시할 수 있도록 상세히 설명한다. 그러나 본 발명은 여러가지 상이한 형태로 구현될 수 있으며, 여기에서 설명하는 실시예에 한정되지 않는다.Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily implement the present invention. However, the present invention may be implemented in various different forms and is not limited to the embodiments described herein.
실시예Example
SiC 분말로는 상용의 모든 분말의 채용이 가능하지만 가급적 순도 99% 이상의 고순도 제품을 사용하였다. 이때 분말의 입도는 용이한 분산성을 유도하기 위하여 평균 직경이 10㎛인 미분을 사용하였다. Any commercially available SiC powder can be used, but high-purity products with a purity of 99% or higher were used whenever possible. At this time, fine powder with an average diameter of 10㎛ was used to induce easy dispersibility.
고분자 과립은 상용 고분자로서 폴리프로필렌 과립 및 폴리에틸렌 과립을 사용하였다. 고분자 과립 크기는 SiC 분말 직경의 3배 내지 5배 인 것을 선별하여 사용하였다.Polypropylene granules and polyethylene granules were used as polymer granules as commercial polymers. Polymer granules with a size of 3 to 5 times the diameter of the SiC powder were selected and used.
이들 SiC 미분말 1500g 및 고분자 과립 300g을 2차 증류수 1000g에 혼합하여 주고, 이때 균질한 분산을 돕기 위하여 상용의 분산제를 증류수 전체 중량에 대하여 0.3중량%로 첨가하여 주고 일정시간 교반하여 주었다.1500g of these SiC fine powders and 300g of polymer granules were mixed with 1000g of secondary distilled water. At this time, to help homogeneous dispersion, a commercial dispersant was added at 0.3% by weight based on the total weight of distilled water and stirred for a certain period of time.
교반을 통하여 균질하게 혼합된 이 SiC-고분자 과립 혼합용액에 강알칼리인 TMAH(Tetramethylammonium hydroxide)를 혼합용액 전체 중량에 대하여 1.4중량%로 첨가해주고 1시간 이상 교반하여 주었다. TMAH를 첨가하고 충분히 교반한 혼합용액의 pH는 11이상으로 증가하였다.Tetramethylammonium hydroxide (TMAH), a strong alkali, was added at 1.4% by weight based on the total weight of the mixed solution to this SiC-polymer granule mixed solution that was homogeneously mixed through stirring and stirred for more than 1 hour. The pH of the mixed solution after adding TMAH and stirring sufficiently increased to over 11.
강알칼리 용액이 혼합된 혼합용액을 상온에서 느린 속도로 교반하며 24시간 정도 에이징해준 후 기포를 제거하기 위하여 진공용기 내에서 탈포 작업을 수행하였다. The mixed solution containing the strong alkaline solution was stirred at a slow speed at room temperature and aged for about 24 hours, and then degassed in a vacuum container to remove air bubbles.
탈포된 SiC-고분자 과립 혼합용액에 TMAH에 대한 당량비로 1.2 내지 1.4당량으로 응고제를 천천히 교반해 주면서 첨가하여 슬러리를 제조하였다. 이때 사용한 응고제는 pH강하제인 포름산메틸(Methyl formate)을 사용하였다. A slurry was prepared by slowly stirring and adding a coagulant in an equivalent ratio of 1.2 to 1.4 equivalents to TMAH to the deaerated SiC-polymer granule mixed solution. The coagulant used at this time was methyl formate, a pH lowering agent.
충분히 교반된 슬러리를 원통형의 정밀 몰드 내에 부어준다. 몰드 주입 후 수분의 증발을 막기 위하여 몰드를 밀봉하였다. 시간이 경과 함에 따라 몰드 내에 주입된 슬러리의 pH는 급격히 떨어지기 시작하여 pH 7.5와 9.5사이에 도달하게 되며 급격히 응고되기 시작하였다. 응고반응이 완결되기까지의 시간은 고체의 양과 응고촉진제의 양에 영향을 받지만 통상 5분에서 10분내에 이루어지는 것이 좋다. Pour the sufficiently stirred slurry into a cylindrical precision mold. After mold injection, the mold was sealed to prevent moisture from evaporating. As time passed, the pH of the slurry injected into the mold began to drop rapidly, reaching a pH between 7.5 and 9.5, and began to rapidly solidify. The time until the coagulation reaction is completed is affected by the amount of solid and the amount of coagulation accelerator, but it is generally recommended to take place within 5 to 10 minutes.
일정시간이 지난 후 응고된 겔상태의 SiC-고분자 과립 성형체를 몰드로부터 제거한 후 24시간 이상 상온에서 건조한 후 다시 110℃의 건조오븐에 넣어 건조해주어 원통형의 모양을 가지는 고강도 SiC0고분자 과립 성형체를 수득하였다.After a certain period of time, the solidified gel-like SiC-polymer granule molded body was removed from the mold, dried at room temperature for more than 24 hours, and then placed in a drying oven at 110°C to dry, thereby obtaining a high-strength SiC0 polymer granule molded body having a cylindrical shape. .
수득된 SiC-고분자 과립 성형체를 공기중에서 700℃ 이상의 온도로 5시간 이상 하소시켰다. 하소 단계에서 성형체 내의 고분자 과립은 산화되며 제거되었고, 고분자 과립이 차지하고 있던 체적만큼 SiC 성형체 내부에 기공이 형성되어 다공성 SiC 성형체를 수득하였다. The obtained SiC-polymer granule molded body was calcined in air at a temperature of 700° C. or higher for more than 5 hours. In the calcination step, the polymer granules in the molded body were oxidized and removed, and pores were formed inside the SiC molded body equal to the volume occupied by the polymer granules, thereby obtaining a porous SiC molded body.
본 발명은 실시예들에 한정되는 것이 아니라 서로 다른 다양한 형태로 제조될 수 있으며, 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자는 본 발명의 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 실시될 수 있다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다.The present invention is not limited to the embodiments, but can be manufactured in various different forms, and a person skilled in the art will understand that the present invention can be manufactured in other specific forms without changing the technical idea or essential features of the present invention. You will understand that it can be done. Therefore, the embodiments described above should be understood in all respects as illustrative and not restrictive.
Claims (15)
상기 혼합용액에 알칼리 물질을 혼합하는 단계;
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;
상기 슬러리를 성형하여 성형체를 제조하는 단계; 및
상기 성형체를 하소시키는 단계;를 포함하고,
상기 용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서 고분자 과립은 폴리프로필렌(Polypropylene), 폴리에틸렌(Polyethylene) 또는 이들의 혼합물이고,
상기 고분자 과립은 SiC 분말 총 중량 대비 5 내지 50중량% 포함되는, SiC 성형체 제조방법.Preparing a mixed solution by mixing and dispersing a dispersant, SiC powder, and polymer granules in a solvent;
Mixing an alkaline substance into the mixed solution;
Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances;
Manufacturing the slurry into a molded body; and
Comprising: calcining the molded body,
Preparing a mixed solution by mixing and dispersing a dispersant, SiC powder, and polymer granules in the solvent; in this, the polymer granules are polypropylene, polyethylene, or a mixture thereof,
A method for producing a SiC molded body, wherein the polymer granules are contained in an amount of 5 to 50% by weight based on the total weight of the SiC powder.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서
SiC 분말은 직경이 10㎛ 이하인, SiC 성형체 제조방법.According to paragraph 1,
Preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent;
SiC powder manufacturing method of SiC molded body with a diameter of 10㎛ or less.
용매에 분산제, SiC 분말, 고분자 과립을 혼합하여 분산시켜 혼합용액을 제조하는 단계;에서
고분자 과립은 직경이 SiC 분말 직경의 1배 내지 10배인, SiC 성형체 제조방법.According to paragraph 1,
Preparing a mixed solution by mixing and dispersing the dispersant, SiC powder, and polymer granules in a solvent;
A method of producing a SiC molded body, wherein the polymer granules have a diameter 1 to 10 times the diameter of the SiC powder.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서
알칼리 물질은 암모니아, NaOH, 및 TMAH (Tetramethylammonium hydroxide)로 이루어진 군 중에서 선택된 1종 이상인, SiC 성형체 제조방법.According to paragraph 1,
mixing an alkaline substance into the mixed solution;
A method of manufacturing a SiC molded body, wherein the alkaline material is at least one selected from the group consisting of ammonia, NaOH, and TMAH (Tetramethylammonium hydroxide).
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서
알칼리 물질이 혼합된 혼합용액의 pH는 10 이상인, SiC 성형체 제조방법.According to paragraph 1,
mixing an alkaline substance into the mixed solution;
A method of manufacturing a SiC molded body in which the pH of the mixed solution containing alkaline substances is 10 or more.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;에서
알칼리 물질은 혼합용액 전체 중량에 대하여 2 중량% 이하로 첨가되는, SiC 성형체 제조방법.According to paragraph 1,
mixing an alkaline substance into the mixed solution;
A method of manufacturing a SiC molded body in which the alkaline substance is added in an amount of 2% by weight or less based on the total weight of the mixed solution.
상기 혼합용액에 알칼리 물질을 혼합하는 단계;는
혼합용액에 알칼리 물질을 혼합한 후 용액을 에이징 하고 탈포하는 단계를 더 포함하는, SiC 성형체 제조방법.According to paragraph 1,
Mixing an alkaline substance into the mixed solution;
A method for producing a SiC molded body, further comprising mixing an alkaline material in the mixed solution and then aging and defoaming the solution.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서
응고제는 염산, 불산 및 포름산메틸(Methyl formate)로 이루어진 군 중에서 선택된 1종 이상인, SiC 성형체 제조방법.According to paragraph 1,
Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances;
A method of producing a SiC molded body, wherein the coagulant is at least one selected from the group consisting of hydrochloric acid, hydrofluoric acid, and methyl formate.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서
응고제는 알칼리 물질에 대하여 당량비로 1.2 내지 1.4 당량으로 첨가되는, SiC 성형체 제조방법.According to paragraph 1,
Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances;
A method for manufacturing a SiC molded body, wherein the coagulant is added in an equivalent ratio of 1.2 to 1.4 with respect to the alkaline material.
상기 알칼리 물질이 혼합된 혼합용액에 응고제를 혼합하여 슬러리를 제조하는 단계;에서
응고제가 투입된 슬러리는 pH가 6 내지 9인, SiC 성형체 제조방법.According to paragraph 1,
Preparing a slurry by mixing a coagulant with the mixed solution of the alkaline substances;
A method of manufacturing a SiC molded body in which the slurry containing the coagulant has a pH of 6 to 9.
상기 슬러리를 성형하여 성형체를 제조하는 단계;는
성형체를 상온에서 건조하는 단계; 및
상온 건조된 성형체를 건조 오븐에서 추가 건조하는 단계;
를 더 포함하는, SiC 성형체 제조방법.According to paragraph 1,
Manufacturing the slurry into a molded body;
Drying the molded body at room temperature; and
Additional drying of the molded body dried at room temperature in a drying oven;
A method for manufacturing a SiC molded body, further comprising:
상기 성형체를 하소시키는 단계;는
온도 700℃ 이상에서 5시간 이상 성형체를 하소시키는 단계인, SiC 성형체 제조방법.According to paragraph 1,
Calcining the molded body;
A method of manufacturing a SiC molded body, which involves calcining the molded body at a temperature of 700°C or higher for more than 5 hours.
상기 성형체를 하소시키는 단계;는
고분자 과립을 산화시켜 다공질 조직을 형성하는 단계인, SiC 성형체 제조방법.According to paragraph 1,
Calcining the molded body;
A method of manufacturing a SiC molded body, which is a step of oxidizing polymer granules to form a porous structure.
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