KR20000040861A - Graphite castings with anti oxidation property - Google Patents

Graphite castings with anti oxidation property Download PDF

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KR20000040861A
KR20000040861A KR1019980056603A KR19980056603A KR20000040861A KR 20000040861 A KR20000040861 A KR 20000040861A KR 1019980056603 A KR1019980056603 A KR 1019980056603A KR 19980056603 A KR19980056603 A KR 19980056603A KR 20000040861 A KR20000040861 A KR 20000040861A
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graphite
oxidation
added
weight
binder
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KR1019980056603A
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KR100299462B1 (en
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박세민
홍기곤
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신현준
재단법인 포항산업과학연구원
홍상복
포스코신기술연구조합
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • C04B35/52—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 carbon, e.g. graphite
    • C04B35/522—Graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

PURPOSE: Graphite castings with anti oxidation property is provided, which can be applicable to heat resistant materials in the various industries. CONSTITUTION: In one embodiment of the invention, a manufacturing process of graphite castings with anti oxidation property is like these. First, 100 parts by weight of crystalline graphite ( purity 99% ) is mixed with 5 parts by weight of phenol-based resin. Second, 5 parts by weight of boric acid dissolved in ethyl alcohol is added thereto. Finally, the mixture is heat-treated at 180°C.

Description

내산화성이 우수한 흑연성형체Graphite molding with excellent oxidation resistance

본 발명은 흑연성형체에 관한 것으로, 상세하게는 흑연골재의 표면을 용매 가용성 의 액상 보론 화합물로 피복하여 흑연성형체의 내산화성을 크게 개선하고 나아가 성형체내에 원료물질의 균일한 혼합도 유도할 수 있는 흑연성형체의 조성에 관한 것이다.The present invention relates to a graphite molded body, and in particular, the surface of the graphite aggregate is coated with a solvent-soluble liquid boron compound to greatly improve the oxidation resistance of the graphite molded body and further induce uniform mixing of raw materials in the molded body. It relates to the composition of the graphite molded body.

탄소재료는 다른 세라믹 재료나 금속재료에 비해, 우수한 전기적, 열적, 기계적 성질을 지니고 있는 재료로서, 반도체 및 우주항공산업에서 철강산업에 이르기까지 고온부위의 내열재료로써 폭넓게 사용되고 있는 재료이다. 그러나, 이러한 우수한 특성에 비해 산화반응에 대한 저항성은 열등하기 때문에 탄소재료의 내산화성을 개선하는데 연구가 집중되고 있다.Carbon materials have excellent electrical, thermal, and mechanical properties compared to other ceramic materials and metal materials, and are widely used as heat-resistant materials in high temperature parts from the semiconductor and aerospace industries to the steel industry. However, since the resistance to oxidation is inferior to these excellent properties, research has been focused on improving the oxidation resistance of carbon materials.

이러한 연구들로는 탄소재료 표면에 CVD 등에 의한 방법으로 SiC 와 같은 탄화물이나 천이금속등의 산화방지층을 형성시키거나, 분말상태의 산화방지제를 첨가하여 혼합하는 내산화성을 개선하는 방법등이 주류를 이루고 있다. 표면에 코팅층을 형성시키는 방법은 고가의 장비를 사용하여야 하므로 일반 내화물이나 단열재와 같은 내열재료로 사용하는데는 가격상의 한계가 있다. 또한, 고상의 분말을 혼합하는 방법에 있어서는 산화방지제 분말의 균일한 혼합을 기대하기 어렵다.These studies are mainly used to form an oxidation-resistant layer of carbides such as SiC, transition metals, or the like by adding CVD to the surface of carbon materials, or to improve oxidation resistance by adding a powdered antioxidant. . Since the method of forming a coating layer on the surface requires the use of expensive equipment, there is a price limitation in using it as a heat resistant material such as a general refractory material or a heat insulating material. Moreover, in the method of mixing solid powder, it is difficult to expect uniform mixing of antioxidant powder.

따라서, 최근에는 금속 유기화합물이나 금속염등을 액체상태로 하여 흑연성형체의 표면에 코팅하는 방법(일본 공개특허공보 평10-226573호)이 제안되었지만, 이들은 원료가 매우 고가라는 약점과 더불어 표면에 코팅층의 쉽게 손상될 수 있다는 문제점이 있다.Therefore, in recent years, a method of coating a surface of the graphite molded body with a metal organic compound or a metal salt in a liquid state (Japanese Patent Laid-Open No. 10-226573) has been proposed. There is a problem that can be easily damaged.

따라서, 본 발명자들은 흑연골재와 산화방지제의 균일한 혼합을 위해서는 저렴한 원료를 사용하여 고체간의 상호 혼합이 아닌, 액상의 산화방지제를 성형체내에 개재시켜 흑연골재를 피복시킬 필요성을 인식하고, 본 발명을 제안하게 이르렀다.Therefore, the present inventors recognize the necessity to coat the graphite aggregate by interposing a liquid antioxidant in the molded body, rather than intermixing solids, using inexpensive raw materials for uniform mixing of the graphite aggregate and the antioxidant. Came to suggest.

본 발명은 기존 탄소재료의 산화방지제의 혼합을 성형체내에서 고체-액체간의 혼합으로 개선하여, 저렴한 가격으로 흑연과 산화방지제의 혼합을 보다 균일하게 행함으로써, 탄소재료의 산화방지효과를 극대화하는데 그 목적이 있다.The present invention improves the oxidation of the carbon material by improving the mixing of the antioxidant of the existing carbon material with the solid-liquid mixing in the molded body, and more uniformly mixing the graphite and antioxidant at a low price. There is a purpose.

상기 목적을 달성하기 위한 본 발명의 흑연성형체는, (a)흑연분말, (b)결합제 및 (c)용매가용성 보론화합물을 포함하여 조성된다.The graphite molded product of the present invention for achieving the above object is composed of (a) graphite powder, (b) binder and (c) solvent-soluble boron compound.

이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

본 발명은 결합재와 함께 액상의 산화방지제를 흑연성형체의 원료로 이용하여 성형체내에서 산화방지제의 균일혼합효과를 극대화함과 동시에 성형체내에 결합재와 흑연분말를 더욱 균일하게 분포시키는데, 그 특징이 있다. 이러한 본 발명의 흑연성형체는 (a)흑연분말골재 100중량부에 대하여 (b)결합제 및 (c)용매 가용성 보론화합물:1-20중량%로 조성되는 것으로, 이를 다음이하에 세분하여 설명한다.The present invention maximizes the homogeneous mixing effect of the antioxidant in the molded body by using a liquid antioxidant together with the binder as a raw material of the graphite molded body and at the same time distributes the binder and the graphite powder in the molded body more uniformly. The graphite molded product of the present invention is composed of (b) a binder and (c) a solvent-soluble boron compound: 1-20% by weight based on 100 parts by weight of graphite powder aggregate, which will be described in detail below.

(a)흑연분말 골재는 통상의 흑연성형체에 이용되는 것으로 인상흑연을 예로 들수 있다.(a) Graphite powder aggregate is used in ordinary graphite molded bodies, and examples thereof include impression graphite.

(b)결합제는 흑연분말을 결합시키는 역할을 하는 것으로, 고상 또는 액상의 결합제가 이용되며, 그 예로는 페놀계 수지 등이 있다. 이 결합제의 혼합량은 통상의 범위로 관리하면 된다.(b) The binder serves to bind the graphite powder, a solid or liquid binder is used, for example, a phenol resin. What is necessary is just to manage the mixing amount of this binder in a normal range.

(c)본 발명의 산화방지제는 일반적으로 탄소재료의 산화방지제로 많이 사용하는 보론산화물(B2O3)의 형태가 아니라, 물 혹은 알코올등의 용매에 용해시킨 액체상태의 보론화합물을 이용한다. 이러한 보론화합물로는, 보론산(H3BO3, 붕산) 또는 염화보론(B2Cl4)을 예로 들 수 있다. 본 발명에 따라 혼합되는 보론화합물의 양은 1-20중량%로 하는 것이 바람직한데, 이는 1중량%미만의 극소량으로 할 경우에는 산화방지의 효과가 충분히 발휘될 수 없으며, 20중량% 이상의 양을 첨가하게 되면 소성시 보론화합물의 분해(예 보론산의 경우 2H3BO3→ B2O3+ 3H2O)에 의해 형성되는 기공에 기인한 소성체 표면의 유효 반응면적이 크게 증가하여 산화방지 효과가 크게 떨어질 수가 있다.(c) Antioxidant of the present invention generally uses a boron compound in a liquid state dissolved in a solvent such as water or alcohol, not in the form of boron oxide (B 2 O 3 ) commonly used as an antioxidant of a carbon material. Examples of such boron compounds include boronic acid (H 3 BO 3 , boric acid) or boron chloride (B 2 Cl 4 ). The amount of the boron compound to be mixed according to the present invention is preferably 1 to 20% by weight. When the amount is less than 1% by weight, the antioxidant effect cannot be sufficiently exhibited, and an amount of 20% or more by weight is added. When it is fired, the effective reaction area on the surface of the fired body due to the pores formed by decomposition of boron compounds (for example, 2H 3 BO 3 → B 2 O 3 + 3H 2 O in the case of boronic acid) increases greatly, thereby preventing oxidation. Can fall significantly.

상기와 같이 원료을 혼합하고 통상의 방법대로 성형한 다음, 소성하면 흑연 성형체가 제공되는데, 이 흑연성형체내에는 산화방지제가 균일하게 분포함과 동시에, 혼합물의 점도를 낮추어 결합재와 흑연골재 분말이 균일혼합되어 있다.As described above, the raw materials are mixed and molded according to a conventional method, and then fired to provide a graphite molded body. In the graphite molded body, an antioxidant is uniformly distributed and the viscosity of the mixture is lowered to uniformly mix the binder and the graphite aggregate powder. It is.

이하, 본 발명을 실시예를 통해서 구체적으로 설명한다.Hereinafter, the present invention will be described in detail through examples.

[실시예 1]Example 1

인상흑연(순도: 99%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 5% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 10% 의 산화에 의한 중량감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 18% 의 중량감소를 나타내었다.5% phenolic resin was added to the impression graphite (purity: 99%) as a binder, and 5% of boronic acid dissolved in ethyl alcohol was added to the mixture. Oxidation for 1 hour in the furnace maintained resulted in a weight loss of 10% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a weight loss of 18%.

[실시예 2]Example 2

인상 흑연(순도: 99%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 3% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃ 를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 12% 의 산화에 의해 중량 감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 18% 의 중량감소를 나타내었다.5% phenolic resin was added to the impression graphite (purity: 99%) as a binder, and 3% of boronic acid dissolved in ethyl alcohol was added at the time of mixing. Oxidation for 1 hour in the holding furnace showed weight loss by oxidation of 12%. Graphite moldings prepared by the same process without addition of antioxidants showed a weight loss of 18%.

[실시예 3]Example 3

인상 흑연(순도 : 99%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸알코올에 용해시킨 보론산을 3% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 11% 의 산화에 의한 중량 감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 18% 의 중량감소를 나타내었다.5% phenolic resin was added as a binder to the impression graphite (purity: 99%) powder, and 3% of boronic acid dissolved in ethyl alcohol was added at the time of mixing. Oxidation for 1 hour in the holding furnace showed a weight loss of 11% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a weight loss of 18%.

[실시예 4]Example 4

인상흑연(순도: 98%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 5% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 15% 의 산화에 의한 중량 감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 20% 의 중량감소를 나타내었다.5% phenolic resin was added to the impression graphite (purity: 98%) as a binder, and 5% of boronic acid dissolved in ethyl alcohol was added at the time of mixing. Oxidation in the holding furnace for 1 hour resulted in a weight loss of 15% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a 20% weight loss.

[실시예 5]Example 5

인상흑연(순도: 98%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 3% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃ 를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 13% 의 산화에 의한 중량감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 20% 의 중량감소를 나타내었다.5% phenolic resin was added to the graphite powder (purity: 98%) as a binder, and 3% of boronic acid dissolved in ethyl alcohol was added at the time of mixing. Oxidation for 1 hour in the furnace maintained resulted in a weight loss of 13% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a 20% weight loss.

[실시예 6]Example 6

인상흑연(순도 : 98%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 1% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃ 를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 12% 의 산화에 의한 중량감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 20% 의 중량감소를 나타내었다.5% phenolic resin was added to the impression graphite (purity: 98%) as a binder, 1% boronic acid dissolved in ethyl alcohol was added at the time of mixing, and the formed body was heat-treated at 180 ° C. Oxidation for 1 hour in the furnace maintained resulted in a weight loss of 12% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a 20% weight loss.

[실시예 7]Example 7

인상흑연(순도: 85%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 3% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃ 를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 18% 의 산화에 의한 중량감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 26% 의 중량감소를 나타내었다.5% phenolic resin was added to the impression graphite (purity: 85%) as a binder, and 3% of boronic acid dissolved in ethyl alcohol was added at the time of mixing. Oxidation in the holding furnace for 1 hour resulted in a weight loss of 18% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a 26% weight loss.

[실시예 8]Example 8

인상흑연(순도: 85%) 분말에 페놀계 수지를 결합재로 5% 첨가하고, 혼합시 에틸 알코올에 용해시킨 보론산을 1% 첨가하여, 180℃에서 열처리한 성형체를, 대기분위기, 1000℃를 유지하고 있는 로에서 1시간 동안 산화시킨 결과 15% 의 산화에 의한 중량 감소를 나타내었다. 산화방지제를 첨가하지 않은 동일한 공정으로 제조한 흑연성형체의 경우에는 26% 의 중량감소를 나타내었다.5% phenolic resin was added to the graphite powder (purity: 85%) as a binder, 1% boronic acid dissolved in ethyl alcohol was added to the mixture, and the molded article was heat-treated at 180 ° C. Oxidation in the holding furnace for 1 hour resulted in a weight loss of 15% oxidation. Graphite moldings prepared by the same process without addition of antioxidants showed a 26% weight loss.

상술한 바와 같이, 본 발명은 산화방지제를 성형체내에 개재시켜 액상으로서 흑연골재를 피복함으로써 흑연성형체의 산화방지 효과를 크게 향상시킬 수 있다.As described above, the present invention can greatly improve the antioxidant effect of the graphite molded body by interposing the graphite aggregate as a liquid by interposing an antioxidant in the molded body.

Claims (2)

흑연분말과 결합제로 이루어지는 흑연성형체에 있어서,In the graphite molded body consisting of graphite powder and a binder, 상기 흑연분말 100중량부에 대하여 용매가용성 보론화합물:1-20중량%를 포함하여 조성됨을 특징으로 하는 내산화성이 우수한 흑연성형체Excellent graphite resistance, characterized in that the composition containing the solvent-soluble boron compound: 1-20% by weight based on 100 parts by weight of the graphite powder 제 1항에 있어서, 상기 보론화합물은 보론산 또는 염화보론의 그룹에서 선택된 1종임을 특징으로 하는 흑연성형체.The graphite molded body according to claim 1, wherein the boron compound is one selected from the group consisting of boronic acid or boron chloride.
KR1019980056603A 1998-12-21 1998-12-21 FORMED GRAPHITE WITH excellent OXIDATION RESISTANCE KR100299462B1 (en)

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KR100574698B1 (en) * 2003-11-18 2006-04-27 박정현 Process for manufacturing a graphite heating element and a graphite heating element manufactured by the same

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KR20050064539A (en) * 2003-12-24 2005-06-29 재단법인 포항산업과학연구원 Manufacturing method of exfoliated graphite from surface-treated graphite

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100574698B1 (en) * 2003-11-18 2006-04-27 박정현 Process for manufacturing a graphite heating element and a graphite heating element manufactured by the same

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