KR970001053B1 - Process for preparation cordierite matrix ceramics - Google Patents

Process for preparation cordierite matrix ceramics Download PDF

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KR970001053B1
KR970001053B1 KR1019940006463A KR19940006463A KR970001053B1 KR 970001053 B1 KR970001053 B1 KR 970001053B1 KR 1019940006463 A KR1019940006463 A KR 1019940006463A KR 19940006463 A KR19940006463 A KR 19940006463A KR 970001053 B1 KR970001053 B1 KR 970001053B1
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cordierite
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KR950026836A (en
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손건석
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사단법인 고등기술연구원 연구조합
김준성
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
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    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
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    • 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
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • 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
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract

Process for preparing cordierite matrix ceramics is described. Thus, the process comprises i)mixing allumina sol and silica sol at a molar ratio of Al2O3 to SIO2 of 1.37-1.76, ii)mixing obtained mixture with dispersed solution of reinforcing agent such as SiC whisker and magnesia sol by turns to give a gel mixture, iii)drying and sintering at 300-500 deg.C.in a ball mill, and grinded. The process improves hardness of ceramic product.

Description

코디에라이트 복합체 세라믹의 제조방법Manufacturing method of cordierite composite ceramic

본 발명은 코디에라이트 복합체의 제조방법에 관한 것이다.The present invention relates to a method for producing a cordierite composite.

세라믹은 종래의 소재에 비해 많은 장점을 가지나 취성에 의한 파괴가 큰 문제점으로 지적되었다. 이러한 단점을 극복하고 보다 가혹한 환경에서 사용하기 위해 제2상인 보강재로서 섬유, 휘스커(whisker), 플레이트 또는 입자 등을 혼합하여 복합체를 제조하는 방법이 개발되어 왔다. 일반적으로 이들 보강재는 개별적인 공정을 거쳐 제조된 후 세라믹 재료와 혼합, 건조, 성형 및 소결의 과정을 거쳐 최종 세라믹 제품으로 제조된다.Ceramics have many advantages over conventional materials, but have been pointed out as a major problem due to brittleness. In order to overcome these disadvantages and use in a harsher environment, a method of preparing a composite by mixing fibers, whiskers, plates, or particles as a reinforcing material as a second phase has been developed. In general, these reinforcements are manufactured through a separate process and then mixed with a ceramic material, dried, molded and sintered into a final ceramic product.

파인 세라믹(fine ceramic)중 코디에라이트(coordierite)는 열팽창성 및 유전성(dielectric)이 낮고 화학적, 열적 안정성이 높기 때문에 전자 산업, 환경산업 또는 우주 산업 등에 널리 사용되고 있다. 일반적인 코디에라이트 글래스 세라믹은 적정량의 여러 산화막 세라믹을 균일하게 혼합한 후 건조하고 이를 고온에서 용융한 후 퀀칭(quenching)하여 고체로 성형하고, 얻어진 고체를 분쇄하여 분말을 얻고, 분말을 900 내지 1000℃에서 하소(calcining)하는 방법을 제조된다.Among fine ceramics, coordierite is widely used in the electronics industry, the environmental industry, or the space industry because of low thermal expansion and dielectric, high chemical and thermal stability. A typical cordierite glass ceramic is uniformly mixed with various oxide film ceramics in an appropriate amount, dried, melted at a high temperature, quenched to form a solid, the obtained solid is pulverized to obtain a powder, and the powder is 900 to 1000 A method of calcining at 캜 is prepared.

그러나 이 방법에 의해 제조된 코디에라이트 세라믹은 소결온도 범위가 좁아 충분한 충분한 소결이 어렵고 분자구조내에 있는 H2O의 영향으로 고밀도의 소결체 제조가 불가능하다. 따라서 일반적인 코디에라이트는 저밀도의 소결체로 제조되기 때문에 기계적 강도가 낮아서 그 사용 폭이 제한될 수 밖에 없다.However, the cordierite ceramics produced by this method have a narrow sintering temperature range, making it difficult to sufficiently sinter sufficiently and making high density sintered bodies under the influence of H 2 O in the molecular structure. Therefore, since general cordierite is made of a sintered compact of low density, the mechanical strength is low and the use width thereof is limited.

이러한 문제점을 극복하기 위해서 고밀도의 코디에라이트를 제조하기 위한 방법으로 K2O 또는 TiO2와 같은 소결첨가제를 사용하는 방법이 개발되었다. 이러한 첨가제의 사용에 의해서 고밀도의 코디에라이트가 제조되었으나 이들 첨가제의 작용으로 인해 코디에라이트의 최대 장점인 낮은 열팽창계수가 높아지는 결과를 초래하였다.In order to overcome this problem, a method of using a sintering additive such as K 2 O or TiO 2 has been developed as a method for producing high density cordierite. High density cordierite was produced by the use of such additives, but the action of these additives resulted in a high coefficient of thermal expansion, which is the greatest advantage of cordierite.

따라서 낮은 열팽창계수를 유지하면서 고밀도 코디에라이트를 제조하는 방법으로서 미국 특허 제5,064,783호는 SSG(solution sol-gel) 방법을 제안하였다. 이 방법에서는 중합 알콕시드(alkoxide)를 사용하여 금속 알콕시드를 형성한 후 분해와 결합의 과정을 거쳐 금속-산소-금속 결합을 형성하는 원리를 이용하고 있다. 미국 특허 제5,045,514호는 뮬라이드 졸과 코디에라이트 졸을 별도로 제조한 후 뮬라이트 졸 및 코디에라이트 졸을 혼합하고 겔화시키고, 얻어진 겔을 1200℃ 내지 1400℃에서 하소(calcining)한 후 소결함으로써 뮬라이트/코디에라이트 세라믹 파우더를 제조하는 방법을 개시하고 있다.Therefore, US Pat. No. 5,064,783 proposes a solution sol-gel (SSG) method as a method for producing high density cordierite while maintaining a low coefficient of thermal expansion. In this method, the polymer alkoxide is used to form a metal alkoxide, followed by decomposition and bonding to form a metal-oxygen-metal bond. U.S. Patent No. 5,045,514 discloses mullite by separately preparing a mullide sol and cordierite sol, mixing and gelling the mullite sol and cordierite sol, calcining the obtained gel at 1200 ° C to 1400 ° C and then sintering / Method for producing cordierite ceramic powder is disclosed.

한편, 보강재는 일반적으로 탄소 열환원법(carbothermal reduction process) 또는 증기-액체-고체 제법(vapor-liquid-solid process)에 의해 제조된다. 예컨대, SiC 휘스커의 경우 원료를 900℃에서 하소한 후 1700℃에서 열분해하여 제조한다. 이렇게 별개로 제조된 보강재와 세라믹 분말을 분산용매에서 교반 또는 초음파 처리를 통해 균일하게 분산시킨 후 항온기에서 건조한 후 하소하고 볼밀로 분쇄한다. 이 혼합체를 성형 및 소결하여 세라믹 제품이 완성된다.Reinforcements, on the other hand, are generally produced by a carbon thermal reduction process or a vapor-liquid-solid process. For example, in the case of SiC whiskers are prepared by calcining the raw material at 900 ℃ and then pyrolyzed at 1700 ℃. The separately prepared reinforcing material and ceramic powder are uniformly dispersed by stirring or ultrasonication in a dispersion solvent, dried in a thermostat, calcined, and pulverized with a ball mill. The mixture is molded and sintered to complete the ceramic product.

그러나 상술한 것과 같은 방법에서는 세라믹 분말과 보강재의 균일한 분산을 위해 pH의 조절과 교반 또는 초음파 분산 등의 처리를 해야 하기 때문에 제조 비용이 증가하고 시간이 오래 걸리는 문제점이 있다. 더욱이 코디에라이트의 제조와 복합체의 제조 공정 모두에 건조 단계가 필요하므로 긴 시간을 요하는 건조 공정이 중복되어 박대한 시간과 비용이 초래되며 공정도 복잡하기 때문에 상업적인 생산방법으로는 적합하지 않다.However, the method as described above has a problem that the manufacturing cost increases and takes a long time because the process of adjusting the pH and stirring or ultrasonic dispersion for uniform dispersion of the ceramic powder and the reinforcing material. Moreover, since the drying step is required for both the manufacturing process of cordierite and the composite, the drying process which takes a long time is overlapped, which leads to a great time and cost, and the process is complicated, which is not suitable for commercial production methods.

따라서 본 발명의 목적은 세라믹 제조와 보강재 첨가를 단일공정으로 하여 공정을 단순화하고 시간과 비용을 절감하는 코디에라이트 제조방법을 제공하는 것이다.Accordingly, it is an object of the present invention to provide a method of manufacturing cordierite that simplifies the process and saves time and costs by using a ceramic manufacturing process and adding a reinforcing material in a single process.

본 발명에 따라서, 알루미나 졸 및 실리카 졸을 혼합하는 단계와, 얻어진 혼합물에 보강재의 분산액 및 마그네시아 졸을 차례로 첨가하고 균일학 혼합하여 겔 혼합물을 얻는 단계와, 생성된 혼합물을 건조시킨 후 하소한 다음 분쇄하여 코디에라이트 분말을 제조하는 단계를 포함하는 코디에라이트 기지의 세라믹 복합체의 제조방법이 제공된다.According to the present invention, the steps of mixing alumina sol and silica sol, adding a dispersion of reinforcing agent and magnesia sol to the obtained mixture in order and homogeneously mixing to obtain a gel mixture, drying the resulting mixture and then calcining Provided is a method for producing a cordierite-based ceramic composite, comprising the step of pulverizing cordierite powder.

본 발명에 따른 알루미나졸 및 실리카 졸은 졸 상태의 제품을 상업적으로 구입하거나 알루미나 분말 및 실리카 분말을 적절한 용매에 녹여서 제조할 수 있다. 알루미나 졸과 실리카 졸의 혼합비는 원하는 제품의 성질에 따라 적합하게 선택될 수 있으며, 일반적으로 Al2O3/SiO2의 몰비로 1.37 내지 1.76으로 혼합될 수 있다.The alumina sol and silica sol according to the present invention can be prepared by commercially purchasing a sol product or by dissolving alumina powder and silica powder in a suitable solvent. The mixing ratio of the alumina sol and the silica sol may be appropriately selected depending on the properties of the desired product, and may generally be mixed at 1.37 to 1.76 in a molar ratio of Al 2 O 3 / SiO 2 .

상기 알루미나 졸 및 실리카 졸의 혼합물에 보강재를 혼합하여 균일하게 교반한다. 보강재는 분산액 상태로 첨가되며 보강재의 분말이나 섬유 또는 플레이크 등을 적절한 용매에 분산시켜 제조할 수 있다. 예컨대 보강재로서 SiC 휘스커를 사용하는 경우 SiC 분말을 메틸 알콜 또는 에틸 알콜에서 교반하거나 초음파 프로브(ultrasonic probe) 등으로 균일하게 분산시켜 제조할 수 있다. 기타 보강재로서 알루미나, 지르코니아, 실리콘 나이트라이드 등을 사용할 수 있으며, 이들 보강재의 혼합량은 보강재와 최종 제품에 요구되는 성질에 따라 그 양을 조절할 수 있으나 일반적으로 조성물에 대하여 5 내지 30중량%의 범위로 첨가된다.The reinforcing material is mixed with the mixture of the alumina sol and the silica sol and stirred uniformly. The reinforcing material is added in the form of a dispersion and may be prepared by dispersing powder, fiber, or flake of the reinforcing material in a suitable solvent. For example, when SiC whiskers are used as the reinforcing material, the SiC powder may be prepared by stirring in methyl alcohol or ethyl alcohol or uniformly dispersing it with an ultrasonic probe or the like. As other reinforcing materials, alumina, zirconia, silicon nitride, and the like may be used, and the mixing amount of these reinforcing materials may be adjusted according to the properties required for the reinforcing material and the final product, but generally in the range of 5 to 30% by weight based on the composition. Is added.

이렇게 얻어진 알루미나 졸, 실리카 졸 및 보강재 분산액의 혼합물에 다시 마그네시아 졸을 첨가하여 혼합한다. 본 발명에서 사용되는 마그네시아 졸은 예컨대 마그네시아 분말을 탈이온수에 넣고 질산(HNO3)을 가하여 콜로이드 용액을 제조하여 사용할 수 있다. 본 발명에서 알루미나 졸, 실리카 졸 및 마그네시아 졸은 2MgO-2Al2O3-5SiO2를 형성할 수 있는 비율로 혼합된다.Magnesia sol is further added to the mixture of the alumina sol, the silica sol and the reinforcing material dispersion thus obtained and mixed. The magnesia sol used in the present invention may be used by preparing a colloidal solution by, for example, adding magnesia powder to deionized water and adding nitric acid (HNO 3 ). In the present invention, alumina sol, silica sol and magnesia sol are mixed in a ratio capable of forming 2MgO-2Al 2 O 3 -5SiO 2 .

이렇게 제조된 겔(gel) 상태의 혼합물을 약 100℃에서 공지의 방법, 예컨대 스프레이 드라이(spray dry) 등의 방법으로 건조시킨다. 건조된 복합체를 약 300 내지 500℃에서 하소한 후 볼밀(ball mill)로 분쇄하고, 시브(seive)로 걸러서 원하는 메시(mesh)의 분말을 선별하는 등의 방법으로 분말을 제조한다. 얻어진 분말을 필요에 따라 성형(forming) 및 소결(sintering)이 과정을 거쳐 제품화된다.The gel mixture thus prepared is dried at about 100 ° C. by a known method such as spray dry or the like. The dried composite is calcined at about 300 to 500 ℃ and then pulverized in a ball mill (ball mill), the sieve (sieve) to filter the powder of the desired mesh (mesh) to prepare a powder by the method. The powder obtained is molded and sintered as necessary to produce a product.

본 발명에 따른 코디에라이트 세라믹 복합체의 제조방법은 코디에라이트 제조시와 복합체의 제조시 중복되는 교반과정 및 건조과정을 단일화함으로써 작업시간과 비용을 절감할 수 있고 공정을 단순화함으로써 회분(batch)식 작업에 의한 대량 생산이 가능할 뿐만 아니라 이물질의 유입이 방지될 수 있다. 또한 본 발명에 따라 제조된 복합체 분말은 낮은 온도(약 1,300℃)에서 단시간(약 2시간) 소결이 가능할 뿐만 아니라 제품의 밀도가 높아서 높은 강도를 제공한다. 또한 보강재에 의해 취성 파괴가 지연되므로 세라믹 제품의 강도 및 신뢰도가 현저히 향상된다.The method for producing a cordierite ceramic composite according to the present invention can reduce work time and cost by unifying overlapping stirring and drying processes in the production of cordierite and in the production of the composite, and batches are simplified by simplifying the process. Not only mass production by food operations is possible, but foreign substances can be prevented from entering. In addition, the composite powder prepared according to the present invention is capable of sintering for a short time (about 2 hours) at a low temperature (about 1,300 ℃) as well as high density of the product provides a high strength. In addition, brittle fracture is delayed by the reinforcing material, which significantly improves the strength and reliability of the ceramic product.

Claims (5)

알루미나 졸 및 실리카 졸을 혼합하여 단계와, 얻어진 혼합물에 보강재의 분산액 및 마그네시아 졸을 차례로 첨가하고 균일하게 혼합하여 겔 혼합물을 얻는 단계와, 생성된 혼합물을 건조시킨 후 하소한 다음 분쇄하여 코디에라이트 분말을 제조하는 단계를 포함하는 코디에라이트 기지의 세라믹 복합체의 제조방법.Mixing the alumina sol and the silica sol, adding the dispersion of the reinforcing agent and the magnesia sol to the obtained mixture in order and mixing them uniformly to obtain a gel mixture, drying the resulting mixture, calcining and then pulverizing the cordierite Method for producing a ceramic composite based on cordierite comprising the step of preparing a powder. 제1항에 있어서, 상기 알루미나 졸, 실리카 졸 및 마그네시아 졸이 2MgO-2Al2O3-5SiO2를 형성할 수 있는 비율로 혼합되는 것을 특징으로 하는 방법.The method of claim 1, wherein the alumina sol, silica sol and magnesia sol are mixed in a ratio capable of forming 2MgO-2Al 2 O 3 -5SiO 2 . 제1항에 있어서, 상기 보강재가 SiC 휘스커임을 특징으로 하는 방법.The method of claim 1 wherein the stiffener is a SiC whisker. 제1항에 있어서, 300℃ 내지 500℃의 온도에서 하소하는 것을 특징으로 하는 방법.The method according to claim 1, which is calcined at a temperature of 300 ° C to 500 ° C. 제1항 내지 제4항중 어느 한 항에 있어서, 상기 코디에라이트 기지의 세라믹 복합체의 분말을 성형 및 소결하는 단계를 더 포함함을 특징으로 하는 방법.The method of any one of claims 1 to 4, further comprising forming and sintering a powder of the cordierite-based ceramic composite.
KR1019940006463A 1994-03-30 1994-03-30 Process for preparation cordierite matrix ceramics KR970001053B1 (en)

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Publication number Priority date Publication date Assignee Title
KR100761452B1 (en) * 2006-11-06 2007-10-04 한양대학교 산학협력단 Method for manufacturing cement having minute particle by chemical synthesis and method for manufacturing concrete using thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100761452B1 (en) * 2006-11-06 2007-10-04 한양대학교 산학협력단 Method for manufacturing cement having minute particle by chemical synthesis and method for manufacturing concrete using thereof

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