KR970001054B1 - Process for preparing cordierite matrix ceramics - Google Patents

Process for preparing cordierite matrix ceramics Download PDF

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KR970001054B1
KR970001054B1 KR1019940006464A KR19940006464A KR970001054B1 KR 970001054 B1 KR970001054 B1 KR 970001054B1 KR 1019940006464 A KR1019940006464 A KR 1019940006464A KR 19940006464 A KR19940006464 A KR 19940006464A KR 970001054 B1 KR970001054 B1 KR 970001054B1
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cordierite
sol
powder
magnesium nitrate
mixture
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KR950026837A (en
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최병철
손건석
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사단법인 고등기술연구원 연구조합
김준성
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract

Process for preparing codierite matrix ceramic consists of i)mixing boehmite sol and silica sol, ii)adding obtained mixture with the dispersion solution of a reinforcing agent and magnesium nitrate by turns and adding it uniformly to give a gel, iii)drying at 100 deg.C, sintering at 300-500 deg.C, crushed with a ball mill, passed through a seive, formed, and sintered. Magnesium nitrate is Mg(NO3)2.6H2O.

Description

코디에라이트 복합체 세라믹의 제조방법Manufacturing method of cordierite composite ceramic

본 발명은 코디에라이트 복합체의 제조 방법에 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 위한 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. A method of manufacturing a composite by mixing fibers, whiskers, plates, or the like as a reinforcing material as a second phase for overcoming these disadvantages and for use in a harsher environment 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 우주산업 등에 널리 사용되고 있다. 일반적으로 코디에라이트 글래스 세라믹은 적정량의 여러 산화막 세라믹을 균일하게 혼합한 후 건조하고 이를 고온에서 응용한 퀀칭(quenching)하여 고체로 성형하고, 얻어진 고체를 분쇄하여 분말을 얻고 분말을 900 내지 1000℃에서 하소(calcinig)하는 방법으로 제조된다.Among the fine ceramics (coordierite) is widely used in the electronic industry, environmental industry or aerospace industry because of low thermal expansion and dielectric, high chemical and thermal stability. In general, cordierite glass ceramics are uniformly mixed with various oxide ceramics in an appropriate amount, dried, and quenched at a high temperature to form a solid, and the obtained solid is pulverized to obtain a powder and the powder is 900 to 1000 ° C. It is prepared by the method of calcining (calcinig).

그러나 이 방법에 의해 제조된 코디에라이트 세라믹은 소결온도 범위가 좋아 충분한 소결이 어렵고 분자 구조 내에 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 high sintering temperature range, which makes it difficult to sinter enough and to produce 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 고밀도이 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 제5,045,514호로 뮬라이트 졸과 코디에라이트 졸을 별도로 제조한 후 뮬라이트 졸 및 코디에라이트 졸을 혼합하여 겔화시키고, 얻어진 겔을 1200℃ 내지 1400℃에서 하소한 후 소결함으로써 뮬라이트/코디에라이트 세라믹을 제조하는 방법을 개시하고 있다. 또한 미국 특허 제4,888,314호는 낮은 온도에서 소결하여 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. Mullite sol and cordierite sol were separately prepared in US Pat. No. 5,045,514, followed by mixing and gelling the mullite sol and cordierite sol, and calcining the obtained gel at 1200 ° C to 1400 ° C and then sintering the mullite / cordierite ceramics. Disclosed is a method of preparing the same. U. S. Patent No. 4,888, 314 also discloses a process for producing cordierite ceramic powder by sintering at low temperatures.

한편, 보강재는 일반적으로 탄소 열환원법(carbothremal reduction process) 또는 증기-액체-고체 제법(vapor-liquid-solid process)에 의해 제조된다.On the other hand, reinforcements are generally produced by a carbon thermal reduction process or a vapor-liquid-solid process.

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 세라믹이 완성된다.For example, SiC whiskers are prepared by calcining the raw material at 900 ° C. and then pyrolyzing at 1700 ° C. 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.

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 공정이 필요하므로 긴 시간을 요하는 건조 공정이 중복되어 막대한 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 process is required in both the manufacturing process of cordierite and the composite, the drying process which takes a long time is overlapped, which entails enormous 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, 보에마이트 졸 및 실리카 졸을 혼합하는 단계와, 얻어진 혼합물에 보강재의 분산액 및 마그네슘 나이트레이트 용액을 차례로 첨가하고 균일하게 혼합하여 겔 혼합물을 얻는 단계와, 생성된 혼합물을 건조시킨 후 하소한 다음 분쇄하여 코디에라이트 분말을 제조하는 단계를 포함하는 코디에라이트 기지(matrix)의 세라믹 복합체의 제조 방법이 제공된다.According to the present invention, a step of mixing a boehmite sol and a silica sol, adding a dispersion of a reinforcing agent and a magnesium nitrate solution to the obtained mixture in order and uniformly mixing to obtain a gel mixture, and drying the resulting mixture After calcination and then pulverized to provide a cordierite powder is provided a method of producing a ceramic composite of cordierite matrix (matrix).

본 발명에 따른 보에마이트(boehmite) 졸은 탈이온수에 보에마이트 분말을 넣고 질산(1N HNO3)을 가하여 pH3, 또는 4에서 오팔레슨트 졸(opalescent sol)로 제조한다. 이렇게 얻어진 보에마이트 졸에 실리카 졸을 가하여 교반함으로써 균일하게 혼합한다.The boehmite sol according to the present invention is prepared by adding boehmite powder to deionized water and adding nitric acid (1N HNO 3 ) to an opalescent sol at pH 3 or 4. A silica sol is added to the boehmite sol thus obtained, and it mixes uniformly by stirring.

상기 보에마이트 졸 및 실리카 졸의 혼합물에 보강재로 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 mixture of boehmite sol and silica sol is mixed as a reinforcing material 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 can be used. The amount of the reinforcing material can be adjusted according to the properties required for the reinforcing material and the final product, but is generally added in the range of 5 to 30% by weight based on the composition. do.

이렇게 얻어진 보에마이트 졸, 실리카 졸 및 보강재 분산액의 혼합물에 다시 마그네슘 나이트레이트 용액, 바람직하게는 Mg(NO3)2·6H2O 용액을 첨가하여 혼합한다. 본 발명에서 사용되는 Mg(NO3)2·6H2O 용액은 예컨대 마그네슘 나이트레이트 분말을 탈이온 수에 가하여 용액(solution) 상태로 제조하여 사용할 수 있다. 본 발명에서 보에마이트 졸, 실리카 졸 및 마그네슘 나이트레이트 용액은 2Mg-2Al2O3-5SiO2를 형성할 수 있는 비율로 혼합된다.Magnesium nitrate solution, preferably Mg (NO 3 ) 2 .6H 2 O solution is added to the mixture of the boehmite sol, silica sol and reinforcing agent dispersion thus obtained and mixed. The Mg (NO 3 ) 2 .6H 2 O solution used in the present invention may be prepared by, for example, adding magnesium nitrate powder to deionized water in a solution state. In the present invention, the boehmite sol, the silica sol, and the magnesium nitrate solution are mixed in a ratio capable of forming 2Mg-2Al 2 O 3 -5SiO 2 .

이렇게 제조진 혼합물을 충분히 교반한 후 겔(gel) 상태의 혼합물을 약 100℃에서의 공지의 방법, 예컨대 스프레이 드라이(spray dry)하여 건조시킨다. 건조된 복합체를 약 300 내지 500℃의 온도에서 하소한 후 볼밀(ball mill)로 분쇄하고 시브(seive)로 걸러서 원하는 메시(mesh)의 분말을 선별하는 등의 방법으로 분말을 제조한다. 얻어진 분말은 필요에 따라 성형(forming) 및 소결(sintering)의 과정을 거쳐 제품화된다.The mixture thus prepared is sufficiently stirred and then the gelled mixture is dried by a known method at about 100 ° C., such as spray dry. The dried composite is calcined at a temperature of about 300 to 500 ℃ and then pulverized in a ball mill (ball mill) and sieve (sieve) to filter the desired mesh (mesh) to select the powder (mesh) to prepare a powder. The powder obtained is commercialized through a process of forming and sintering as necessary.

본 발명에 따른 코디에라이트 세라믹 복합체의 제조 방법은 코디에라이트 제조시와 복합체 제조시 중복되는 교반과정 및 건조과정을 단일화함으로써 작업시간과 비용을 복합체 제조시 중복되는 교반과정 및 건조과정을 단일화함으로써 작업시간과 비용을 절감할 수 있고 공정을 단순화함으로써 회분(batch)식 작업에 의한 대량생산이 가능할 뿐만 아니라 이물질의 유입을 방지될 수 있다. 또한 본 발명에 따라 제조된 복합체 분말을 낮은 온도(약 1,300℃)에서 단시간(약 2시간) 소결이 가능할 뿐만 아니라 제품의 밀도가 높아서 높은 강도를 제공하낟. 더욱이 첨가된 보강재에 의해 취성 파괴가 지연되므로 세라믹의 강도 및 신뢰도가 현저히 향상된다.Method for producing a cordierite ceramic composite according to the present invention by unifying the overlapping stirring process and drying process in the production of cordierite and composites by unifying the overlapping stirring process and drying process in manufacturing the composite By reducing the working time and cost, and simplifying the process, not only mass production by batch operation can be carried out, but also foreign substances can be prevented from entering. In addition, the composite powder prepared according to the present invention is capable of sintering at low temperatures (about 1,300 ° C.) for a short time (about 2 hours) as well as providing high strength due to the high density of the product. Moreover, the brittle fracture is delayed by the added reinforcing material, which significantly improves the strength and reliability of the ceramic.

Claims (6)

보에마이트 졸 및 실리카 졸을 혼합하는 단계와, 얻어진 혼합물에 보강재의 분산액 및 마그네슘 나이트레이트 용액을 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 boehmite sol and the silica sol, adding the dispersion of the reinforcing agent and the magnesium nitrate solution to the obtained mixture in order and mixing them uniformly to obtain a gel mixture, drying the resulting mixture, calcining and then grinding Method for producing a cordierite-based ceramic composite comprising the step of producing a cordierite powder. 제1항에 있어서, 상기 보에마이트 졸, 실리칼 졸 및 마그네시아 졸이 2MgO-2Al2O3-5SiO2를 형성할 수 있는 비율로 혼합되는 것을 특징으로 하는 방법.The method of claim 1 wherein the boehmite sol, the silica sol and the magnesia sol are mixed in a proportion capable of forming 2MgO-2Al 2 O 3 -5SiO 2 . 제1항에 있어서, 상기 마그네슘 나이트레이트 용액이 Mg(NO3)2·6H2O 용액임을 특징으로 하는 방법.The method of claim 1 wherein the magnesium nitrate solution is Mg (NO 3 ) 2 .6H 2 O solution. 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 to 500 ° C. 제1항 내지 제5항중 어느 한 항에 있어서, 상기 코디에라이트 기지의 세라믹 복합체의 분말을 충전 및 소결하는 단계를 더 포함함을 특징으로 하는 방법.The method of any one of claims 1 to 5, further comprising the step of filling and sintering powder of the cordierite-based ceramic composite.
KR1019940006464A 1994-03-30 1994-03-30 Process for preparing cordierite matrix ceramics KR970001054B1 (en)

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