KR20030095118A - Method for preparing alumina-zirconia composite - Google Patents

Method for preparing alumina-zirconia composite Download PDF

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KR20030095118A
KR20030095118A KR1020020032642A KR20020032642A KR20030095118A KR 20030095118 A KR20030095118 A KR 20030095118A KR 1020020032642 A KR1020020032642 A KR 1020020032642A KR 20020032642 A KR20020032642 A KR 20020032642A KR 20030095118 A KR20030095118 A KR 20030095118A
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alumina
zirconia
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composite
aqueous solution
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KR100481057B1 (en
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황규홍
이종국
조명제
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대한민국 (경상대학교 총장)
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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
    • C04B35/01—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
    • C04B35/10—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 aluminium oxide
    • C04B35/101—Refractories from grain sized mixtures
    • C04B35/106—Refractories from grain sized mixtures containing zirconium oxide or zircon (ZrSiO4)
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802—Powder coating materials
    • C04B35/62805—Oxide ceramics
    • C04B35/62818—Refractory metal oxides
    • C04B35/62823—Zirconium or hafnium oxide
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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
    • C04B35/6261—Milling
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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
    • C04B35/64—Burning or sintering processes

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Abstract

PURPOSE: A process for making an alumina-zirconia composite wherein zirconia particles are dispersed homogeneously in alumina ceramics is provided to improve the mechanical strength and toughness of the composite. CONSTITUTION: The process for making an alumina-zirconia composite comprises the steps of: adding conventional alumina(Al2O3) powder to an aqueous solution of zirconium oxychloride(ZrOCl2) to disperse 5-20 volume% of zirconia; co-precipitating or hydrolyzing the aqueous solution of zirconium oxychloride(ZrOCl2) in which the alumina(Al2O3) powders are dispersed to deposit zirconium-hydroxide on the surface of the alumina(Al2O3) particles; and sintering and firing the composite.

Description

알루미나-지르코니아 복합체의 제조 방법{Method for preparing alumina-zirconia composite}Method for preparing alumina-zirconia composite {Method for preparing alumina-zirconia composite}

본 발명은 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 제조 방법에 관한 것이다. 더욱 상세하게는 복합체의 하소 및 소결 과정에서 지르코니아(ZrO2)의 입자 성장을 억제하는 것에 의해 기계적 강도와 인성을 향상시킬 수 있는 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 제조 방법에 관한 것이다.The present invention relates to a method for preparing an alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite. More specifically, a method for producing an alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite which can improve mechanical strength and toughness by inhibiting grain growth of zirconia (ZrO 2 ) during calcination and sintering of the composite. It is about.

종래 알루미나(Al2O3) 세라믹스에 지르코니아(ZrO2) 입자를 분산시켜 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 기계적 강도와 인성을 향상시키려는 많은 시도가 있었다. 그러나, 종래 두 분말의 기계적 혼합에 의한 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 제조에서는 첨가되는 지르코니아(ZrO2)의 초기 입자 크기가 크고, 알루미나(Al2O3)의 높은 소결 온도 때문에 지르코니아(ZrO2)의 입자 크기의 제어가 힘들었고 균일한 분산도 어려운 문제점이 있었다.Many attempts have been made to improve the mechanical strength and toughness of alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composites by dispersing zirconia (ZrO 2 ) particles in alumina (Al 2 O 3 ) ceramics. However, in the preparation of alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite by the mechanical mixing of the two powders, the initial particle size of the added zirconia (ZrO 2 ) is large, the high of the alumina (Al 2 O 3 ) Due to the sintering temperature, it was difficult to control the particle size of zirconia (ZrO 2 ) and uniform dispersion was also difficult.

공침법이나 가수 분해에 의해 제조된 10 내지 50 nm 크기의 지르코니아(ZrO2) 분말일지라도 2차 입자로의 응집을 피하기 어렵기 때문에 이를 알루미나(Al2O3)에 혼합하여 하소 및 소결하는 경우, 치밀화되는 과정에서 0.2 내지 1㎛ 이상의 결정립으로 순식간에 성장하게 되므로 진정한 의미의 초미립 나노 입자가 분산된 소결 복합체를 얻기는 힘들다.Even in the case of 10 to 50 nm zirconia (ZrO 2 ) powders prepared by coprecipitation or hydrolysis, it is difficult to avoid agglomeration into secondary particles, so that when they are mixed with alumina (Al 2 O 3 ) and calcined and sintered, In the process of densification, since 0.2 to 1 ㎛ grains are grown in an instant, it is difficult to obtain a sintered composite in which ultrafine nanoparticles are dispersed in a true sense.

따라서, 본 발명은 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 제조 시 지르코니아(ZrO2)가 2차 입자로 응집이 이루어지지 않는 상태에서 알루미나(Al2O3) 세라믹스에 분산시키는 것이 무엇보다도 중요하다는 사실에 기초하여 완성하게 된 것으로 본 발명의 목적은 복합체의 하소 및 소결 과정에서 지르코니아(ZrO2)의 입자 성장을 억제하는 것에 의해 기계적 강도와 인성을 향상시킬 수 있는 알루미나(Al2O3)-지르코니아(ZrO2) 복합체의 제조 방법을 제공하고자 하는 것이다.Accordingly, the present invention is to disperse the zirconia (ZrO 2 ) in the alumina (Al 2 O 3 ) ceramics in the state that the zirconia (ZrO 2 ) is not agglomerated into secondary particles in the preparation of the alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite The object of the present invention is to alumina (Al) which can improve the mechanical strength and toughness by inhibiting the growth of zirconia (ZrO 2 ) particles during the calcination and sintering of the composite. It is to provide a method for preparing a 2 O 3 ) -zirconia (ZrO 2 ) complex.

본 발명은 알루미나(Al2O3) 상용 분말을 옥시염화지르코늄(ZrOCl2) 수용액에 첨가하되 부피의 비로 5 내지 20％의 지르코니아(ZrO2)가 분산될 수 있도록 상기 수용액을 혼합하고, 이어서, 상기 알루미나(Al2O3) 분말이 분산된 옥시염화지르코늄(ZrOCl2) 수용액을 공침 하거나 가수분해시켜서 알루미나(Al2O3) 입자 표면에 지르코늄-히드록시드가 부착되도록 한 후 하소 및 소결 처리하여서 알루미나(Al2O3)-지르코니아(ZrO2) 복합체를 제조하는 방법임을 특징으로 한다.In the present invention, alumina (Al 2 O 3 ) commercial powder is added to an aqueous solution of zirconium oxychloride (ZrOCl 2 ), but the aqueous solution is mixed so that 5 to 20% of zirconia (ZrO 2 ) can be dispersed in a volume ratio, and then, The zirconium hydroxide is attached to the surface of the alumina (Al 2 O 3 ) particles by immersion or hydrolysis of the zirconium oxychloride (ZrOCl 2 ) aqueous solution in which the alumina (Al 2 O 3 ) powder is dispersed, followed by calcination and sintering. It characterized in that the method for producing an alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) complex.

본 발명의 방법에 의하면, 평균 입경이 0.1 내지 0.5㎛ 정도의 범위에 있는 이소결성의 상용 알루미나(Al2O3) 분말이나, 저온 소결용 고순도 알루미나(Al2O3) 분말을 옥시염화지르코늄(ZrOCl2) 수용액에 첨가하되 부피의 비로 5 내지 20％의 지르코니아(ZrO2)가 분산될 수 있도록 상기 수용액을 혼합한다.According to the method of the present invention, zirconium oxychloride is used to form commercially available sinterable alumina (Al 2 O 3 ) powder having an average particle diameter of about 0.1 to 0.5 μm or high purity alumina (Al 2 O 3 ) powder for low temperature sintering. ZrOCl 2 ) is added to the aqueous solution, but the aqueous solution is mixed so that 5 to 20% of zirconia (ZrO 2 ) can be dispersed in a volume ratio.

여기서, 옥시염화지르코늄(ZrOCl2)을 사용하는 것은 미세한 ZrO2의 균일 분산성을 달성하기 위한 것이다.Here, the use of zirconium oxychloride (ZrOCl 2 ) is to achieve uniform dispersibility of fine ZrO 2 .

본 발명에 의하면, 이후의 공정에서 지르코니아(ZrO2)의 안정화를 위해서 지르코니아(ZrO2)에 대해 2 내지 3 몰％의 질산이트륨[Y(NO3)3]을 첨가할 수 있고, 소결을 돕기 위하여 염화알루미늄(AlCl3)도 0 내지 20몰％를 첨가할 수 있다.According to the present invention, 2 to 3 mol% of yttrium nitrate [Y (NO 3 ) 3 ] can be added to zirconia (ZrO 2 ) for stabilization of zirconia (ZrO 2 ) in a subsequent process, and aid in sintering. Aluminum chloride (AlCl 3 ) may also be added in an amount of 0 to 20 mol%.

이어서, 상기 알루미나(Al2O3) 분말이 분산된 옥시염화지르코늄(ZrOCl2) 수용액을 암모니아로 공침 하거나 80 내지 100℃에서 6 내지 10시간 동안 가수분해시켜서 알루미나(Al2O3) 입자 표면에 지르코늄-히드록시드가 부착되도록 한 후 세척 및 건조시킨 다음에 600 내지 900℃에서 하소 및 1400 내지 1600℃ 소결 처리하게 되면 미립의 지르코니아(ZrO2)가 균일하게 분산된 약 99％의 이론 밀도를 갖는 치밀한 알루미나(Al2O3)-지르코니아(ZrO2) 복합체를 제조할 수 있다.Subsequently, an aqueous solution of zirconium oxychloride (ZrOCl 2 ) in which the alumina (Al 2 O 3 ) powder is dispersed is co-precipitated with ammonia or hydrolyzed at 80 to 100 ° C. for 6 to 10 hours to surface the alumina (Al 2 O 3 ) particles. After zirconium-hydroxide is attached, washed and dried, and then calcined at 600 to 900 ° C and sintered at 1400 to 1600 ° C, a theoretical density of about 99% of uniformly dispersed fine zirconia (ZrO 2 ) is obtained. Dense alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composites having the same can be prepared.

본 발명에 따른 방법은 상기에서 언급한 바와 같이, 알루미나(Al2O3)-지르코니아(ZrO2) 복합체를 제조하는데 있어서, 상용의 알루미나(Al2O3) 분말을 옥시염화지르코늄(ZrOCl2) 수용액에 첨가한 후, 침전이나 가수분해시킴으로써 지르코니아(ZrO2)의 침전 생성물이 알루미나(Al2O3) 분말 입자에 균일하게 흡착되어 하소 및 소결 과정에서 지르코니아(ZrO2)의 입자 성장을 더욱 억제할 수 있는 장점이 있다.As mentioned, the process according to the invention in the above, alumina (Al 2 O 3) - zirconia (ZrO 2) in the manufacture of a composite, alumina commercially available (Al 2 O 3) powder, a zirconium oxychloride (ZrOCl2) aqueous solution After addition to the precipitate, the precipitated product of zirconia (ZrO 2 ) is uniformly adsorbed onto the alumina (Al 2 O 3 ) powder particles to further suppress the growth of zirconia (ZrO 2 ) particles during calcination and sintering. There are advantages to it.

이하 본 발명을 실시예에 의거하여 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail with reference to Examples.

실시예 1Example 1

먼저 알루미나(Al2O3)의 출발원료로 이소결성의 상용 알루미나(Al2O3)(평균입경 0.4㎛)를 사용하였다. 미세한 지르코니아(ZrO2)의 균일 분산성을 달성하기 위하여 옥시염화지르코늄(ZrOCl2) 수용액을 사용하였으며, 여기에 부피비로 10％의 지르코니아(ZrO2)가 분산되도록 알루미나(Al2O3) 분말을 혼합하였다.First it was used an alumina (Al 2 O 3) commercially available alumina (Al 2 O 3) of isopropyl formed as the starting material (average particle diameter 0.4㎛) of. In order to achieve uniform dispersibility of fine zirconia (ZrO 2 ), an aqueous solution of zirconium oxychloride (ZrOCl 2 ) was used, whereby alumina (Al 2 O 3 ) powder was dispersed so that 10% of zirconia (ZrO 2 ) was dispersed in a volume ratio. Mixed.

지르코니아(ZrO2)의 안정화를 위하여 지르코니아(ZrO2)에 대해 2몰％의 질산이트륨[Y(NO3)3]을 첨가하였고, 소결을 돕기 위하여 염화알루미늄(AlCl3)을 10몰％ 첨가하였다.Zirconia (ZrO 2) was added in 2 mol% of yttrium nitrate [Y (NO 3) 3] for zirconia (ZrO 2) in order to stabilize, was added aluminum chloride (AlCl 3)% 10 mol to aid in sintering .

이렇게 알루미나(Al2O3) 분말이 분산된 옥시염화지르코늄(ZrOCl2) 수용액을암모니아로 공침 시켜서 알루미나(Al2O3) 입자 표면에 지르코늄히드록시드가 부착되도록 하였다.The zirconium oxychloride (ZrOCl 2 ) aqueous solution in which the alumina (Al 2 O 3 ) powder was dispersed was co-precipitated with ammonia to attach zirconium hydroxide to the surface of the alumina (Al 2 O 3 ) particles.

이를 세척하여 Cl 이온을 제거한 다음 건조한 후 700℃로 하소하고 밀링을 하였다. 이를 과립으로 만든 다음에 성형하여 1550℃에서 소결하여 초미립의 지르코니아(ZrO2)가 균일하게 분산된 99.8％의 이론 밀도를 갖는 치밀한 알루미나(Al2O3)-지르코니아(ZrO2) 복합체를 제조하였다.It was washed to remove Cl ions, dried and calcined at 700 ° C. and milled. The granules were granulated and then sintered at 1550 ° C. to prepare a dense alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite having a theoretical density of 99.8% in which ultrafine zirconia (ZrO 2 ) was uniformly dispersed. It was.

실시예 2Example 2

먼저 알루미나(Al2O3)의 소결온도를 낮추기 위하여 저온 소결용 고순도 알루미나(Al2O3)(평균입경 0.4㎛)를 사용하였다. 미세한 지르코니아(ZrO2)의 균일 분산성을 달성하기 위하여 옥시염화지르코늄(ZrOCl2) 수용액을 사용하였으며, 여기에 부피비로 20％의 지르코니아(ZrO2)가 분산되도록 옥시염화지르코늄(ZrOCl2) 수용액을 혼합하였다.First it was used for low temperature co-fired high-purity alumina (Al 2 O 3) (average particle diameter 0.4㎛) to lower the sintering temperature of alumina (Al 2 O 3). It was used as the fine zirconia (ZrO 2) uniformly minutes zirconium oxychloride (ZrOCl 2) an aqueous solution to achieve the dispersion of, in a volume ratio here a zirconium oxychloride (ZrOCl 2) an aqueous solution so that the dispersion is zirconia (ZrO 2) 20% Mixed.

지르코니아(ZrO2)의 안정화를 위하여 지르코니아(ZrO2)에 대해 3몰％의 질산이트륨[Y(NO3)3]을 첨가하였고, 소결을 돕기 위하여 염화알루미늄(AlCl3)을 20몰％ 첨가하였다.Zirconia (ZrO 2) was added to the 3 mole% yttrium nitrate [Y (NO 3) 3] for zirconia (ZrO 2) in order to stabilize, was added aluminum chloride (AlCl 3)% 20 mol to aid in sintering .

이렇게 알루미나(Al2O3) 분말이 분산된 옥시염화지르코늄(ZrOCl2) 수용액을 90℃에서 8시간 동안 가수분해시켜서 알루미나(Al2O3) 입자 표면에 지르코늄히드록시드가 부착되도록 하였다.The zirconium oxychloride (ZrOCl 2 ) aqueous solution in which the alumina (Al 2 O 3 ) powder was dispersed was hydrolyzed at 90 ° C. for 8 hours to allow zirconium hydroxide to adhere to the surface of the alumina (Al 2 O 3 ) particles.

이를 세척하여 Cl 이온을 제거한 다음 건조한 후 900℃로 하소하고 밀링을 하였다. 이를 과립으로 만든 다음에 성형하여 1450℃에서 소결하여 초미립의 지르코니아(ZrO2)가 균일하게 분산된 99％의 이론 밀도를 갖는 치밀한 알루미나(Al2O3)-지르코니아(ZrO2) 복합체를 제조하였다.It was washed to remove Cl ions, dried and calcined at 900 ° C. and milled. It was formed into granules and then sintered at 1450 ° C. to prepare a dense alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite having a theoretical density of 99% in which ultrafine zirconia (ZrO 2 ) was uniformly dispersed. It was.

본 발명은 알루미나(Al2O3) 세라믹스에 지르코니아(ZrO2) 입자를 균질 하게 분산시켜 그 기계적 강도와 인성을 향상시키려고 한 것으로, 분산되는 지르코니아(ZrO2)의 입자 크기도 작고 균질 하게 분산될 수 있도록 하기 위하여 알루미나(Al2O3)는 상용의 분말을 사용하되 이를 옥시염화지르코늄(ZrOCl2) 수용액에 첨가한 후, 침전이나 가수분해시킴으로써 지르코니아(ZrO2)의 침전 생성물이 알루미나(Al2O3) 분말 입자에 균일하게 흡착되게 하고, 하소 및 소결 과정에서 지르코니아(ZrO2)의 입자 성장을 억제함으로써 최종적으로 얻어지는 알루미나(Al2O3)-지르코니아(ZrO2) 복합체가 99％ 이상의 이론 밀도를 가질 뿐 아니라 기계적 강도와 인성도 향상되는 효과가 있다.The present invention is to homogeneously disperse zirconia (ZrO 2 ) particles in alumina (Al 2 O 3 ) ceramics to improve its mechanical strength and toughness, the particle size of the dispersed zirconia (ZrO 2 ) is also small and homogeneously dispersed. be alumina (Al 2 O 3), after, but using the commercially available in powder added it to the zirconium oxychloride (ZrOCl 2) aqueous solution, the precipitated product of zirconia (ZrO 2) alumina by decomposition precipitation or singer (Al 2 in order that O 3 ) The alumina (Al 2 O 3 ) -zirconia (ZrO 2 ) composite finally obtained by uniformly adsorbing to powder particles and suppressing the growth of zirconia (ZrO 2 ) particles during calcination and sintering process is more than 99% In addition to having a density, the mechanical strength and toughness are also improved.

Claims (4)

알루미나(Al2O3) 상용 분말을 옥시염화지르코늄(ZrOCl2) 수용액에 첨가하되 부피의 비로 5 내지 20％의 지르코니아(ZrO2)가 분산될 수 있도록 상기 수용액을 혼합하고, 이어서, 상기 알루미나(Al2O3) 분말이 분산된 옥시염화지르코늄(ZrOCl2) 수용액을 공침 하거나 가수분해시켜서 알루미나(Al2O3) 입자 표면에 지르코늄-히드록시드가 부착되도록 한 후 하소 및 소결 처리하여서 제조함을 특징으로 하는 알루미나-지르코니아 복합체의 제조 방법.Alumina (Al 2 O 3 ) commercial powder is added to an aqueous solution of zirconium oxychloride (ZrOCl 2 ), but the aqueous solution is mixed so that 5 to 20% of zirconia (ZrO 2 ) can be dispersed in a volume ratio, and then the alumina ( Al 2 O 3 ) Prepared by calcination and sintering after zirconium hydroxide is deposited on the surface of alumina (Al 2 O 3 ) particles by coprecipitation or hydrolysis of zirconium oxychloride (ZrOCl 2 ) solution in which powder is dispersed. Method for producing alumina-zirconia composite, characterized in that. 제 1항에 있어서, 상기 수용액에는 지르코니아(ZrO2)에 대해 2 내지 3몰％의 질산이트륨[Y(NO3)3]과 염화알루미늄(AlCl3)을 0 내지 20몰％ 첨가하여서 됨을 특징으로 하는 알루미나-지르코니아 복합체의 제조 방법.The method of claim 1, wherein the aqueous solution is added by adding 0 to 20 mol% of 2 to 3 mol% of yttrium nitrate [Y (NO 3 ) 3 ] and aluminum chloride (AlCl 3 ) to zirconia (ZrO 2 ). Method of producing an alumina-zirconia composite. 제 1항에 있어서, 상기 공침은 암모니아로 공침을 하고, 상기 가수분해는 80 내지 100℃에서 6 내지 10시간 동안 실시하여서 됨을 특징으로 하는 알루미나-지르코니아 복합체의 제조 방법.The method of claim 1, wherein the coprecipitation is coprecipitation with ammonia, and the hydrolysis is performed at 80 to 100 ° C. for 6 to 10 hours. 제 1항에 있어서, 상기 하소는 600 내지 900℃에서 실시하고, 소결 처리는1400 내지 1600℃에서 실시함을 특징으로 하는 알루미나-지르코니아 복합체의 제조 방법.The method of claim 1, wherein the calcination is performed at 600 to 900 ° C., and the sintering is performed at 1400 to 1600 ° C. 6.
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WO2006080730A1 (en) * 2004-10-08 2006-08-03 Lg Chem, Ltd. Zirconia-alumina nano-composite powder and preparation method thereof
WO2024051651A1 (en) * 2022-09-05 2024-03-14 北京大学口腔医学院 High-strength high-toughness nano zirconium oxide ceramic material, preparation method therefor, and use thereof

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