KR0169573B1 - Aluminum titanate ceramic sintered body and its manufacturing - Google Patents

Aluminum titanate ceramic sintered body and its manufacturing Download PDF

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KR0169573B1
KR0169573B1 KR1019960033363A KR19960033363A KR0169573B1 KR 0169573 B1 KR0169573 B1 KR 0169573B1 KR 1019960033363 A KR1019960033363 A KR 1019960033363A KR 19960033363 A KR19960033363 A KR 19960033363A KR 0169573 B1 KR0169573 B1 KR 0169573B1
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aluminum titanate
ceramics
tio
high temperature
manufacturing
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KR19980014400A (en
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김원배
이종일
태범석
전용진
장현태
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김원배
인성파우더테크주식회사
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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
    • C04B35/46—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 titanium oxides or titanates
    • C04B35/462—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 titanium oxides or titanates based on titanates
    • C04B35/478—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 titanium oxides or titanates based on titanates based on aluminium titanates
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62695—Granulation or pelletising
    • 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
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
    • 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
    • C04B2235/32—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
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof

Abstract

본 발명은 내열 충격성이 높은 세라믹스를 경제적으로 개발하고자 하는 것으로 열팽창 계수가 낮은 알루미늄 티타네이트 세라믹스의 특성에 고온에서 반복 사용할 때에도 상변화에 의한 특성 변화가 일어나지 않도록 Mg, Zr, Si 및 Ba 등의 첨가제를 첨가하여 원료과립 및 세라믹스를 제조하는 것이다.The present invention aims to economically develop ceramics having high thermal shock resistance, so that additives such as Mg, Zr, Si, and Ba do not occur even when repeated use at high temperatures for the properties of aluminum titanate ceramics having a low thermal expansion coefficient. To add the raw material granules and ceramics.

상기 특성 향상과 함께 경제성을 고려하여 Al2O3, TiO2및 각종 첨가제들을 혼합하여 단 한차례의 소성으로 알루미늄 티타네이트 세라믹스가 생성될 수 있도록 입자크기를 0.3㎛이하로 유지하도록 하는 것이다. 고온에서 오랜 시간 사용 후에도 상분해가 일어나지 않으므로 고온용구조재, 촉매담체, 용융금속의 Filter용 등으로 이용의 폭을 넓혀나갈 수 있다.In consideration of economics as well as the above properties, Al 2 O 3 , TiO 2, and various additives are mixed to maintain particle sizes of 0.3 μm or less so that aluminum titanate ceramics can be produced by only one firing. Phase decomposition does not occur even after long time use at high temperature, so it can be used for high temperature structural material, catalyst carrier, filter of molten metal, etc.

Description

알루미늄 티타네이트 원료과립 및 세라믹스 제조방법Aluminum Titanate Raw Granules and Ceramics Manufacturing Method

알루미늄 티타네이트는 낮은 열팽창 특성으로 인한 고온 안정성을 바탕으로 고온용 구조 재료, 촉매 담체, 용융금속의 Filter용 등으로 이용의 폭이 넓어지고 있다.Aluminum titanate has been widely used for high temperature structural materials, catalyst carriers, and molten metal filters based on high temperature stability due to low thermal expansion properties.

알루미늄 티타네이트 원료 분말을 제조하는 방법으로는 고상반응법, Sol-Gel법, 알콕사이드법 및 CVD법 등이 알려져 있으며 이 반응들을 혼용하는 방법들도 있다. 이들 방법으로 제조된 알루미늄 티타네이트 분말을 기존의 세라믹스 제조방법에 의해 성형 및 소결하여 최종제품을 만들게 된다. 한편 알루미늄 티타네이트는 자체로서는 고온에서 쉽게 분해되어 Al2O3와 TiO2상으로 분리되기 때문에 이를 방지하기 위하여 MgO, Fe2O3, Cr2O3, SiO2, ZrO2, Al2O3등을 첨가한다. 이들은 Al2TiO5와 고용체를 형성하거나 Grain 이나 Micro-crack 의 성장을 방해하여 Al2TiO5의 분해를 방지한다.As a method for producing an aluminum titanate raw material powder, a solid phase reaction method, a Sol-Gel method, an alkoxide method, and a CVD method are known, and there are also methods in which these reactions are mixed. The aluminum titanate powder produced by these methods is molded and sintered by the conventional ceramics manufacturing method to produce the final product. On the other hand, aluminum titanate is easily decomposed at high temperature and separated into Al 2 O 3 and TiO 2 phases. Therefore, in order to prevent it, MgO, Fe 2 O 3 , Cr 2 O 3 , SiO 2 , ZrO 2 , Al 2 O 3 Etc. are added. They form a solid solution with Al 2 TiO 5 or prevent the growth of Al 2 TiO 5 by inhibiting grain or micro-crack growth.

본 발명에서는 Al2TiO5를 별도로 합성하여 원료로 사용하지 않고 초미분 이소결성 Al2O3(평균입경: 0.3㎛)와 안료용 TiO2(평균입경: 0.1㎛)를 원료로 사용하였으며 첨가제로는 지르코늄 실리케이트(평균입경: 1.0㎛)와 MgCO3및 BaCO3를 사용하였다. 특히 BaO 성분을 첨가하므로서 알루미늄 티타네이트의 생성 및 열분해 방지효과가 우수하였다.In the present invention, instead of separately synthesizing Al 2 TiO 5 as a raw material, ultrafine sintered Al 2 O 3 (average particle diameter: 0.3 μm) and pigment TiO 2 (average particle size: 0.1 μm) were used as raw materials. Zirconium silicate (average particle size: 1.0㎛) and MgCO 3 and BaCO 3 were used. In particular, the addition of BaO component was excellent in the production and prevention of thermal decomposition of aluminum titanate.

본 발명으로 제조한 알루미늄 티타네이트 세라믹스는 열적 특성 뿐만 아니라, 기계적 특성도 우수하며 최종제품의 제조시 기존의 원료 분말을 합성한 후 세라믹스 제품 제조 공정을 필요로 하는 2단계 작업 공정을 거칠 필요없이 기본원료로부터 1단계 공정으로 제품의 제조가 가능하므로 매우 경제적인 알루미늄 티타네이트 세라믹스이다.The aluminum titanate ceramics manufactured by the present invention have excellent thermal properties as well as mechanical properties, and do not need to go through a two-step work process that requires the production of ceramic products after synthesizing the existing raw material powder in the manufacture of the final product. It is very economical aluminum titanate ceramics because it can manufacture products from raw materials in one step process.

본 발명의 상세한 내용은 다음과 같다.Details of the present invention are as follows.

알루미나(Al2O3)와 티타니아(TiO2)의 몰비(Al2O3/TiO2)가 1.0~1.2이 되도록 Al2O3와 TiO2를 취하고, 둘을 합한 양에 대하여 중량비로 2~3%의 MgO 가 되도록 MgCO3를 취하고, 또한 3~8%가 되도록 지르코늄 실리케이트를 취하여 1~2%의 BaO 가 되도록 취해진 BaCO3와 함께 모두 혼합하여 슬러리를 만들고 Attrition-type Mill에서 ø1㎜의 지르코니아 비드를 사용하여 평균입경이 0.3㎛이하가 되도록 3시간 동안 충분히 분쇄혼합한다.Al 2 O 3 and TiO 2 are taken so that the molar ratio (Al 2 O 3 / TiO 2 ) of alumina (Al 2 O 3 ) to titania (TiO 2 ) is 1.0 to 1.2, and 2 to 3 by weight based on the combined amount. Take MgCO 3 to 3% MgO, and also take zirconium silicate to 3-8%, mix all together with BaCO 3 taken to 1 ~ 2% BaO to make slurry and ø1mm zirconia in Attrition-type Mill Using the beads, the mixture is ground and mixed sufficiently for 3 hours so that the average particle diameter is 0.3 탆 or less.

분쇄가 완료된 슬러리에 PVA나 MC 등의 유기 바인더를 고형분 대비 2중량 퍼센트, 유기윤활제로서 스테아린산 에멀젼을 고형분 대비 1.5중량 펴센트 첨가하여 다시 30분 동안 Attrition-type Mill에서 충분히 혼합한다.To the slurry, the pulverized slurry is added 2 wt.% Of organic binders such as PVA and MC, and 1.5 wt.% Of stearic acid emulsion is used as an organic lubricant, and mixed in the Attrition-type Mill for 30 minutes.

위와 같이 제조된 슬러리의 고형분 농도는 약 50%가 되도록 수분의 양을 조절한 후 스프레이 드라이어에서 건조하여 과립상태의 알루미늄 티타네이트 원료를 만들었으며, 이 과립을 프레스로 성형하고 이를 1450℃~1600℃ 사이에서 소성하여 고강도 저팽창성 알루미늄 티타네이트 세라믹스를 제조할 수 있었다.The solid content of the slurry prepared as described above was adjusted to an amount of about 50%, and then dried in a spray dryer to produce a granular aluminum titanate raw material. Firing in between could produce high strength low-expansion aluminum titanate ceramics.

본 발명의 장점은 Al2TiO5를 별도로 합성하지 않고 각각의 Al2O3, TiO2및 첨가물들을 동시에 첨가하여 슬러리 상태로 만들어 스프레이 드라이어를 사용하여 알루미늄 티타네이트 원료 과립을 제조할 수 있으므로 기존의 2단계 공정에 비해 1 단계 공정으로 저렴한 원료를 공급할 수 있다는 것이다.The advantage of the present invention is that the aluminum titanate raw material granules can be prepared using a spray dryer by adding Al 2 O 3 , TiO 2 and additives simultaneously to make a slurry without synthesizing Al 2 TiO 5 separately. Compared to the two-step process, it is possible to supply cheaper raw materials in one step.

본 발명의 특징은 다음과 같다.Features of the present invention are as follows.

① Al2O3, TiO2및 첨가물들을 동시에 첨가하여 본쇄 혼합하고 건조하여 프레스 성형용 과립을 만들 수 있다.① Al 2 O 3 , TiO 2 and additives can be added at the same time, mixed with chain and dried to make granules for press molding.

② 첨가물로서 MgCO3, BaCO3, 그리고 ZrSiO4를 사용한다.② MgCO 3 , BaCO 3 , and ZrSiO 4 are used as additives.

③ 상기 혼합물들을 분쇄하여 평균 입경을 0.3㎛ 이하로 조절하므로서 반응성을 높여 소결온도를 낮추고 소결시간을 줄일 수 있다. BaCO3를 첨가하고 평균 입경을 0.3㎛ 이하로 조절하므로서 기존방법의 단점이었던 Al2TiO5를 먼저 합성하지 않고도 1단계로 알루미늄 티타네이트 세라믹스 합성이 가능하며, 최종 알루미늄 티타네이트의 열분해 방지효과도 우수하였다.③ By grinding the mixture to adjust the average particle diameter to 0.3㎛ or less by increasing the reactivity can lower the sintering temperature and reduce the sintering time. By adding BaCO 3 and adjusting the average particle size to 0.3㎛ or less, it is possible to synthesize aluminum titanate ceramics in one step without first synthesizing Al 2 TiO 5 , which was a disadvantage of the existing method, and also excellent in preventing thermal decomposition of final aluminum titanate. It was.

아래의 실시예 및 비교 실시예의 조성과 이를 1550℃에서 2시간 동안 소성하였을 경우에 XRD 분석에 의한 주 Phase 와 이를 1000℃에서 2시간 동안 열처리 한 후의 XRD 분석에 의한 주 Phase를 나타내었다. 표에서 보면 알 수 있듯이 본 발명에서 제조된 알루미늄 티타네이트는 열분해가 일어나지 않으므로 본 발명으로 제조된 알루미늄 티타네이트의 열안정성 및 고온 특성이 우수하다.The composition of the following Examples and Comparative Examples and the main phase by XRD analysis when firing at 1550 ℃ for 2 hours and the main phase by XRD analysis after heat treatment at 1000 ℃ for 2 hours are shown. As can be seen from the table, the aluminum titanate prepared in the present invention is excellent in thermal stability and high temperature characteristics of the aluminum titanate prepared in the present invention because no pyrolysis occurs.

Claims (2)

알루미늄 티타네이트 과립 및 세라믹스 제조시 Al2O3와 TiO2를 합한 양에 대해 첨가제로서 중량비로 2~3%의 MgO 가 되도록 MgCO3, 3~8%가 되도록 ZrSiO4, 1~2%의 BaO가 되도록 BaCO3를 사용하는 방법.For the production of aluminum titanate granules and ceramics, ZrSiO 4 , 1 ~ 2% BaO to MgCO 3 , 3 ~ 8% to make MgO of 2 ~ 3% by weight as an additive to the combined amount of Al 2 O 3 and TiO 2 To use BaCO 3 . 제1항에 있어서, 제조된 혼합물들의 평균입경이 0.3㎛ 이하가 되도록 분쇄하여 슬러리를 만든 후 PVA나 MC 등의 유기바인더와 스테아린산 에멀젼 등의 유기윤활제를 혼합하여 세라믹스 제조용 과립을 제조하는 방법.The method of claim 1, wherein the mixture is pulverized to have an average particle diameter of 0.3 μm or less, to form a slurry, and then an organic binder such as PVA or MC is mixed with an organic lubricant such as stearic acid emulsion to prepare granules for ceramics manufacture.
KR1019960033363A 1996-08-12 1996-08-12 Aluminum titanate ceramic sintered body and its manufacturing KR0169573B1 (en)

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KR100335393B1 (en) * 2000-02-09 2002-05-06 한상목 the processing method of infrared radiator using composites of aluminum titanate and clay

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