KR19980014400A - Process for producing aluminum titanate raw material granules and ceramics - Google Patents

Process for producing aluminum titanate raw material granules and ceramics Download PDF

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KR19980014400A
KR19980014400A KR1019960033363A KR19960033363A KR19980014400A KR 19980014400 A KR19980014400 A KR 19980014400A KR 1019960033363 A KR1019960033363 A KR 1019960033363A KR 19960033363 A KR19960033363 A KR 19960033363A KR 19980014400 A KR19980014400 A KR 19980014400A
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ceramics
aluminum titanate
raw material
tio
material granules
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KR1019960033363A
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KR0169573B1 (en
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김원배
이종일
태범석
전용진
장현태
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김원배
인성파우더테크 주식회사
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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 특성변화가 일어나지 않도록 Mg, Zr, Si 및 Ba 등의 첨가제를 첨가하여 원료과립 및 세라믹스를 제조하는 것이다.The present invention aims to economically develop ceramics having a high thermal shock resistance and is characterized in that the properties of aluminum titanate ceramics having a low thermal expansion coefficient are such that additives such as Mg, Zr, Si and Ba, To produce 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, 용융 금속의 Filter용 등으로 이용의 폭을 넓혀나갈 수 있다.Al 2 O 3 , TiO 2 and various additives are mixed in consideration of economical efficiency along with the improvement of the characteristics, so that the particle size is kept at 0.3 μm or less so that the aluminum titanate ceramics can be produced by only one firing. Since the phase decomposition does not occur even after long use at high temperature, it can be widely used for high temperature structural materials, catalyst carriers, and filters for molten metals.

Description

알루미늄 티타네이트 원료과립 및 세라믹스의 제조방법Process for producing aluminum titanate raw material granules and ceramics

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

알루미늄 티타네이트를 제조하는 방법으로 고상반응법, Sol-Gel법, 알콕사이드법 및 CVD법 등이 알려져 있으며 이 반응들을 혼용하는 방법들도 있다. 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 Grain이나 Micro-crack의 성장을 방해하여 Al2TiO5의 분해를 방지한다.Solid phase reaction, sol-gel method, alkoxide method, and CVD method are known as methods for producing aluminum titanate, and there are methods in which these reactions are mixed. On the other hand, aluminum titanate itself is easily decomposed at high temperature and separated into Al 2 O 3 and TiO 2 phases. Therefore, MgO, Fe 2 O 3 , Cr 2 O 3 , SiO 2 , ZrO 2 , Al 2 O 3 . They prevent the decomposition of Al 2 TiO 5 by forming a solid solution with Al 2 TiO 5 or interfering with the growth of grains or micro-cracks.

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:0.1㎛)와 MgCO3및 BaCO3를 사용하였다.In the present invention, Al 2 TiO 5 was separately synthesized and used as raw material, and ultrafine powder-unmodified Al 2 O 3 (average particle diameter: 0.3 μm) and TiO 2 pigment (average particle diameter: 0.1 μm) Zirconium silicate (average particle size: 0.1 탆) and MgCO 3 and BaCO 3 were used.

따라서 본 발명으로 제조한 알루미늄 티타네이트 세라믹스는 열적특성 뿐만 아니라, 기계적 특성도 우수하며 매우 경제적인 알루미늄 티타네이트 세라믹스이다.Therefore, the aluminum titanate ceramics produced by the present invention are aluminum titanate ceramics which are excellent in not only thermal properties but also mechanical properties and are very economical.

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

알루미나(Al2O3)와 티타니아(TiO2)의 몰비(Al2O3/TiO5)가 1.0~1.2이 되도록 Al2O3와 TiO2를 취하고, 둘을 합한 양에 대하여 중량비로 2~3%의 MgO가 되도록 MgCO3를 취하고, 또한 3~8%가 되도록 지르코늄 실리케이트를 취하여 1~2%의 BaO가 되도록 취해진 BaCO3와 함께 모두 혼합하여 슬러리를 만들고 Attrition-type Mill에서 ø1mm의 지르코니아 비드를 사용하여 평균입경이 0.3㎛ 이하가 되도록 3시간 동안 충분히 분쇄혼합 한다.Al 2 O 3 and TiO 2 are taken such that the molar ratio (Al 2 O 3 / TiO 5 ) of alumina (Al 2 O 3 ) and titania (TiO 2 ) is 1.0 to 1.2, MgCO 3 is taken to be 3% MgO, zirconium silicate is taken to be 3 to 8% and mixed with BaCO 3 , which is taken to be 1 to 2% BaO, to make a slurry, and zirconia beads of ø1 mm in Attrition- Is sufficiently pulverized and mixed for 3 hours so that the average particle diameter becomes 0.3 탆 or less.

분쇄가 완료된 슬러리에 유기 바인더를 고형분 대비 2중량 퍼센트, 유기 윤활제를 고형분 대비 1.5중량 퍼센트 첨가하여 다시 30분 동안 Attrition-type Mill에서 충분히 혼합한다.Add 2 wt% of organic binder and 1.5 wt% of organic lubricant to the pulverized slurry and mix thoroughly in Attrition-type Mill for 30 min.

위와 같이 제조된 슬러리의 고형분 농도는 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 slurry thus prepared was adjusted to have a solid content of 50% and then dried in a spray drier to form a granular aluminum titanate raw material. The granules were molded into a press and were heated at a temperature of 1450 ° C to 1600 ° C To produce high strength and 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 매우 간단한 공정으로 저렴한 원료를 공급할 수 있다는 것이다.An advantage of the present invention is that it is possible to produce aluminum titanate raw material granules by using a spray drier by making Al 2 O 3 , TiO 2 and additives separately in the form of slurry without separately synthesizing Al 2 TiO 5 , The process can supply low-cost raw materials.

본 발명의 특징은 다음과 같다.The 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 the main chain, and dried to form the granules for press molding.

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

③ 상기 혼합물들을 분쇄하여 평균 입경을 0.3㎛ 이하로 조절하므로서 반응이 쉽게 일어나도록 조절한다.(3) The mixture is pulverized to adjust the average particle size to 0.3 탆 or less so that the reaction easily occurs.

아래의 실시예 및 비교 실시예의 조성과 이를 1550℃에서 2시간 동안 소성하였을 경우에 XRD 분석에 의한 주 Phase와 이를 1000℃에서 2시간 동안 열처리 한 후 XRD분석에 의한 주 Phase를 나타내었다. 표에서 보면 알 수 있듯이 본 발명에서 제조된 방법으로는 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 calcined at 1550 ° C. for 2 hours and the main phase by XRD analysis after heat treatment at 1000 ° C. for 2 hours are shown. As can be seen from the table, since the thermal decomposition does not occur in the method of the present invention, the aluminum titanate produced by the present invention has excellent thermal stability and high temperature characteristics.

Claims (2)

알루미늄 티타네이트 과립 및 세라믹스 제조시 첨가제로서 Al2O3와 TiO2에 더해 MgCO3, ZrSiO4및 BaCO3를 사용하는 방법Method of using MgCO 3 , ZrSiO 4 and BaCO 3 in addition to Al 2 O 3 and TiO 2 as additives in the production of aluminum titanate granules and ceramics 상기 혼합물들을 평균입경이 0.3㎛ 이하가 되도록 분쇄하여 슬러리를 만든 후 과립을 제조하는 방법.The mixture is pulverized to have an average particle diameter of 0.3 탆 or less to prepare a slurry, and granules are produced.
KR1019960033363A 1996-08-12 1996-08-12 Aluminum titanate ceramic sintered body and its manufacturing KR0169573B1 (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6924998B2 (en) 2003-09-08 2005-08-02 Hynix Semiconductor Inc. FeRAM using programmable register
US6967897B2 (en) 2003-12-04 2005-11-22 Hynix Semiconductor Inc. FeRAM having wide page buffering function
US7009907B2 (en) 2003-12-23 2006-03-07 Hynix Semiconductor Inc. FeRAM having sensing voltage control function
US7075845B2 (en) 2003-12-04 2006-07-11 Hynix Semiconductor Inc. FeRAM and sense amplifier array having data bus pull-down sensing function and sensing method using the same
US7081779B2 (en) 2003-05-30 2006-07-25 Hynix Semiconductor Inc. Reset signal generating circuit
US7382641B2 (en) 2003-12-26 2008-06-03 Hynix Semiconductor Inc. FeRAM for high speed sensing

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100335393B1 (en) * 2000-02-09 2002-05-06 한상목 the processing method of infrared radiator using composites of aluminum titanate and clay

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7081779B2 (en) 2003-05-30 2006-07-25 Hynix Semiconductor Inc. Reset signal generating circuit
US6924998B2 (en) 2003-09-08 2005-08-02 Hynix Semiconductor Inc. FeRAM using programmable register
US6967897B2 (en) 2003-12-04 2005-11-22 Hynix Semiconductor Inc. FeRAM having wide page buffering function
US7075845B2 (en) 2003-12-04 2006-07-11 Hynix Semiconductor Inc. FeRAM and sense amplifier array having data bus pull-down sensing function and sensing method using the same
US7009907B2 (en) 2003-12-23 2006-03-07 Hynix Semiconductor Inc. FeRAM having sensing voltage control function
US7382641B2 (en) 2003-12-26 2008-06-03 Hynix Semiconductor Inc. FeRAM for high speed sensing

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