JP5537827B2 - チタン酸アルミニウム系セラミックスの製造方法およびチタン酸アルミニウム系セラミックス - Google Patents
チタン酸アルミニウム系セラミックスの製造方法およびチタン酸アルミニウム系セラミックス Download PDFInfo
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- JP5537827B2 JP5537827B2 JP2009085012A JP2009085012A JP5537827B2 JP 5537827 B2 JP5537827 B2 JP 5537827B2 JP 2009085012 A JP2009085012 A JP 2009085012A JP 2009085012 A JP2009085012 A JP 2009085012A JP 5537827 B2 JP5537827 B2 JP 5537827B2
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- B01D39/2068—Other inorganic materials, e.g. ceramics
- B01D39/2072—Other inorganic materials, e.g. ceramics the material being particulate or granular
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Description
(チタニウム源粉末)
本発明に用いられるチタニウム源粉末は、チタンを含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、好ましくは酸化チタンの粉末である。酸化チタンとしては、たとえば、酸化チタン(IV)、酸化チタン(III)、酸化チタン(II)などが挙げられるが、なかでも酸化チタン(IV)が好ましく用いられる。酸化チタン(IV)の結晶型としては、アナターゼ型、ルチル型、ブルッカイト型などが挙げられ、不定形(アモルファス)であってもよい。より好ましくは、アナターゼ型またはルチル型の酸化チタン(IV)である。
本発明で用いられるアルミニウム源粉末は、アルミニウムを含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、好ましくはアルミナ(酸化アルミニウム)の粉末である。アルミナの結晶型としては、γ型、δ型、θ型、α型などが挙げられ、不定形(アモルファス)であってもよい。なかでも、α型のアルミナが好ましく用いられる。
本発明において、上記原料混合物は、負の熱膨張材料および/または焼成により負の熱膨張材料に導かれる前駆体混合物を含む。これにより、熱膨張係数が小さい、さらには、熱膨張係数がゼロに近い(すなわち、熱による体積変化が小さい)チタン酸アルミニウム系セラミックスを得ることが可能となる。ここで、負の熱膨張材料とは、加熱したときの熱膨張率が負の値を示す材料を意味する。
上記原料混合物は、マグネシウム源粉末をさらに含有してもよい。この場合、チタン酸アルミニウム系セラミックスとしてチタン酸アルミニウムマグネシウム結晶からなる焼成体を得ることができる。マグネシウム源粉末は、マグネシウムを含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、たとえば、マグネシア(酸化マグネシウム)の粉末のほか、空気中で焼成することによりマグネシアに導かれる化合物の粉末が挙げられ、好ましくはマグネシアである。
上記原料混合物は、ケイ素源粉末をさらに含有していてもよい。ケイ素源粉末は、ケイ素元素を含有し、Si成分としてチタン酸アルミニウム系セラミックスに含まれる化合物の粉末であり、ケイ素源粉末の併用により、耐熱性がより向上されたチタン酸アルミニウム系セラミックスを得ることが可能となる。ケイ素源粉末としては、たとえば、二酸化ケイ素、一酸化ケイ素などの酸化ケイ素の粉末が挙げられる。
本発明の製造方法においては、通常、上記各原料粉末を混合することで原料混合物を得ることができる。混合方法は、乾式雰囲気にて混合を行なう方法(乾式混合法)、湿式雰囲気で混合を行なう方法(湿式混合法)のいずれを用いてもよい。
乾式雰囲気で混合する場合は、たとえば、上記の各原料粉末を混合し、液体媒体中に分散させることなく、粉砕容器内で撹拌すればよく、粉砕メディアの共存下に粉砕容器内で撹拌することによって原料粉末の粉砕を同時に行なってもよい。
原料粉末を乾式にて粉砕するにあたっては、粉砕助剤、解膠剤などの添加剤を加えてもよい。粉砕助剤としては、たとえば、メタノール、エタノール、プロパノールなどのアルコール類;プロピレングリコール、ポリプロピレングリコール、エチレングリコールなどのグリコール類;トリエタノールアミンなどのアミン類;パルチミン酸、ステアリン酸、オレイン酸などの高級脂肪酸類;カーボンブラック、グラファイトなどの炭素材料などが挙げられる。これらはそれぞれ単独または2種以上を組み合わせて用いられる。
湿式雰囲気で混合する場合は、たとえば、ケイ素源粉末等の原料粉末を溶媒中に分散させた状態で他の原料粉末と混合すればよく、通常は、ケイ素源粉末が溶媒に分散された状態で他の原料粉末と混合される。その際、溶媒として、通常は水が用いられ、不純物が少ない点で、イオン交換水が好適に用いられる。溶媒の使用量は、原料粉末の合計量100質量部に対して、通常、20〜1000質量部であり、好ましくは30〜300質量部である。
本発明の製造方法においては、上述のようにして得られた粉末状の原料混合物を焼成することにより、チタン酸アルミニウム系セラミックスを得る。焼成にあたっては、原料混合物を所望の形状に成形した後、焼成を行なってもよく、あるいは、粉末状の原料混合物のまま焼成を行なってもよい。後者の場合、焼成により得られた焼成物を、必要に応じて解砕した後、所望の形状に成形し、成形体を得てもよい。また、粉末状の原料混合物を焼成することにより成形体を得た後、該成形体をさらに焼成してもよい。
原料混合物の焼成前における成形または焼成により得られた焼成物(チタン酸アルミニウム系セラミックス)の成形には、通常用いられる成形方法を用いることができ、一軸成形や押し出し成形などが用いられる。成形に用いる成形機としては、一軸プレス、押出成形機、打錠機、造粒機などが挙げられる。
チタン酸アルミニウム化率(AT化率)は、粉末X線回折スペクトルにおける2θ=27.4°の位置に現れるピーク〔チタニア・ルチル相(110)面〕の積分強度(IT)と、2θ=33.7°の位置に現れるピーク〔チタン酸アルミニウムマグネシウム相(230)面〕の積分強度(IAT)とから、下記式:
AT化率=IAT/(IT+IAT)×100(%)
により算出した。
チタン酸アルミニウム系セラミックス成形体を治具の上に固定用樹脂で固定し、長さ13mm、幅4mm、厚さ4mmの直方体形状に切り出した。ついで、切り出された焼成体を、200℃/hで600℃まで昇温して熱処理を行ない、切り出し作業に用いた固定用樹脂を消失させた。熱処理を施した試験片について、熱機械的分析装置(SIIテクノロジー(株)製 TMA6300)を用いて、室温(25℃)から1000℃まで600℃/hで昇温させた際の試験片の膨張率から、下記式に基づき、熱膨張係数〔K-1〕を算出した。
熱膨張係数〔K-1〕=試験片の膨張率/975〔K〕
ここで、試験片の膨張率とは、
(1000℃まで昇温させたときの試験片の長さ−昇温前(25℃)における試験片の長さ)/(昇温前(25℃)における試験片の長さ)
を意味する。
体積基準の累積百分率50%相当粒子径(D50)および体積基準の累積百分率90%相当粒子径(D90)は、レーザ回折式粒度分布測定装置〔日機装社製「Microtrac HRA(X−100)」〕を用いて測定した。
原料粉末として以下のものを用いた。
酸化チタン(IV)(チタニア)粉末(デュポン(株)製「R−900」、ルチル型結晶、D50:0.49μm、D90:0.63μm)
24.8g(54.0質量部)
(2)アルミニウム源粉末
αアルミナ粉末(BET比表面積:0.6g/cm2、D50:40.2μm、D90:70.2μm)
21.1g(46.0質量部)
(3)マグネシウム源粉末
マグネシア粉末(宇部マテリアル(株)製「UC−95M」、D50:3.47μm、D90:4.76μm)
2.1g(4.6質量部)
(4)ケイ素源粉末
ガラスフリット(タカラスタンダード(株)製「CK−0832M2」、D50:6.0μm、D90:18.4μm)
1.0g(2.2質量部)
(5)負の熱膨張材料
タングステン酸ジルコニウム粉末(和光純薬社製、D50:0.94μm、D90:3.18μm)
1.0g
チタニア〔TiO2〕換算のチタニウム源粉末およびアルミナ〔Al2O3〕換算のアルミニウム源粉末の合計量100質量部に対するタングステン酸ジルコニウム粉末の使用量は、2.2質量部である。
ガラスフリットの使用量を2.0gに変更し、タングステン酸ジルコニウム粉末を用いなかったこと以外は、実施例1と同様にしてチタン酸アルミニウム系セラミックス焼成体を得た。得られたチタン酸アルミニウム系セラミックスは、組成式:Al2(1−x)MgxTi(1+x)O5で表され、xの値は約0.23である。
Claims (9)
- チタニウム源粉末と、アルミニウム源粉末と、タングステン酸ジルコニウムおよび/または焼成によりタングステン酸ジルコニウムに導かれる前駆体混合物とを含む原料混合物を焼成する工程を備え、
前記原料混合物は、チタニア換算のチタニウム源粉末およびアルミナ換算のアルミニウム源粉末の合計量100質量部に対して、タングステン酸ジルコニウム換算で、0.5〜5質量部のタングステン酸ジルコニウムおよび/または焼成によりタングステン酸ジルコニウムに導かれる前駆体混合物を含む、チタン酸アルミニウム系セラミックスの製造方法。 - 前記原料混合物は、マグネシウム源粉末をさらに含む、請求項1に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 前記原料混合物は、チタニア換算のチタニウム源粉末およびアルミナ換算のアルミニウム源粉末の合計量100質量部に対して、マグネシア換算で、0.1〜10質量部のマグネシウム源粉末を含む、請求項2に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 前記原料混合物は、ケイ素源粉末をさらに含む、請求項1〜3のいずれか一項に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 前記ケイ素源粉末は、ガラスフリットである、請求項4に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 前記原料混合物は、チタニア換算のチタニウム源粉末およびアルミナ換算のアルミニウム源粉末の合計量100質量部中、チタニア換算で、30〜70質量部のチタニウム源粉末を含み、
チタニア換算のチタニウム源粉末およびアルミナ換算のアルミニウム源粉末の合計量100質量部に対して、シリカ換算で、0.1〜20質量部のケイ素源粉末を含む、請求項4または5に記載のチタン酸アルミニウム系セラミックスの製造方法。 - 前記焼成の温度は、1300〜1650℃の範囲内である、請求項1〜6のいずれか一項に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 前記原料混合物の焼成により得られた焼成物を解砕する工程をさらに含む、請求項1〜7のいずれか一項に記載のチタン酸アルミニウム系セラミックスの製造方法。
- 請求項1〜8のいずれか一項に記載の製造方法により得られるチタン酸アルミニウム系セラミックス。
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