JP5502135B2 - チタン酸アルミニウム系セラミックスの製造方法 - Google Patents
チタン酸アルミニウム系セラミックスの製造方法 Download PDFInfo
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Description
バインダーとしては、例えばメチルセルロース、カルボキシルメチルセルロース、ナトリウムカルボキシルメチルセルロースなどのセルロース類、ポリビニルアルコールなどのアルコール類、リグニンスルホン酸塩などの塩、パラフィンワックス、マイクロクリスタリンワックスなどのワックス、EVA、ポリエチレン、ポリスチレン、液晶ポリマー、エンジニアリングプラスチックなどの熱可塑性樹脂などが挙げられる。なお、物質によっては造孔剤とバインダーの両方の役割を兼ねるものも存在する。成形時は粒子同士を接着して成形体を保形させることができ、その後の焼成時にそれ自身が燃焼して空孔を形成させることができる物質が該当し、具体的にはポリエチレンなどを挙げることができる。
AT化率(%)=100×IAT/(IAT +IT)・・・(1)
微粒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を解砕し、目開き33μmの篩を通過させて、最大粒子径33μm、中心粒子径(D50)16.3μm、累積百分率90%相当粒子径(D90)29.1μmのチタン酸アルミニウムマグネシウム粉末〔組成はTiO239質量%、Al2O356質量%、MgO1.4質量%〕5gを得た。このチタン酸アルミニウムマグネシウム粉末を、酸化チタン(IV)粉末〔デュポン(株)、「R−900」〕17.6g、αアルミナ粉末〔住友化学(株)製、「AES−12」〕24.3g、炭酸マグネシウム粉末〔神島化学(株)、「金星」〕1.4g、粉末状長石〔特殊精礦(株)より入手した大平長石、型番「SS−300」、SiO2換算のシリコン含有量は67.1質量%、Al2O3換算のアルミニウム含有量は18.1質量%〕1.6gおよびアルミナビーズ〔直径15mm〕5kgと共にアルミナ製粉砕容器〔内容積3.3L〕に投入した。これら微粒チタン酸アルミニウムマグネシウム、酸化チタン粉末、αアルミナ粉末および長石の混合物の合計容積は約50cm3であった。その後、粉砕容器を振動ミルにより振幅5.4mm、振動数1760回/分、動力5.4kWにて2分間振動させることにより粉砕容器内の混合物を粉砕しながら混合し、前駆体混合物を得た。
微粒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を解砕し、目開き33μmの篩を通過させて、最大粒子径33μm、中心粒子径(D50)16.3μm、累積百分率90%相当粒子径(D90)29.1μmのチタン酸アルミニウム粉末〔組成はTiO239質量%、Al2O356質量%、MgO1.4質量%〕2000gを得た。この微粒チタン酸アルミニウム系セラミックスを、酸化チタン粉末〔デュポン(株)、「R−900」〕3193g、αアルミナ粉末〔一次粒子径4μm、二次粒子径80μm〕4393g、マグネシア粉末〔宇部マテリアル(株)、「UC−95M」〕124gおよび粉末状長石〔特殊精礦(株)より入手した大平長石、型番「SS−300」〕291gを、アルミナビーズ〔直径15mm〕80kgと共にアルミナ製粉砕容器〔内容積50L〕に投入した。これら酸化チタン粉末、αアルミナ粉末および長石の混合物の合計容積は約10000cm3であった。その後、容器を振動ミルにより振幅10mm、振動数1200回/分、動力5.5kWにて30分間振動させることにより粉砕容器内の混合物を粉砕し、前駆体混合物を得た。この前駆体混合物のうち5gをアルミナ製ルツボに入れ、大気中、箱型電気炉により昇温速度300℃/時間で1500℃まで昇温し、同温度を4時間保持することにより焼成した。その後、室温まで放冷して、焼成物を得た。得られた焼成物のBET比表面積は0.29m2/gであった。この焼成物を解砕してチタン酸アルミニウム粉末を得た。得られたチタン酸アルミニウム粉末の細孔容量の値は2.9×10−3cm3/gであった。前記粉末のX線回折スペクトルを得たところ、チタン酸アルミニウムマグネシウムの結晶ピークを示した。
酸化チタン粉末〔デュポン(株)、「R−900」〕3991g、αアルミナ粉末〔一次粒子径4μm、二次粒子径80μm〕5491g、マグネシア粉末〔宇部マテリアル(株)、「UC−95M」〕154gおよび粉末状長石〔特殊精礦(株)より入手した大平長石、型番「SS−300」〕364gを、アルミナビーズ〔直径15mm〕80kgと共にアルミナ製粉砕容器〔内容積50L〕に投入した。これら酸化チタン粉末、αアルミナ粉末および長石の混合物の合計容積は約10000cm3であった。その後、容器を振動ミルにより振幅10mm、振動数1200回/分、動力5.5kWにて30分間振動させることにより粉砕容器内の混合物を粉砕し、前駆体混合物を得た。この前駆体混合物のうち5gをアルミナ製ルツボに入れ、大気中、箱型電気炉により昇温速度300℃/時間で1500℃まで昇温し、同温度を4時間保持することにより焼成した。その後、室温まで放冷して、焼成物を得た。得られた焼成物のBET比表面積は0.38m2/gであった。この焼成物を解砕してチタン酸アルミニウム粉末を得た。得られたチタン酸アルミニウム粉末の細孔容量の値は3.3×10−3cm3/gであった。粉末X線回折法により、前記粉末のX線回折スペクトルを得たところ、チタン酸アルミニウムマグネシウムの結晶ピークを示した。
Claims (9)
- チタン酸アルミニウム系セラミックス粉末をチタニア源(チタニウムアルコキシドを除く)、アルミナ源(アルミニウムアルコキシドを除く)、マグネシア源およびシリカ源と混合して前駆体混合物を得、得られた前記前駆体混合物を焼成することを特徴とするチタン酸アルミニウム系セラミックスの製造方法。
- 前記焼成の前に、さらに前記前駆体混合物を成形することを特徴とする請求項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。
- 前記チタニア源のチタニア換算での使用量、前記アルミナ源のアルミナ換算での使用量および前記マグネシア源のマグネシア換算での使用量の合計量100質量部あたり、前記チタニア源のチタニア換算での使用量が20質量部〜60質量部、前記アルミナ源のアルミナ換算での使用量が30質量部〜70質量部、前記マグネシア源のマグネシア換算での使用量が0.1質量部〜10質量部、および前記シリカ源のシリカ換算での使用量が、通常0.1質量部〜20質量部である請求項1または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。
- 前記シリカ源が、ガラスフリットである請求項1〜3のいずれか1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。
- 前駆体混合物を、1400℃〜1550℃での温度で焼成する請求項1〜4のいずれか1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。
- 前記前駆体混合物を得る前に、
原料混合物を焼成し、第1のチタン酸アルミニウム系セラミックスを得る工程、及び
前記第1のチタン酸アルミニウム系セラミックスを解砕、及び分級して最大粒径が40μm以下である前記チタン酸アルミニウム系セラミックス粉末を得る工程、
を備える請求項1〜5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。 - 前記チタン酸アルミニウム系セラミックス粉末が、マグネシアおよび/またはシリカを含む請求項1〜6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。
- 前記チタン酸アルミニウム系セラミックス粉末が、粒度分布のD50の値が20μm以下、かつD90の値が40μm以下のチタン酸アルミニウムであることを特徴とする請求項1〜7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たチタン酸アルミニウム系セラミックスを解砕することを特徴とするチタン酸アルミニウム系セラミックス粉末の製造方法。
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JP2010100510A (ja) * | 2008-01-07 | 2010-05-06 | Sumitomo Chemical Co Ltd | チタン酸アルミニウムセラミックスの製造方法 |
CN101925538A (zh) * | 2008-01-21 | 2010-12-22 | 住友化学株式会社 | 钛酸铝镁的制备方法 |
US20110156323A1 (en) * | 2008-09-04 | 2011-06-30 | Sumitomo Chemical Company, Limited | Process for producing aluminum titanate-based ceramics |
WO2010113893A1 (ja) | 2009-03-30 | 2010-10-07 | 住友化学株式会社 | チタン酸アルミニウム系セラミックス体の製造方法 |
JP5607319B2 (ja) * | 2009-07-16 | 2014-10-15 | 住友化学株式会社 | チタン酸アルミニウム系焼成体の製造方法 |
CN102811972B (zh) * | 2010-03-26 | 2015-03-25 | 大塚化学株式会社 | 柱状钛酸铝及其制造方法 |
WO2012101285A1 (de) * | 2011-01-28 | 2012-08-02 | Mann+Hummel Gmbh | Keramischer körper aus einer aluminiumtitanatmischung |
DE102012003338A1 (de) | 2012-02-17 | 2013-08-22 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Zusammensetzung für die Herstellung von Glaslotenfür Hochtemperaturanwendungen sowie derenVerwendung |
US9623360B2 (en) | 2013-05-20 | 2017-04-18 | Corning Incorporated | Porous ceramic article and method of manufacturing the same |
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CN104014764B (zh) * | 2014-05-22 | 2015-10-14 | 泰州市旺鑫耐火材料有限公司 | 一种铝合金低压铸造用陶瓷浇注口衬套的制作方法 |
US11229902B2 (en) | 2016-05-31 | 2022-01-25 | Corning Incorporated | Porous article and method of manufacturing the same |
CN111527055A (zh) | 2017-10-31 | 2020-08-11 | 康宁股份有限公司 | 包含预反应过的无机颗粒的批料组合物及由其制造生坯体的方法 |
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