JP4844770B2 - チタン酸アルミニウム系焼成体の製造方法 - Google Patents
チタン酸アルミニウム系焼成体の製造方法 Download PDFInfo
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- JP4844770B2 JP4844770B2 JP2008315945A JP2008315945A JP4844770B2 JP 4844770 B2 JP4844770 B2 JP 4844770B2 JP 2008315945 A JP2008315945 A JP 2008315945A JP 2008315945 A JP2008315945 A JP 2008315945A JP 4844770 B2 JP4844770 B2 JP 4844770B2
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Description
(V0.5-3+V15-75)/Vtotal≧0.7 (1)
1/2≦V15-75/V0.5-3≦3/2 (2)
ここで、上記式(1)および(2)中、V0.5-3は粒径0.5〜3μmの累積頻度、V15-75は粒径15〜75μmの累積頻度、Vtotalは粒径0.1μm以上の累積頻度である。
(V0.5-3+V15-75)/Vtotal≧0.7 (1)
1/2≦V15-75/V0.5-3≦3/2 (2)
上記式(1)および(2)中、V0.5-3は粒径0.5〜3μmの累積頻度、V15-75は粒径15〜75μmの累積頻度、Vtotalは粒径0.1μm以上の累積頻度である。
焼成前(押し出し成形後)のハニカム形状の成形体と、焼成後の成形体の押し出し断面方向(成形体における押し出し方向とは垂直な方向の断面)の長さ(隔壁ピッチ幅)を、それぞれ5点測定し、それらの値を平均することに得られる焼成前の平均長さおよび焼成後の平均長さから、下記式に基づき焼成収縮率を算出した。
焼成収縮率(%)={1−(焼成後の平均長さ)/(焼成前の平均長さ)}×100
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、下記式により算出した。
AT化率=IAT/(IT+IAT)×100(%)
得られたチタン酸アルミニウム系焼成体から、約4mm×4mm×50mmの試験片を切り出した。ついで、この試験片に対して、300℃/hの昇温速度で1100℃まで昇温し、同温度で48時間保持した後、300℃/hの降温速度で室温まで冷却する熱処理を施した。当該熱処理を行なう前のAT化率R0(%)と熱処理を行なった後のAT化率R(%)を上記方法により測定し、熱処理による焼成体中のチタンアルミニウムマグネシウム結晶の減少率として、下記式に基づき、耐熱分解率を求めた。
耐熱分解率(%)=(R/R0)×100
チタン酸アルミニウム系焼成体から、原料混合物の押し出し成形時の押出し方向に長さ50mm、幅5mm、厚さ5mm程度の直方体形状に切り出した。この切り出した焼成体の外表面を紙やすり(#1500)を用いて凹凸がなくなるまで研磨した。得られたサンプルの三点曲げ強度を、JIS R 1601に準拠した方法により測定した。
チタン酸アルミニウム系焼成体から、約4mm×4mm×10mmの試験片を切り出した。ついで、この試験片に対して、200℃/hの昇温速度で1000℃まで昇温し、直ちに室温(25℃)まで冷却する熱処理を施した。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体積−昇温前(25℃)における試験片の体積)/(昇温前(25℃)における試験片の体積)
を意味する。
0.4gの焼成体を砕き、得られた約2mm角の小片を、120℃で4時間、空気中で、電気炉を用いて乾燥させた後、水銀圧入法により、細孔半径測定範囲0.001〜100.0μmまで測定し、頻度の最大値を示す細孔半径を得た。この細孔半径を2倍した値を細孔径(モード径)とした。測定装置には、Micromeritics社製の「オートポアIII9420」を用いた。
JIS R1634に準拠した、水中浸漬によるアルキメデス法により、焼成体の水中重量M2(g)、飽水重量M3(g)および乾燥重量M1(g)を測定し、下記式により開気孔率を算出した。
開気孔率(%)=100×(M3−M1)/(M3−M2)
原料粉末の、粒径分布および体積基準の累積百分率50%相当粒子径(D50)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。なお、各原料粉末の「質量%」は、原料粉末(アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびケイ素源粉末)の合計量を100質量%としたときの値である。下記の原料粉末の仕込み組成は、アルミナ〔Al2O3〕、チタニア〔TiO2〕、マグネシア〔MgO〕およびシリカ〔SiO2〕換算のモル比で、〔Al2O3〕/〔TiO2〕/〔MgO〕/〔SiO2〕=34.3%/50.2%/9.4%/6.1%である。
(1)アルミニウム源粉末
D50が33μmの酸化アルミニウム粉末(α−アルミナ粉末) 28質量%
(2)チタニウム源粉末
下記表1および図1に示される粒径分布を有するD50が1.8μmの酸化チタンA(ルチル型結晶) 48質量%
(3)マグネシウム源粉末
D50が5.5μmのマグネシアスピネル粉末 18質量%
(4)ケイ素源粉末
D50が8.5μmのガラスフリット(タカラスタンダード社製「CK0832」) 6質量%
上記アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびケイ素源粉末からなる混合物に、該混合物100質量部に対して、バインダとしてメチルセルロース 7.5質量部、界面活性剤としてポリオキシアルキレンアルキルエーテル 9.3質量部、および、潤滑剤としてグリセリン 0.8質量部を加え、さらに、分散媒として水を38質量部加えた後、混練機を用いて混練することにより、坏土(成形用原料混合物)を調製した。ついで、この坏土を押し出し成形することにより、ハニカム形状の成形体を作製した。得られた成形体を、大気雰囲気下で、バインダを除去する仮焼(脱脂)工程を含む焼成を行ない、ハニカム形状の多孔質焼成体(ハニカム構造体)を得た。焼成時の最高温度は、1450℃とし、最高温度での保持時間は5時間とした。
以下の原料粉末および添加剤を用いたこと以外は、実施例1と同様にしてハニカム形状の多孔質焼成体を得た。なお、各原料粉末、添加剤の「質量%」は、原料粉末(アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびケイ素源粉末)および添加剤の合計量を100質量%としたときの値である。下記の原料粉末の仕込み組成は、実施例1と同じく、アルミナ〔Al2O3〕、チタニア〔TiO2〕、マグネシア〔MgO〕およびシリカ〔SiO2〕換算のモル比で、〔Al2O3〕/〔TiO2〕/〔MgO〕/〔SiO2〕=34.3%/50.2%/9.4%/6.1%である。
(1)アルミニウム源粉末
D50が33μmの酸化アルミニウム粉末(α−アルミナ粉末) 24質量%
D50が1.0μmの水酸化アルミニウム粉末 1.5質量%
(2)チタニウム源粉末
下記表1および図1に示される粒径分布を有するD50が14.2μmの酸化チタンB(ルチル型結晶) 43質量%
(3)マグネシウム源粉末
D50が5.5μmのマグネシアスピネル粉末 16質量%
(4)ケイ素源粉末
D50が8.5μmのガラスフリット(タカラスタンダード社製「CK0832」) 5.5質量%
(5)造孔剤
D50が23μmのポリエチレン粉末 10質量%
以下の原料粉末を用いたこと以外は、実施例1と同様にしてハニカム形状の多孔質焼成体を得た。下記の原料粉末の仕込み組成は、実施例1と同じく、アルミナ〔Al2O3〕、チタニア〔TiO2〕、マグネシア〔MgO〕およびシリカ〔SiO2〕換算のモル比で、〔Al2O3〕/〔TiO2〕/〔MgO〕/〔SiO2〕=34.3%/50.2%/9.4%/6.1%である。
(1)アルミニウム源粉末
D50が33μmの酸化アルミニウム粉末(α−アルミナ粉末) 28質量%
(2)チタニウム源粉末
下記表1および図1に示される粒径分布を有するD50が34.4μmの酸化チタンC(ルチル型結晶) 48質量%
(3)マグネシウム源粉末
D50が5.5μmのマグネシアスピネル粉末 18質量%
(4)ケイ素源粉末
D50が8.5μmのガラスフリット(タカラスタンダード社製「CK0832」) 6質量%
Claims (8)
- アルミニウム源粉末、チタニウム源粉末およびマグネシウム源粉末を含む原料混合物の成形体を焼成する工程を備え、
前記チタニウム源粉末は、レーザ回折法により測定される粒径分布において、体積基準で、下記式(1)および(2):
(V0.5-3+V15-75)/Vtotal≧0.7 (1)
1/2≦V15-75/V0.5-3≦3/2 (2)
(式中、V0.5-3は粒径0.5〜3μmの累積頻度、V15-75は粒径15〜75μmの累積頻度、Vtotalは粒径0.1μm以上の累積頻度である。)
を満たし、
前記マグネシウム源粉末の体積基準の累積百分率50%相当粒子径が、0.5〜30μmであり、
前記原料混合物中における、Al2O3換算での前記アルミニウム源粉末とTiO2換算での前記チタニウム源粉末とのモル比は、35:65〜45:55の範囲内(但し、45:55を除く)であり、かつ、Al2O3換算での前記アルミニウム源粉末とTiO2換算での前記チタニウム源粉末との合計量に対する、MgO換算での前記マグネシウム源粉末の量は、モル比で0.03〜0.15の範囲内であるチタン酸アルミニウム系焼成体の製造方法。 - 前記原料混合物は、ケイ素源粉末をさらに含む請求項1に記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記ケイ素源粉末の体積基準の累積百分率50%相当粒子径が、0.5〜30μmである請求項2に記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記アルミニウム源粉末の体積基準の累積百分率50%相当粒子径が、10〜50μmである請求項1〜3のいずれかに記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記ケイ素源粉末は、長石あるいはガラスフリット、またはそれらの混合物である請求項2〜4のいずれかに記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記原料混合物中における、SiO2換算での前記ケイ素源粉末の量は、Al2O3換算での前記アルミニウム源粉末とTiO2換算での前記チタニウム源粉末との合計量100質量部に対して、0.1〜10質量部である請求項2〜5のいずれかに記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記成形体がハニカム形状である請求項1〜6のいずれかに記載のチタン酸アルミニウム系焼成体の製造方法。
- 前記焼成の温度が1300〜1650℃であり、焼成時間が10分〜24時間である請求項1〜7のいずれかに記載のチタン酸アルミニウム系焼成体の製造方法。
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JP2008315945A JP4844770B2 (ja) | 2008-12-11 | 2008-12-11 | チタン酸アルミニウム系焼成体の製造方法 |
EP09831962A EP2368866A4 (en) | 2008-12-11 | 2009-12-11 | PROCESS FOR MANUFACTURING COOKED PRODUCT BASED ON ALUMINUM TITANATE |
KR1020117011875A KR20110095273A (ko) | 2008-12-11 | 2009-12-11 | 티탄산 알루미늄계 소성체의 제조 방법 |
CN2009801491760A CN102245534A (zh) | 2008-12-11 | 2009-12-11 | 钛酸铝系烧成体的制造方法 |
PCT/JP2009/070740 WO2010067859A1 (ja) | 2008-12-11 | 2009-12-11 | チタン酸アルミニウム系焼成体の製造方法 |
TW098142556A TW201033155A (en) | 2008-12-11 | 2009-12-11 | Process for producing an aluminum titanate-based fired body |
US13/131,488 US20110287921A1 (en) | 2008-12-11 | 2009-12-11 | Process for producing aluminum titanate-based fired body |
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JP5771085B2 (ja) * | 2010-07-14 | 2015-08-26 | 住友化学株式会社 | グリーン成形体、および、チタン酸アルミニウム焼成体の製造方法 |
CN103008662B (zh) * | 2011-09-23 | 2015-06-03 | 复盛应用科技股份有限公司 | 复合金属的一体成型方法 |
US9878958B2 (en) * | 2012-02-29 | 2018-01-30 | Corning Incorporated | Dimensional control of ceramic structures via composition |
US9475734B2 (en) | 2012-05-31 | 2016-10-25 | Corning Incorporated | Shrinkage control in aluminum titanate using carbonates |
US8865054B1 (en) * | 2013-03-15 | 2014-10-21 | Ibiden Co., Ltd. | Method for manufacturing aluminum-titanate-based ceramic honeycomb structure |
JP6502495B2 (ja) * | 2014-11-19 | 2019-04-17 | コーニング インコーポレイテッド | 制御されたサイズ分布を有するセラミック粉末 |
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