JP5495545B2 - 多孔質セラミック部材およびその製法ならびにフィルタ - Google Patents
多孔質セラミック部材およびその製法ならびにフィルタ Download PDFInfo
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- JP5495545B2 JP5495545B2 JP2008327194A JP2008327194A JP5495545B2 JP 5495545 B2 JP5495545 B2 JP 5495545B2 JP 2008327194 A JP2008327194 A JP 2008327194A JP 2008327194 A JP2008327194 A JP 2008327194A JP 5495545 B2 JP5495545 B2 JP 5495545B2
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- 239000000919 ceramic Substances 0.000 title claims description 63
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000002245 particle Substances 0.000 claims description 206
- 239000013078 crystal Substances 0.000 claims description 163
- 239000000843 powder Substances 0.000 claims description 133
- 239000002994 raw material Substances 0.000 claims description 41
- 229910052782 aluminium Inorganic materials 0.000 claims description 25
- 238000001354 calcination Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 23
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 19
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 description 32
- 239000011148 porous material Substances 0.000 description 22
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 20
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 18
- 238000001125 extrusion Methods 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 229910052749 magnesium Inorganic materials 0.000 description 17
- 230000035939 shock Effects 0.000 description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000006104 solid solution Substances 0.000 description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 6
- 239000001095 magnesium carbonate Substances 0.000 description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
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- 238000013001 point bending Methods 0.000 description 4
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- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910052878 cordierite Inorganic materials 0.000 description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910017682 MgTi Inorganic materials 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- NJFMNPFATSYWHB-UHFFFAOYSA-N ac1l9hgr Chemical compound [Fe].[Fe] NJFMNPFATSYWHB-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 238000004332 deodorization Methods 0.000 description 1
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
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- 230000008646 thermal stress Effects 0.000 description 1
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Description
また、本発明の多孔質セラミック部材は、任意断面における前記単一結晶粒子の面積比率が10%以上であることにより、単一結晶粒子および非晶質材料による多結晶粒子の接合が強固となり、機械的強度を向上させることができる。
また、本発明の多孔質セラミック部材は、前記多結晶粒子の面積比率が60%以上であるため、このような多孔質セラミック部材では、結晶軸の向きが異なる複数の前記結晶からなる(種々の方向を向いた複数の柱状の単一結晶粒子からなる)多結晶粒子の存在比率が多くなり、さらに耐熱衝撃性を向上させることができる。
また、本発明の多孔質セラミック部材は、多結晶粒子は、平均粒径が25μm以上であることを特徴とする。このような多孔質セラミック部材では、気孔径、気孔率を大きくすることができる。
また、本発明の多孔質セラミック部材は、SiをSiO2換算で全量中0.5〜5質量%含有することを特徴とする。SiをSiO2換算で全量中0.5〜5質量%とすることにより、擬ブルッカイト型の結晶粒子同士を、Siを含有する非晶質材料で十分に連結でき、強度を向上できるとともに、Si量が少量であるため、気孔率および気孔径の低下を抑制できる。
このような多孔質セラミック部材の製造方法では、仮焼粉末を解砕して、Al、TiおよびOを含有する単一の結晶からなる仮焼単一結晶粉末と、結晶軸の向きが異なる複数の前記結晶からなる仮焼多結晶粉末とを具備する混合粉末を作製し、この混合粉末にSiO2粉末を添加してなる原料粉末を成形し、仮焼温度よりも低い温度で焼成するため、単一結晶粒子同士および単一結晶粒子と多結晶粒子とが殆ど焼結することなく、Siを含有する非晶質材料で接合できるため、造孔剤を用いることなく、気孔率が大きく、気孔径が大きい多孔質セラミック部材を得ることができる。
Al、TiおよびOを含有する単一の結晶は、Al、TiおよびOを含有する化合物であるチタン酸アルミニウム型の結晶であり、擬ブルッカイト型結晶ということがある。擬ブルッカイト型の結晶には、モル比による組成式がAl2TiO5で表されるチタン酸アルミニウム以外に、MgTi2O5で表されるチタン酸マグネシウムがあり、これらの成分はお互いに全率固溶体を形成することが知られており、Al2(1−x)MgxTi(1+x)O5(0.21≦x≦0.5)で表されるチタン酸アルミニウムとチタン酸マグネシウムとの固溶体(別名:チタン酸アルミニウムマグネシウム)からなる結晶が知られている。
本発明では、任意断面における単一結晶粒子11の面積比率は10%以上、多結晶粒子12の面積比率は60%以上とされている。
本発明の多孔質セラミック部材は、単一結晶粒子11に加えて単一結晶粒子11の集合体である多結晶粒子12が存在することにより、例えば排ガス触媒用ハニカム構造体に適用するために押出成形によってハニカム構造体を作製した場合、柱状の単一結晶粒子11は押出方向に配向しやすいが、ほぼ球状、もしくは球状に近い形状を有している多結晶粒子12を構成している柱状の単一結晶粒子11は種々の方向を向いている。これら単一結晶粒子と多結晶粒子内の各粒子の結晶方向は、EBSD(Electron Backscattered Diffraction)分析により測定することができる。
また、本発明の多孔質セラミック部材では、SiをSiO2換算で全量中0.5〜5質量%含有することが望ましい。SiをSiO2換算で全量中0.5〜5質量%とすることにより、擬ブルッカイト型の結晶粒子同士を、Siを含有する非晶質材料で十分に連結でき、強度を向上できるとともに、Si量が少量であるため、気孔率および気孔径の低下を抑制できる。Si量は、強度および所定の気孔率および気孔径を得るという観点から、SiO2換算で全量中1〜3質量%含有することが望ましい。Si量は、蛍光X線分析法やICP(Inductively Coupled Plasma)発光分析法により測定することができる。
得られたハニカム構造体を切り出して、気孔率および気孔径を水銀圧入法により求めた。また、このハニカム構造体を大気中において1400℃まで1分で急激に昇温した後放冷した時にハニカム構造体内部にクラックが発生したかどうかをX線透過法で観察して調べた。具体的には急激に昇温した各10個のハニカム構造体を用意し、透過型X線装置を用いて、このハニカム構造体にX線を照射してハニカム構造体表面または内部にクラックがないかを調べた。表2には各10個のハニカム構造体いずれにもクラックが認められなかったものを○、1〜2個のクラックが認められたものを△、3個以上のクラックが認められたものを×として表記した。なお、このクラックは隙間が数百μm以上のものであり、隙間が1μm未満のマイクロクラックを含まない。
1375℃で4時間焼成して、多孔質セラミック部材からなる円柱状ハニカム体を得た。
2・・・外周壁
3・・・セル
4・・・隔壁
11・・・単一結晶粒子
12・・・多結晶粒子
13・・・非晶質材料
Claims (5)
- モル比による組成式がAl2TiO5、Al2(1−x)MgxTi(1+x)O5 (0.21≦x≦0.5)、Al2(1−x−y)MgxFe2yTi(1+x)O5 (0.21≦x≦0.8、0.05≦y≦0.2)のいずれかで表される単一の結晶からなる単一結晶粒子と、結晶軸の向きが異なる複数の前記結晶からなる多結晶粒子とを具備してなり、任意断面における前記単一結晶粒子の面積比率が10%以上、前記多結晶粒子の面積比率が60%以上であって、前記単一結晶粒子同士および前記単一結晶粒子と前記多結晶粒子とを、Siを含有する非晶質材料で部分的に接合してなることを特徴とする多孔質セラミック部材。
- 前記多結晶粒子は、平均粒径が25μm以上であることを特徴とする請求項1に記載の多孔質セラミック部材。
- SiをSiO2換算で全量中0.5〜5質量%含有することを特徴とする請求項1または請求項2に記載の多孔質セラミック部材。
- 請求項1乃至請求項3のいずれかに記載の多孔質セラミック部材の製造方法であって、Al源粉末およびTi源粉末を含有する混合粉末、Al源粉末,Ti源粉末およびMg源粉末を含有する混合粉末、Al源粉末,Ti源粉末,Mg源粉末およびFe源粉末を含有する混合粉末のいずれかを用いて造粒粉末を作製する造粒工程と、前記造粒粉末を1400℃以上の仮焼温度で仮焼して仮焼粉末を作製する仮焼工程と、前記仮焼粉末を解砕して、Al、TiおよびOを含有する単一の結晶からなる仮焼単一結晶粒子粉末と、結晶軸の向きが異なる複数の前記結晶からなる仮焼多結晶粒子粉末とを具備する混合粉末を作製する解砕工程と、前記混合粉末にSiO2粉末を添加してなる原料粉末を作製する原料粉末作製工程と、前記原料粉末を用いて成形体を作製する成形工程と、前記成形体を、前記仮焼温度よりも低い1400℃未満の温度で焼成する焼成工程とを具備することを特徴とする多孔質セラミック部材の製造方法。
- 請求項1乃至3のうちいずれかに記載の多孔質セラミック部材からなるフィルタエレメントを具備することを特徴とするフィルタ。
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CN200980133200.1A CN102131747B (zh) | 2008-08-28 | 2009-08-28 | 多孔质陶瓷部件及其制作方法以及过滤器 |
EP20090810031 EP2319816A4 (en) | 2008-08-28 | 2009-08-28 | POROUS CERAMIC ELEMENT, MANUFACTURING METHOD AND FILTER THEREOF |
PCT/JP2009/065070 WO2010024383A1 (ja) | 2008-08-28 | 2009-08-28 | 多孔質セラミック部材およびその製法ならびにフィルタ |
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JP5445997B2 (ja) * | 2009-06-25 | 2014-03-19 | 大塚化学株式会社 | ハニカムフィルタ |
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CN102718541B (zh) * | 2012-02-21 | 2013-11-06 | 山东科技大学 | 孔内带有晶须或棒晶的多孔材料及其制备方法 |
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US9623360B2 (en) | 2013-05-20 | 2017-04-18 | Corning Incorporated | Porous ceramic article and method of manufacturing the same |
US9376347B2 (en) * | 2013-05-20 | 2016-06-28 | Corning Incorporated | Porous ceramic article and method of manufacturing the same |
US9908260B2 (en) | 2013-05-20 | 2018-03-06 | Corning Incorporated | Porous ceramic article and method of manufacturing the same |
CN103343251B (zh) * | 2013-06-30 | 2015-08-05 | 成都易态膜分离技术有限公司 | 烧结Ti-Al基合金多孔材料、应用及改善其孔结构的方法 |
US10252441B2 (en) | 2013-08-28 | 2019-04-09 | Corning Incorporated | System and method for cutting a wet green ceramic article |
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