JP5230935B2 - チタン酸アルミニウムマグネシウム結晶構造物及びその製造方法 - Google Patents
チタン酸アルミニウムマグネシウム結晶構造物及びその製造方法 Download PDFInfo
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- JP5230935B2 JP5230935B2 JP2006512851A JP2006512851A JP5230935B2 JP 5230935 B2 JP5230935 B2 JP 5230935B2 JP 2006512851 A JP2006512851 A JP 2006512851A JP 2006512851 A JP2006512851 A JP 2006512851A JP 5230935 B2 JP5230935 B2 JP 5230935B2
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- magnesium titanate
- aluminum magnesium
- containing compound
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- aluminum
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000013078 crystal Substances 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000011777 magnesium Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 35
- 239000002994 raw material Substances 0.000 claims description 18
- 239000002210 silicon-based material Substances 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 229910052596 spinel Inorganic materials 0.000 claims description 8
- 239000011029 spinel Substances 0.000 claims description 8
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 229910052650 alkali feldspar Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 229910052655 plagioclase feldspar Inorganic materials 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000002734 clay mineral Substances 0.000 claims description 3
- 229910052878 cordierite Inorganic materials 0.000 claims 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 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- -1 quasifeldspar Inorganic materials 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 239000006104 solid solution Substances 0.000 abstract description 15
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 6
- 230000035939 shock Effects 0.000 abstract description 4
- 239000002344 surface layer Substances 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 description 22
- 239000010936 titanium Substances 0.000 description 21
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 15
- 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 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 229910020068 MgAl Inorganic materials 0.000 description 4
- 239000002518 antifoaming agent Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000010433 feldspar Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GLDUZMNCEGHSBP-UHFFFAOYSA-N 2-(2-octylphenoxy)ethanol Chemical compound CCCCCCCCC1=CC=CC=C1OCCO GLDUZMNCEGHSBP-UHFFFAOYSA-N 0.000 description 1
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
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- C04B35/465—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 alkaline earth metal titanates
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
(1)組成式:MgxAl2(1-x)Ti(1+x)O5(式中、0.1≦x<1)で表わされるチタン酸アルミニウムマグネシウムにおけるMg,Al及びTiの金属成分比と同様の金属成分比で含む、Mg含有化合物、Al含有化合物及びTi含有化合物を含有する混合物100質量部に対し、融点が700〜1500℃を有するケイ素含有化合物(但し、アルカリ長石を除く)を、それぞれ酸化物に換算して、1〜10質量部混合した原料混合物を1200〜1700℃で焼成することを特徴とするチタン酸アルミニウムマグネシウム結晶構造物の製造方法。
(2)チタン酸アルミニウムマグネシウム結晶をケイ素含有化合物の液相下にて生成させる上記(1)に記載の製造方法。
(3)原料混合物に成形助剤を添加し、次いで成形した成形体を焼成する上記(1)又は(2)に記載の製造方法。
(4)原料混合物を、700〜1000℃の温度範囲において仮焼成し、次いで焼成する上記(1)〜(3)のいずれかに記載の製造方法。
(5)ケイ素含有化合物がアルミノケイ酸塩である上記(1)〜(4)のいずれかに記載の製造方法。
(6)アルミノケイ酸塩が、斜長石、準長石、雲母粘土鉱物、ゼオライト、及びコーディエライトから選ばれる鉱物である上記(5)に記載の製造方法。
(7)原料混合物が、更に、SiO2、ZrO2、Fe2O3、MgO、Al2O3、TiO2、CaO、Y2O3又はMgを含むスピネル型構造の酸化物を含有する上記(1)〜(6)に記載の製造方法。
易焼結α型アルミナ26.7質量%(20モル%)、アナタース型酸化チタン62.8質量%(60モル%)及び天然鉱物として存在するペリクレース(Periclase)型の酸化マグネシウム10.5質量%(20モル%)からなる混合物100質量部に対して、化学式:(Na0.6K0.4)AlSi3O8で表されるアルカリ長石を、表1に示されるようなSi原子の固溶率(置換率)になるように1〜10質量部添加し、また、バインダーとしてポリビニルアルコールを0.25質量部、解膠剤としてジエチルアミンを1質量部、消泡剤としてポリプロピレングリコールを0.5質量部それぞれ添加した。次いで、ボールミルで3時間混合後、120℃の乾燥機で12時間以上乾燥させて原料粉末を得た。
得られた原料粉末を150メッシュ程度に粉砕し、60MPaの成形圧でプレスして100mm×100mm×10mmの成形体を得た。
この成形体について、下記の加熱パターンにしたがって大気中で焼成した後、放冷してチタン酸アルミニウムマグネシウム焼結体を得た。
室温−140℃ 21時間
140℃保持 14時間
140−216℃ 21時間
216−295℃ 16時間
295−379℃ 46時間
379−458℃ 20時間
458−700℃ 28時間
700℃保持 3時間
700−1000℃ 26時間
1000−1400℃ 3時間
1400℃保持 4時間
上記実施例1〜5において、アルカリ長石を添加することなく、それ以外は、実施例1〜5と同様に実施することによりチタン酸アルミニウムマグネシウム焼結体を得た。
まず、チタン酸アルミニウムマグネシウムが熱分解するときにTiO2(ルチル)とMgAl2O4(スピネル)を生じるので、ルチルの(110)面の回折ピークの積分強度(ITiO2(110))とチタン酸アルミニウムマグネシウムの(023)面の回折ピークの積分強度(IMAT(023))を用いてチタン酸アルミニウムマグネシウムのルチルに対する強度比Rを下記式より求めた。
R=IMAT(023)/{IMAT(023)+ITiO2(110)}
更に、1100℃における熱処理を行う前の焼結体についても、同様の方法でチタン酸アルミニウムマグネシウムのルチルに対する強度比R0を求めた。
α=(R/R0)×100
次に、上記実施例1〜5と比較例1の各焼結体について、3mm×4mm×40mmに切り出し、表面研磨および稜研磨(角取り)を行った。これについて、JIS R1601にしたがって3点曲げ強度を測定し、その結果をそれぞれ表1に示す。
易焼結α型アルミナ26.7質量%(20モル%)、アナタース型酸化チタン62.8質量%(60モル%)及び天然鉱物として存在するペリクレース(Periclase)型の酸化マグネシウム10.5質量%(20モル%)からなる混合物100質量部に対して、表2に示される化学式及び融点を有するアルミノケイ酸塩鉱物を、SiO2換算にして1質量部になるよう添加した。
Claims (7)
- 組成式:MgxAl2(1-x)Ti(1+x)O5(式中、0.1≦x<1)で表わされるチタン酸アルミニウムマグネシウムにおけるMg,Al及びTiの金属成分比と同様の金属成分比で含む、Mg含有化合物、Al含有化合物及びTi含有化合物を含有する混合物100質量部に対し、融点が700〜1500℃を有するケイ素含有化合物(但し、アルカリ長石を除く)を、それぞれ酸化物に換算して、1〜10質量部混合した原料混合物を1200〜1700℃で焼成することを特徴とするチタン酸アルミニウムマグネシウム結晶構造物の製造方法。
- チタン酸アルミニウムマグネシウム結晶をケイ素含有化合物の液相下にて生成させる請求項1に記載の製造方法。
- 原料混合物に成形助剤を添加し、次いで成形した成形体を焼成する請求項1又は2に記載の製造方法。
- 原料混合物を、700〜1000℃の温度範囲において仮焼成し、次いで焼成する請求項1〜3のいずれかに記載の製造方法。
- ケイ素含有化合物がアルミノケイ酸塩である請求項1〜4のいずれかに記載の製造方法。
- アルミノケイ酸塩が、斜長石、準長石、雲母粘土鉱物、ゼオライト、及びコーディエライトから選ばれる鉱物である請求項5に記載の製造方法。
- 原料混合物が、更に、SiO2、ZrO2、Fe2O3、MgO、Al2O3、TiO2、
CaO、Y2O3又はMgを含むスピネル型構造の酸化物を含有する請求項1〜6に記
載の製造方法。
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EP1741684A4 (en) | 2009-08-19 |
JPWO2005105704A1 (ja) | 2008-03-13 |
KR20070012365A (ko) | 2007-01-25 |
CA2563600A1 (en) | 2005-11-10 |
EP1741684A1 (en) | 2007-01-10 |
WO2005105704A1 (ja) | 2005-11-10 |
EP1741684B1 (en) | 2018-11-07 |
CN1946653A (zh) | 2007-04-11 |
CN100447105C (zh) | 2008-12-31 |
US8557216B2 (en) | 2013-10-15 |
US20130345043A1 (en) | 2013-12-26 |
KR101158383B1 (ko) | 2012-06-22 |
US20070224110A1 (en) | 2007-09-27 |
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