CN102245534A - 钛酸铝系烧成体的制造方法 - Google Patents
钛酸铝系烧成体的制造方法 Download PDFInfo
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- CN102245534A CN102245534A CN2009801491760A CN200980149176A CN102245534A CN 102245534 A CN102245534 A CN 102245534A CN 2009801491760 A CN2009801491760 A CN 2009801491760A CN 200980149176 A CN200980149176 A CN 200980149176A CN 102245534 A CN102245534 A CN 102245534A
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- Prior art keywords
- source power
- titanium
- magnesium
- molar weight
- aluminium
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- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 47
- 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 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000010936 titanium Substances 0.000 claims abstract description 80
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 79
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 72
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000203 mixture Substances 0.000 claims abstract description 58
- 239000011777 magnesium Substances 0.000 claims abstract description 51
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 50
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002245 particle Substances 0.000 claims abstract description 45
- 238000010304 firing Methods 0.000 claims abstract description 32
- 238000009826 distribution Methods 0.000 claims abstract description 22
- 239000004411 aluminium Substances 0.000 claims description 67
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 43
- 239000010703 silicon Substances 0.000 claims description 43
- 229910052710 silicon Inorganic materials 0.000 claims description 43
- 230000001186 cumulative effect Effects 0.000 claims description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 12
- 238000002050 diffraction method Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000001413 cellular effect Effects 0.000 claims description 4
- 239000010433 feldspar Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 abstract description 73
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 38
- 239000002994 raw material Substances 0.000 abstract description 38
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000919 ceramic Substances 0.000 abstract description 10
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 229940091250 magnesium supplement Drugs 0.000 description 45
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 26
- 239000000395 magnesium oxide Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 19
- -1 aluminum magnesium titanate class Chemical class 0.000 description 16
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000002425 crystallisation Methods 0.000 description 10
- 230000008025 crystallization Effects 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- 238000013001 point bending Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 229960001866 silicon dioxide Drugs 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 5
- 229940024545 aluminum hydroxide Drugs 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052596 spinel Inorganic materials 0.000 description 5
- 239000011029 spinel Substances 0.000 description 5
- 238000007669 thermal treatment Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000004902 Softening Agent Substances 0.000 description 3
- 159000000013 aluminium salts Chemical class 0.000 description 3
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910001593 boehmite Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- RCYJPSGNXVLIBO-UHFFFAOYSA-N sulfanylidenetitanium Chemical compound [S].[Ti] RCYJPSGNXVLIBO-UHFFFAOYSA-N 0.000 description 3
- 230000000930 thermomechanical effect Effects 0.000 description 3
- 150000003608 titanium Chemical class 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 description 2
- 229940063655 aluminum stearate Drugs 0.000 description 2
- 230000002902 bimodal effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000005368 silicate glass Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 description 1
- LQYXNJNEDCJEGG-UHFFFAOYSA-N 2-methylpropan-2-ol;titanium Chemical compound [Ti].CC(C)(C)O LQYXNJNEDCJEGG-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- BMTAFVWTTFSTOG-UHFFFAOYSA-N Butylate Chemical group CCSC(=O)N(CC(C)C)CC(C)C BMTAFVWTTFSTOG-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- MPCRDALPQLDDFX-UHFFFAOYSA-L Magnesium perchlorate Chemical compound [Mg+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O MPCRDALPQLDDFX-UHFFFAOYSA-L 0.000 description 1
- MQHWFIOJQSCFNM-UHFFFAOYSA-L Magnesium salicylate Chemical compound [Mg+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O MQHWFIOJQSCFNM-UHFFFAOYSA-L 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 235000015076 Shorea robusta Nutrition 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical group CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001398 aluminium Chemical class 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- KMJRBSYFFVNPPK-UHFFFAOYSA-K aluminum;dodecanoate Chemical compound [Al+3].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O KMJRBSYFFVNPPK-UHFFFAOYSA-K 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
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- 238000001816 cooling Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- XZTWHWHGBBCSMX-UHFFFAOYSA-J dimagnesium;phosphonato phosphate Chemical compound [Mg+2].[Mg+2].[O-]P([O-])(=O)OP([O-])([O-])=O XZTWHWHGBBCSMX-UHFFFAOYSA-J 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 229950006191 gluconic acid Drugs 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229920000591 gum Polymers 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 235000019357 lignosulphonate Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
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- DZBOAIYHPIPCBP-UHFFFAOYSA-L magnesium;2-methylprop-2-enoate Chemical compound [Mg+2].CC(=C)C([O-])=O.CC(=C)C([O-])=O DZBOAIYHPIPCBP-UHFFFAOYSA-L 0.000 description 1
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- 238000007493 shaping process Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
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- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- JXJTWJYTKGINRZ-UHFFFAOYSA-J silicon(4+);tetraacetate Chemical compound [Si+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O JXJTWJYTKGINRZ-UHFFFAOYSA-J 0.000 description 1
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- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- 235000019698 starch Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- POWFTOSLLWLEBN-UHFFFAOYSA-N tetrasodium;silicate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])[O-] POWFTOSLLWLEBN-UHFFFAOYSA-N 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- PLSARIKBYIPYPF-UHFFFAOYSA-H trimagnesium dicitrate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PLSARIKBYIPYPF-UHFFFAOYSA-H 0.000 description 1
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical class [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明的目的在于，提供可以制造可以使烧成时的收缩率(烧成收缩率)低的同时，耐热分解性优异的包含钛酸铝类系陶瓷的烧成体的方法。本发明为具有将含有铝源粉末、钛源粉末和镁源粉末的原料混合物的成型体烧成的步骤，该钛源粉末表现出特定的粒径分布特性的钛酸铝系烧成体的制造方法。优选该原料混合物中的按照Al2O3换算的铝源粉末的摩尔量与按照TiO2换算的钛源粉末的摩尔量之比为35:65～45:55，且按照MgO换算的镁源粉末的摩尔量与按照Al2O3换算的铝源粉末的摩尔量和按照TiO2换算的钛源粉末的摩尔量的总计之比为0.03～0.15。
Description
技术领域
本发明涉及包含钛酸铝系陶瓷的烧成体的制造方法，更具体地说，涉及将含有铝源粉末、钛源粉末和镁源粉末的原料混合物的成型体烧成而制造包含钛酸铝镁类陶瓷的烧成体的方法。
背景技术
钛酸铝系陶瓷，含有钛和铝作为构成元素，为在X射线衍射光谱中，具有钛酸铝的结晶图案的陶瓷，作为耐热性优异的陶瓷已知。钛酸铝系陶瓷迄今用作坩锅等烧成用冶具等。该钛酸铝系陶瓷近年作为构成用于捕集从柴油机等内燃机排出的废气中含有的微细碳粒子的陶瓷过滤器的材料，工业上的利用价值提高。
作为钛酸铝系陶瓷的制造方法，已知将含有二氧化钛等钛源化合物的粉末和氧化铝等铝源化合物的粉末的原料混合物烧成的方法(专利文献1)。
但是，钛酸铝，其通过将含有铝源粉末和钛源粉末的原料粉末或该原料粉末的成型体烧成来制造的情况下，存在烧成时大幅收缩，即原料粉末的成型体的烧成收缩率高的问题。若烧成收缩率高则在原料粉末的成型体的烧成时易产生裂纹。
为了解决上述问题，专利文献2中公开了将含有表现出特定的粒径分布特性的TiO2粉末和Al2O3粉末的原料混合物成型为蜂窝状，将该成型体烧成，由此制造钛酸铝质陶瓷蜂窝结构体的方法。
现有技术文献
专利文献
专利文献1：国际公开第05/105704号小册子
专利文献2：国际公开第08/078747号小册子。
发明内容
钛酸铝的熔点高，为1860℃，如上所述，耐热性优异，但通常在800～1200℃附近的温度缓慢地分解为氧化铝(Al2O3)和二氧化钛(TiO2)。因此，要求提高其耐热分解性。
因此，本发明的目的在于，提供可以制造可以使烧成时的收缩率(烧成收缩率)低的同时，耐热分解性优异的包含钛酸铝系陶瓷的烧成体的方法。
本发明提供钛酸铝系烧成体的制造方法，该方法具有将含有铝源粉末、钛源粉末和镁源粉末的原料混合物的成型体烧成的步骤，该钛源粉末在通过激光衍射法测定得到的粒径分布中，按照体积基准，满足下式(1)和(2)。
(V0.5-3＋V15-75)/Vtotal≥0.7 (1)
1/2≤V15-75/ V0.5-3≤3/2 (2)
其中，上式(1)和(2)中，V0.5-3表示粒径为0.5～3μm的累积频率，V15-75表示粒径为15～75μm的累积频率，Vtotal表示粒径为0.1μm以上的累积频率。
此外，优选上述原料混合物中的铝源粉末的摩尔量与钛源粉末的摩尔量之比为35:65～45:55，且镁源粉末的摩尔量与铝源粉末的摩尔量和钛源粉末的摩尔量的总计之比为0.03～0.15。
上述铝源粉末的摩尔量指的是按照Al2O3(氧化铝)换算的摩尔量，通过下式(A)求出。
(铝源粉末的摩尔量)=(w1×M1)/(N1×2) (A)
式(A)中，w1表示铝源粉末的用量(g)，M1表示铝源粉末1摩尔中的铝的摩尔数，N1表示铝源粉末的式量。使用两种以上铝源粉末时，通过式(A)分别求出各铝源粉末的摩尔量，将各摩尔量合计，由此可以求出所使用的铝源粉末的摩尔量(以下在求摩尔量的情况下相同)。
上述钛源粉末的摩尔量指的是按照TiO2(二氧化钛)换算的摩尔量，通过下式(B)求得。
(钛源粉末的摩尔量)=(w2×M2)/N2 ( B)
式(B)中，w2表示钛源粉末的用量(g)，M2表示钛源粉末1摩尔中的钛的摩尔数，N2表示钛源粉末的式量。使用两种以上钛源粉末时，通过式(B)分别求出各钛源粉末的摩尔量，将各摩尔量合计，由此可以求出所使用的钛源粉末的摩尔量(以下在求摩尔量的情况下相同)。
上述镁源粉末的摩尔量指的是按照MgO(氧化镁)换算的摩尔量，通过下式(C)求得。
(镁源粉末的摩尔量)=(w3×M3)/N3 (C)
式(C)中，w3表示镁源粉末的用量(g)，M3表示镁源粉末1摩尔中的镁的摩尔数，N3表示镁源粉末的式量。使用两种以上镁源粉末时，通过式(C)分别求出各镁源粉末的摩尔量，将各摩尔量合计，由此可以求出所使用的镁源粉末的摩尔量(以下在求摩尔量的情况下相同)。
铝源粉末和镁源粉末的D50(50%对应粒径)分别优选为10～50μm和0.5～30μm。
上述原料混合物优选进一步含有硅源粉末。此外，硅源粉末优选为长石、玻璃料（glass frit）或包含它们的混合物的粉末。优选按照SiO2换算的硅源粉末的摩尔量与按照Al2O3换算的铝源粉末的摩尔量和按照TiO2换算的钛源粉末的摩尔量的总计之比约为0.0011～0.123。硅源粉末的D50优选为0.5～30μm。
按照SiO2换算的硅源粉末的摩尔量通过下式(D)求得。
(硅源粉末的摩尔量)=(w4×M4)/N4 (D)
式(D)中，w4表示硅源粉末的用量(g)，M4表示硅源粉末1摩尔中的硅的摩尔数，N4表示硅源粉末的式量。使用两种以上硅源粉末时，通过式(D)分别求出各硅源粉末的按照SiO2换算的摩尔量，将各摩尔量合计，由此可以求出所使用的硅源粉末的摩尔量(以下在求摩尔量的情况下相同)。
作为上述原料混合物的成型体的形状，例如可以为蜂窝状。上述烧成的温度例如为1300～1650℃，烧成时间例如为10分钟～24小时。
而且，本说明书中，“D50”指的是通过激光衍射法测定得到的体积基准的累积百分率达到50%时所对应的粒径。
根据本发明的方法，可以制造可以使原料混合物的成型体的烧成收缩率低的同时耐热分解性优异的钛酸铝系烧成体。
附图说明
图1为表示实施例和比较例中使用的氧化钛A～C的粒径分布的图。
具体实施方式
通过本发明的方法得到的钛酸铝系烧成体，通过将含有铝源粉末、钛源粉末和镁源粉末的原料混合物的成型体烧成来制造。使用上述原料混合物得到的钛酸铝系烧成体为包含钛酸铝镁结晶的烧成体。
本发明的钛酸铝系烧成体的制造方法中，作为钛源粉末，使用表现出特定的粒径分布特性的钛源粉末。进一步地，优选适当调整上述原料混合物中的铝源粉末、钛源粉末和镁源粉末的摩尔量之比(摩尔比)。根据本发明，可以制造可以使上述原料混合物的成型体的烧成时的烧成收缩率充分低的同时，耐热分解性优异的钛酸铝系烧成体。
本发明中使用的原料混合物中含有的铝源粉末，为形成构成钛酸铝系烧成体的铝成分的物质的粉末。作为铝源粉末，可以举出例如氧化铝(氧化铝)的粉末。氧化铝可以为结晶性或不定形(无定形)。氧化铝为结晶性的情况下，作为其晶型，可以举出γ型、δ型、θ型、α型等，优选使用α型的氧化铝。
本发明中使用的铝源粉末还可以为通过在空气中烧成得到氧化铝的物质的粉末。作为上述物质，可以举出例如铝盐、铝醇盐、氢氧化铝、铝等。
铝盐可以为与无机酸的盐(无机盐)或与有机酸的盐(有机盐)。作为铝无机盐，具体地说可以举出例如硝酸铝、硝酸铵铝等硝酸盐，碳酸铵铝等碳酸盐等。作为铝有机盐，可以举出例如草酸铝、乙酸铝、硬脂酸铝、乳酸铝、月桂酸铝等。
此外，作为铝醇盐，具体地说可以举出例如异丙醇铝、乙醇铝、仲丁醇铝、叔丁醇铝等。
氢氧化铝可以为结晶性或不定形(无定形)。氢氧化铝为结晶性的情况下，作为其晶型，可以举出例如三水铝石型、三羟铝石型、norstrandite型、软水铝石型（boehmite）、拟软水铝石型（pseudo－boehmite）等。作为无定形的氢氧化铝，可以举出例如将铝盐、铝醇盐等水溶性铝化合物的水溶液水解得到的铝水解物。
其中，作为铝源粉末，优选使用氧化铝粉末，更优选为α型的氧化铝粉末。而且，铝源粉末可以含有在其制备步骤中不可避免地含有的微量成分。
对铝源粉末的粒径不特别限定，通常D50(50%对应粒径)为10～50μm。为了得到烧成收缩率进一步降低、耐热分解性更优异的小的钛酸铝系烧成体，优选使用D50为15～40μm的铝源粉末。
上述原料混合物中含有的钛源粉末为形成构成钛酸铝系陶瓷的钛成分的物质的粉末，作为上述物质，可以举出例如氧化钛的粉末。作为氧化钛，可以举出例如氧化钛(IV)、氧化钛(III)、氧化钛(II)等，优选使用氧化钛(IV)。氧化钛(IV)可以为结晶性或不定形(无定形)。氧化钛(IV)为结晶性的情况下，作为其晶型，可以举出锐钛矿型、金红石型、板钛矿型等。更优选为锐钛矿型、金红石型的氧化钛(IV)。
本发明中使用的钛源粉末还可以为通过在空气中烧成得到二氧化钛(氧化钛)的物质的粉末。作为上述物质，可以举出例如钛盐、钛醇盐、氢氧化钛、氮化钛、硫化钛、钛等。
作为钛盐，具体地说可以举出三氯化钛、四氯化钛、硫化钛(IV)、硫化钛(VI)、硫酸钛(IV)等。作为钛醇盐，具体地说可以举出乙醇钛(IV)、甲醇钛(IV)、叔丁醇钛(IV)、异丁醇钛(IV)、正丙醇钛(IV)、四异丙醇钛(IV)和它们的螯合物等。
其中，作为钛源粉末，优选使用氧化钛粉末，更优选为氧化钛(IV)粉末。而且，钛源粉末可以含有在其制备步骤中不可避免地含有的微量成分。
其中，本发明中，作为钛源粉末，优选使用在通过激光衍射法得到的粒径分布中，按照体积基准，满足下式(1)和(2)的钛源粉末。
(V0.5-3＋V15-75)/Vtotal≥0.7 (1)
1/2≤V15-75/ V0.5-3≤3/2 (2)
上式(1)和(2)中，V0.5-3表示粒径为0.5～3μm的累积频率，V15-75表示粒径为15～75μm的累积频率，Vtotal表示粒径为0.1μm以上的累积频率。
上式(1)指的是粒径为0.5～3μm的粒子和粒径为15～75μm的粒子的总量，与全部粒子(粒径为0.1μm以上的粒子)的量之比，按照体积基准为0.7以上。如此，通过所使用的钛源粉末主要由粒径为0.5～3μm的粒子和粒径为15～75μm的粒子构成，可以充分降低原料混合物的成型体的烧成收缩率。这是由于供于烧成的原料混合物的成型体中的原料粉末的填充性提高。而且，为了达成这种填充性的提高，仅仅所使用的钛源粉末表现出双峰的粒径分布是不够的，特别优选满足上式(1)和(2)。上式(1)中的(V0.5-3＋V15-75)/Vtotal优选为0.8以上。
作为满足上式(1)的钛源粉末，典型地说，可以举出在通过激光衍射法测定得到的粒径分布曲线中，具有在粒径为0.5～3μm的范围内具有极大的第一峰、和在粒径为15～75μm的范围内具有极大的第二峰，构成这两个峰的粒子的比率，相对于全部粒子(粒径为0.1μm以上的粒子)，按照体积基准，为0.7以上的钛源粉末。表现出这种粒径分布的钛源粉末，例如可以通过将D50(50%对应粒径)为0.5～3μm的钛源粉末和D50为15～75μm的钛源粉末混合来得到。D50为0.5～3μm的钛源粉末和D50为15～75μm的钛源粉末，分别优选在通过激光衍射法测定得到的粒径分布曲线中，具有在粒径为0.5～3μm的范围内具有极大的一个峰、在粒径为15～75μm的范围内具有极大的一个峰。此外，为了得到表现出上述粒径分布的钛源粉末，除了上述以外，例如还可以对D50(50%对应粒径)为15～75μm的钛源粉末进行规定时间的粉碎。
本发明中使用的钛源粉末，在通过激光衍射法测定得到的粒径分布曲线中，可以进一步具有上述第一峰和第二峰以外的峰，但是为了进一步有效地降低烧成收缩率，各钛源粉末优选仅具有上述第一峰和第二峰。即，本发明中使用的钛源粉末优选表现出双峰的粒径分布。
此外，如上式(2)所示，V15-75/ V0.5-3为1/2～3/2，优选为1/2～1/1，进一步优选为1/2～3/4。若该累积频率之比小于1/2或超过3/2，则存在不能充分降低烧成收缩率的趋势。上述累积频率的V15-75/ V0.5-3，在钛源粉末通过将D50(50%对应粒径)为15～75μm的钛源粉末和D50为0.5～3μm的钛源粉末混合来得到时，可以通过调整它们的混合比来进行调整。
若使用满足上式(1)和(2)的钛源粉末，则可以得到强度高的烧成体。此外，由于可以得到致密的烧成体，得到的钛酸铝系烧成体表现出小的热膨胀系数。
本发明中，上述原料混合物中的铝源粉末与钛源粉末的摩尔量之比(按照Al2O3换算的摩尔量: 按照TiO2换算的摩尔量)优选为35:65～45:55，更优选为40:60～45:55。该范围内，通过使用相对于铝源粉末过量的钛源粉末，可以提高烧成体的耐热分解性，且可以降低原料混合物的成型体的烧成收缩率。本发明中，如上所述，通过使用调整为这种铝源粉末与钛源粉末的摩尔比的同时具有特定的粒径分布特性的钛源粉末，可以达成充分低的烧成收缩率。
此外，作为上述原料混合物中含有的镁源粉末，除了氧化镁(氧化镁)的粉末之外，还可以举出通过在空气中烧成得到氧化镁的物质的粉末。作为后者的例子，可以举出例如镁盐、镁醇盐、氢氧化镁、氮化镁、镁等。
作为镁盐，具体地说可以举出氯化镁、高氯酸镁、磷酸镁、焦磷酸镁、草酸镁、硝酸镁、碳酸镁、乙酸镁、硫酸镁、柠檬酸镁、乳酸镁、硬脂酸镁、水杨酸镁、肉豆蔻酸镁、葡糖酸镁、二甲基丙烯酸镁、苯甲酸镁等。
作为镁醇盐，具体地说可以举出甲醇镁、乙醇镁等。而且，镁源粉末可以含有在其制备步骤中不可避免地含有的微量成分。
作为镁源粉末，还可以使用兼具镁源和铝源的功能的物质的粉末。作为这种物质，可以举出例如镁氧尖晶石(MgAl2O4)。而且，作为镁源粉末，使用兼具镁源和铝源的功能的物质的粉末时，铝源粉末的按照Al2O3(氧化铝)换算的量和兼具镁源和铝源的功能的物质粉末中含有的Al成分的按照Al2O3(氧化铝)换算的量的总量，与钛源粉末的按照TiO2(二氧化钛)换算的量的摩尔比在原料混合物中，调整为上述范围内。
对镁源粉末的粒径不特别限定，通常使用D50(50%对应粒径)为0.5～30μm的镁源粉末。为了得到烧成收缩率进一步降低、耐热分解性更优异的钛酸铝系烧成体，优选使用D50为3～20μm的镁源粉末。
原料混合物中的镁源粉末的含量，相对于铝源粉末和钛源粉末的总量，按照摩尔量之比(按照MgO换算的摩尔量)/(按照Al2O3换算的摩尔量＋按照TiO2换算的摩尔量)优选为0.03～0.15，更优选为0.03～0.12。通过将镁源粉末的含量调整在该范围内，可以进一步提高钛酸铝系烧成体的耐热分解性。
此外，上述原料混合物可以进一步含有硅源粉末。硅源粉末为形成硅成分而存在于钛酸铝系烧成体中的物质的粉末，通过并用硅源粉末，可以得到耐热分解性进一步提高的钛酸铝系烧成体。作为硅源粉末，可以举出例如二氧化硅、一氧化硅等氧化硅(silica)的粉末。
此外，硅源粉末还可以为通过在空气中烧成得到二氧化硅的物质的粉末。作为上述物质，可以举出例如硅酸、碳化硅、氮化硅、硫化硅、四氯化硅、乙酸硅、硅酸钠、原硅酸钠、长石、玻璃料等。其中，优选使用长石、玻璃料等，从工业上容易得到、组成稳定的观点考虑，更优选为玻璃料等。而且，玻璃料指的是将玻璃粉碎而得到的片（flake）或粉末状的玻璃。
使用玻璃料时，从进一步提高得到的钛酸铝系烧成体的耐热分解性的观点考虑，优选使用屈服点为700℃以上的玻璃料。本发明中，玻璃料的屈服点，使用热机械分析装置(TMA：Thermo Mechanical Analysis)测定。玻璃料的屈服点定义为在玻璃料的升温过程中，停止膨胀，接着开始收缩的温度(℃)。
构成上述玻璃料的玻璃可以使用以硅酸[SiO2]作为主要成分(在全部成分中超过50质量%时)的通常的硅酸玻璃。构成玻璃料的玻璃，作为硅酸以外的含有成分，与通常的硅酸玻璃同样地，可以含有氧化铝[Al2O3]、氧化钠[Na2O]、氧化钾[K2O]、氧化钙[CaO]、氧化镁[MgO]等。此外，构成玻璃料的玻璃，为了提高玻璃自身的耐热水性，可以含有ZrO2。
对硅源粉末的粒径不特别限定，通常使用D50(50%对应粒径)为0.5～30μm的硅源粉末。为了进一步提高原料混合物的成型体的填充率，优选使用D50为1～20μm的硅源粉末。
原料混合物含有硅源粉末时，在原料混合物中，按照SiO2换算的硅源粉末的摩尔量与按照Al2O3换算的铝源粉末的摩尔量和按照TiO2换算的钛源粉末的摩尔量的总计之比，优选约为0.0011～0.123，更优选为0.073以下。而且，硅源粉末可以含有在其制备步骤中不可避免地含有的微量成分。
而且，本发明中，还可以使用如上述镁氧尖晶石(MgAl2O4)等复合氧化物那样以钛、铝、硅和镁中两种以上的金属元素作为成分的物质作为原料粉末。这种物质可以认为与将各金属源物质混合而成的原料混合物等价。基于这种认识，将原料混合物中的铝源原料、钛源原料、镁源原料和硅源原料的含量调整在上述范围内。
此外，原料混合物中还可以含有钛酸铝、钛酸铝镁本身，例如使用钛酸铝镁作为原料混合物的构成成分时，该钛酸铝镁为兼具钛源、铝源和镁源的功能的原料。
本发明中，将含有上述铝源粉末、钛源粉末和镁源粉末以及任意使用的硅源粉末的原料混合物成型得到成型体后，将该成型体烧成，由此得到钛酸铝系烧成体。通过成型后进行烧成，与直接将原料混合物烧成的情况相比，可以抑制烧成中的收缩。因此，可以更有效地抑制得到的钛酸铝系烧成体的裂纹，此外，可以得到通过烧成而生成的多孔质性的钛酸铝结晶的微孔形状得到维持的钛酸铝系烧成体。对成型体的形状不特别限定，可以举出例如蜂窝状、棒状、管状、板状、坩锅状等。
作为原料混合物的成型中使用的成型机，可以举出单轴加压机、挤出成型机、打片机、造粒机等。进行挤出成型时，可以向原料混合物中例如添加造孔剂、粘合剂、润滑剂、增塑剂、分散剂、以及溶剂等添加剂来进行成型。
作为上述造孔剂，可以举出石墨等碳材料，聚乙烯、聚丙烯、聚甲基丙烯酸甲酯等树脂类，淀粉、坚果壳、核桃壳、玉米等植物类材料，冰以及干冰等。造孔剂的添加量，相对于铝源粉末、钛源粉末、镁源粉末和硅源粉末的总量(以下简称为“基准总量”)100质量份，通常为0～40质量份，优选为0～25质量份。
作为上述粘合剂，可以举出甲基纤维素、羧基甲基纤维素、羧基甲基纤维素钠等纤维素类，聚乙烯醇等醇类，木质素磺酸盐等盐，石蜡、微晶蜡等蜡，EVA、聚乙烯、聚苯乙烯、液晶聚合物、工程塑料等热塑性树脂等。粘合剂的添加量，相对于基准总量100质量份，通常为2质量份～20质量份，优选为5质量份～15质量份。
作为润滑剂和增塑剂，可以举出甘油等醇类，辛酸、十二烷酸、软脂酸、花生酸（アラギン酸）、油酸、硬脂酸等高级脂肪酸，硬脂酸铝等硬脂酸金属盐等。润滑剂和增塑剂的添加量，相对于基准总量100质量份，通常为0～10质量份，优选为0.5～5质量份，更优选为1～5质量份。
作为上述分散剂，可以举出例如硝酸、盐酸、硫酸等无机酸，草酸、柠檬酸、乙酸、苹果酸、乳酸等有机酸，甲醇、乙醇、丙醇等醇类，多元羧酸铵、聚氧亚烷基烷基醚等表面活性剂等。分散剂的添加量，相对于基准总量100质量份，通常为0～20质量份，优选为2～8质量份。
此外，作为上述溶剂，例如可以使用甲醇、乙醇、丁醇、丙醇等一元醇类，丙二醇、聚丙二醇、乙二醇等二元醇类，以及水等。其中，优选为水，从杂质少的观点考虑，更优选使用离子交换水。溶剂的用量，相对于基准总量100质量份，通常为10质量份～100质量份，优选为20质量份～80质量份。
用于成型的原料混合物，可以通过将上述铝源粉末、钛源粉末、镁源粉末、以及任意使用的硅源粉末和上述各种添加剂混合(混炼)来得到。
成型体的烧成中的烧成温度通常为1300℃以上，优选为1400℃以上。此外，烧成温度通常为1650℃以下，优选为1550℃以下。对直至烧成温度的升温速度不特别限定，通常为1℃/小时～500℃/小时。使用硅源粉末时，优选在烧成步骤之前设置在1100～1300℃的温度范围保持3小时以上的步骤(扩散步骤)。由此，可以促进硅源粉末的熔解、扩散。原料混合物含有粘合剂等添加燃烧性有机物时，烧成步骤含有除去这些添加燃烧性有机物的脱脂步骤。脱脂，典型地说，为直至烧成温度的升温阶段(例如150～400℃的温度范围)。脱脂步骤中，优选极力抑制升温速度，优选为5℃/小时～60℃/小时。
烧成通常在大气中进行，但是根据所使用的原料粉末，即铝源粉末、钛源粉末、镁源粉末和二氧化硅源粉末的种类、用量比，也可以在氮气、氩气等惰性气体中烧成，还可以在一氧化碳气体、氢气等还原性气体中烧成。此外，也可以在降低了水蒸气分压的氛围气体中进行烧成。
烧成通常使用管状电炉、箱式电炉、隧道式炉、远红外线炉、微波加热炉、竖式炉、反焰炉、旋转炉、辊底式炉等通常的烧成炉来进行。烧成可以以间歇式或连续式进行。此外，可以以静置式或流动式进行。
烧成所需的时间，若为对于将原料混合物的成型体转变为钛酸铝系结晶来说充分的时间即可，根据原料混合物的量、烧成炉的方式、烧成温度、烧成氛围气体等不同而不同，但是通常为10分钟～24小时。
如此，可以得到目的的钛酸铝系烧成体。该钛酸铝系烧成体，如上所述，耐热分解性优异。此外，该钛酸铝系烧成体优选弯曲强度和低热膨胀性等优异。这种钛酸铝系烧成体具有大致维持刚成型后的成型体的形状的形状。得到的钛酸铝系烧成体通过研磨加工等，可以加工成所需的形状。
通过本发明的方法得到的钛酸铝系烧成体，在X射线衍射光谱中，除了含有钛酸铝镁的结晶图案之外，还可以含有氧化铝、二氧化钛等的结晶图案。而且，通过本发明的方法得到的钛酸铝系烧成体，若无视通过硅进行的置换，则可以以组成式：Al2(1－x)MgxTi(1＋x)O5表示，x的值为0.03以上，优选为0.03～0.15，更优选为0.03～0.12。
实施例
以下通过实施例对本发明进行更具体的说明，但是本发明不被它们所限定。而且，各实施例和比较例中的原料混合物的成型体的烧成收缩率、钛酸铝系烧成体的钛酸铝化率(AT化率)、耐热分解率、三点弯曲强度、热膨胀系数、微孔径、开气孔率和所使用的原料粉末的粒度分布通过下述方法测定。
(1) 烧成收缩率
对于烧成前(挤出成型后)的蜂窝形状的成型体和烧成后的成型体的挤出截面方向(与成型体的挤出方向正交的截面)的长度(间隔壁间距宽度)分别测定5点，将它们的值平均，由此得到烧成前的平均长度和烧成后的平均长度，由该烧成前的平均长度和烧成后的平均长度基于下式算出烧成收缩率。
烧成收缩率(%)={1－(烧成后的平均长度)/(烧成前的平均长度)}×100
(2) AT化率
钛酸铝化率(AT化率)，由粉末X射线衍射光谱中的2θ=27.4°的位置出现的峰[归属于二氧化钛·金红石相(110)面]的积分强度(IT)，和2θ=33.7°的位置出现的峰[归属于钛酸铝镁相(230)面]的积分强度(IAT)，通过下式算出。AT化率=IAT/( IT＋IAT)×100(%)
(3) 耐热分解率
由得到的钛酸铝系烧成体，切出约4mm×约4mm×约50mm的试验片。接着对于该试验片实施热处理，即以300℃/h的升温速度升温至1100℃，在该温度下保持48小时后，以300℃/h的降温速度冷却至室温。进行该热处理之前的AT化率R0(%)和进行了热处理之后的AT化率R(%)通过上述方法测定，作为由于热处理造成的烧成体中的钛酸铝镁结晶的减少率，基于下式，求出耐热分解率。
耐热分解率(%)=(1－R/R0)×100
(4) 三点弯曲强度
由钛酸铝系烧成体，在原料混合物的挤出成型时的挤出方向上切出长度约50mm、宽度约5mm、厚度约5mm的长方体。使用砂纸(#1500)将该切出的烧成体的表面抛光至没有凹凸。得到的样品的三点弯曲强度通过根据JIS R 1601的方法测定。
(5) 热膨胀系数
由钛酸铝系烧成体，切出约4mm×约4mm×约10mm的试验片。接着，对于该试验片实施下述热处理，即以200℃/h的升温速度升温至1000℃，立即冷却至室温(25℃)。对于实施了热处理的试验片，使用热机械分析装置(SII テクノロジー(株)制 TMA6300)，以600℃/h由25℃升温至1000℃，由此时的试验片的膨胀率，基于下式，算出热膨胀系数[K－1]
热膨胀系数[K－1]＝试验片的膨胀率/975[K]
其中，试验片的膨胀率指的是(升温至1000℃时的试验片的体积－升温前(25℃)的试验片的体积)/(升温前(25℃)的试验片的体积)
(6) 微孔径
粉碎0.4g的烧成体，得到约2mm见方的小片，将该小片在120℃下在空气中，使用电炉干燥4小时后，通过压汞法，在测定范围0.001～100.0μm下测定微孔半径，得到表现出频率的最大值的微孔半径。将该微孔半径的2倍的值作为微孔径(mode diameter，模径)。测定装置使用Micromeritics公司制的“オートポアIII9420”。
(7) 开气孔率
通过根据JIS R1634的利用水中浸渍进行的阿基米德法，测定烧成体的水中重量M2(g)、饱水重量M3(g)和干燥重量M1(g)，通过下式算出开气孔率。
开气孔率(%)=100×(M3－M1)/(M3－M2)
(8) 原料粉末的粒度分布
原料粉末的粒度分布和D50(50%对应粒径)使用激光衍射式粒度分布装置[日机装社制“Microtrac HRA(X-100)”]测定。
<实施例1>
作为原料粉末，使用以下的原料粉末。而且，各原料粉末的“质量%”为原料粉末(铝源粉末、钛源粉末、镁源粉末和硅源粉末)的总量为100质量%时的值。下述原料粉末的添加组成，按照氧化铝[Al2O3]、二氧化钛[TiO2]、氧化镁[MgO]和二氧化硅[SiO2]换算的摩尔比，为[Al2O3]/[TiO2]/[MgO]/[SiO2]=34.3%/50.2%/9.4%/6.1%。
(1) 铝源粉末
D50为33μm的氧化铝粉末(α-氧化铝粉末)28质量%
(2) 钛源粉末
具有下述表1和图1所示的粒径分布的D50为1.8μm的氧化钛A(金红石型结晶)48质量%
(3) 镁源粉末
D50为5.5μm的镁氧尖晶石粉末18质量%
(4) 硅源粉末
D50为8.5μm的玻璃料(タカラスタンダード社制“CK0832”)6质量%
向上述铝源粉末、钛源粉末、镁源粉末和硅源粉末的混合物中，相对于该混合物100质量份，加入作为粘合剂的甲基纤维素7.5质量份、作为表面活性剂的聚氧亚烷基烷基醚9.3质量份和作为润滑剂的甘油0.8质量份，进而加入作为分散介质的水38质量份后，使用混炼机进行混炼，由此制造瓷土(成型用原料混合物)。接着将该瓷土挤出成型，由此制造蜂窝形状的成型体。大气氛围气体下，对得到的成型体，进行升温过程兼具除去粘合剂的煅烧(脱脂)步骤的功能的烧成，得到蜂窝形状的多孔质烧成体(蜂窝结构体)。烧成时的最高温度为1450℃，最高温度下的保持时间为5小时。
将得到的多孔质烧成体用乳钵粉碎，通过粉末X射线衍射法，测定得到粉末的衍射光谱，可知该粉末表现出钛酸铝镁的结晶峰。求得的该粉末的AT化率为100%。表2示出蜂窝形状的成型体的烧成收缩率、得到的钛酸铝系烧成体的AT化率、耐热分解率、三点弯曲强度、热膨胀系数、微孔径和开气孔率。
<比较例1>
除了使用以下的原料粉末和添加剂之外，与实施例1同样地得到蜂窝形状的多孔质烧成体。而且，各原料粉末、添加剂的“质量%”为原料粉末(铝源粉末、钛源粉末、镁源粉末和硅源粉末)和添加剂的总量为100质量%时的值。下述原料粉末的添加组成，与实施例1同样地，按照氧化铝[Al2O3]、二氧化钛[TiO2]、氧化镁[MgO]和二氧化硅[SiO2]换算的摩尔比，为[Al2O3]/[TiO2]/[MgO]/[SiO2]=34.3%/50.2%/9.4%/6.1%。
(1) 铝源粉末
D50为33μm的氧化铝粉末(α-氧化铝粉末)24质量%
D50为1.0μm的氢氧化铝粉末1.5质量%
(2) 钛源粉末
具有下述表1和图1所示的粒径分布的D50为14.2μm的氧化钛B(金红石型结晶)43质量%
(3) 镁源粉末
D50为5.5μm的镁氧尖晶石粉末16质量%
(4) 硅源粉末
D50为8.5μm的玻璃料(タカラスタンダード社制“CK0832”)5.5质量%
(5) 造孔剂
D50为23μm的聚乙烯粉末10质量%
将得到的多孔质烧成体用乳钵粉碎，通过粉末X射线衍射法，测定得到粉末的衍射光谱，可知该粉末表现出钛酸铝镁的结晶峰。求得的该粉末的AT化率为100%。表2示出蜂窝形状的成型体的烧成收缩率、得到的钛酸铝系烧成体的AT化率、耐热分解率、热膨胀系数、微孔径和开气孔率。而且，对于三点弯曲强度，由得到的多孔质烧成体制造三点弯曲强度测定用的样品时，在对烧成体的外表面进行抛光的步骤中断裂，因此不能测定(表2中以“-”表示)。
<比较例2>
除了使用以下的原料粉末之外，与实施例1同样地得到蜂窝形状的多孔质烧成体。下述原料粉末的添加组成，与实施例1同样地，按照氧化铝[Al2O3]、二氧化钛[TiO2]、氧化镁[MgO]和二氧化硅[SiO2]换算的摩尔比，为[Al2O3]/[TiO2]/[MgO]/[SiO2]=34.3%/50.2%/9.4%/6.1%。
(1) 铝源粉末
D50为33μm的氧化铝粉末(α-氧化铝粉末)28质量%
(2) 钛源粉末
具有下述表1和图1所示的粒径分布的D50为34.4μm的氧化钛C(金红石型结晶)48质量%
(3) 镁源粉末
D50为5.5μm的镁氧尖晶石粉末18质量%
(4) 硅源粉末
D50为8.5μm的玻璃料(タカラスタンダード社制“CK0832”)6质量%
将得到的多孔质烧成体用乳钵粉碎，通过粉末X射线衍射法，测定得到粉末的衍射光谱，可知该粉末表现出钛酸铝镁的结晶峰。求得的该粉末的AT化率为100%。表2示出蜂窝形状的成型体的烧成收缩率、得到的钛酸铝系烧成体的AT化率、耐热分解率、三点弯曲强度、热膨胀系数、微孔径和开气孔率。
[表1]
[表2]
应该认为本次公开的实施方式和实施例都是举例，而并非进行限制。本发明的范围不是被上述说明而是被权利要求书所公开，含有与权利要求书均等的意义以及在权利要求范围内的全部变更。
产业实用性
通过本发明得到的钛酸铝系烧成体，例如可以合适地用于坩锅、setter、烧箱、筑炉材料等烧成炉用冶具，柴油发动机、汽油发动机等内燃机的废气净化中使用的废气过滤器或催化剂载体，啤酒等饮品的过滤中使用的过滤器，用于选择性地透过石油纯化时产生的气体成分，例如一氧化碳、二氧化碳、氮、氧等的选择透过过滤器等的陶瓷过滤器，基板，电容器等电子元件等。其中，用作陶瓷过滤器等时，本发明的钛酸铝系烧成体由于耐热分解性优异，可以长期维持良好的过滤性能。
Claims (10)
1.钛酸铝系烧成体的制造方法，其具有将含有铝源粉末、钛源粉末和镁源粉末的原料混合物的成型体烧成的步骤，
所述钛源粉末在通过激光衍射法测定得到的粒径分布中，按照体积基准满足下式(1)和(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表示粒径为0.5～3μm的累积频率，V15-75表示粒径为15～75μm的累积频率，Vtotal表示粒径为0.1μm以上的累积频率。
2.如权利要求1所述的方法，其中，所述原料混合物中的按照Al2O3换算的所述铝源粉末的摩尔量与按照TiO2换算的所述钛源粉末的摩尔量之比为35:65～45:55，且按照MgO换算的所述镁源粉末的摩尔量与按照Al2O3换算的所述铝源粉末的摩尔量和按照TiO2换算的所述钛源粉末的摩尔量的总计之比为0.03～0.15。
3.如权利要求1或2所述的方法，其中，所述铝源粉末的体积基准的累积百分率达到50%时所对应的粒径为10～50μm。
4.如权利要求1～3中任意一项所述的方法，其中，所述镁源粉末的体积基准的累积百分率达到50%时所对应的粒径为0.5～30μm。
5.如权利要求1～4中任意一项所述的方法，其中，所述原料混合物还含有硅源粉末。
6.如权利要求5所述的方法，其中，所述硅源粉末为长石、玻璃料、或它们的混合物。
7.如权利要求5或6所述的方法，其中，按照SiO2换算的硅源粉末的摩尔量与按照Al2O3换算的铝源粉末的摩尔量和按照TiO2换算的钛源粉末的摩尔量的总计之比为0.0011～0.123。
8.如权利要求5～7中任意一项所述的方法，其中，所述硅源粉末的体积基准的累积百分率达到50%时所对应的粒径为0.5～30μm。
9.如权利要求1～8中任意一项所述的方法，其中，所述成型体为蜂窝状。
10.如权利要求1～9中任意一项所述的方法，其中，所述烧成的温度为1300～1650℃，烧成时间为10分钟～24小时。
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| 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 |
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| KR20100118976A (ko) * | 2008-01-21 | 2010-11-08 | 스미또모 가가꾸 가부시끼가이샤 | 티탄산알루미늄마그네슘의 제조 방법 |
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