CN102143925A - 钛酸铝系陶瓷的制造方法 - Google Patents
钛酸铝系陶瓷的制造方法 Download PDFInfo
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- CN102143925A CN102143925A CN200980134430XA CN200980134430A CN102143925A CN 102143925 A CN102143925 A CN 102143925A CN 200980134430X A CN200980134430X A CN 200980134430XA CN 200980134430 A CN200980134430 A CN 200980134430A CN 102143925 A CN102143925 A CN 102143925A
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- titanium
- aluminium
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- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims abstract description 30
- 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 30
- 238000004519 manufacturing process Methods 0.000 title description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 65
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000000203 mixture Substances 0.000 claims abstract description 57
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000010936 titanium Substances 0.000 claims abstract description 29
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- 239000007858 starting material Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims description 110
- 239000004411 aluminium Substances 0.000 claims description 56
- 239000002994 raw material Substances 0.000 claims description 46
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 43
- 238000000465 moulding Methods 0.000 claims description 24
- 239000011777 magnesium Substances 0.000 claims description 22
- 229910052749 magnesium Inorganic materials 0.000 claims description 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 20
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- 239000010433 feldspar Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims 2
- 238000010304 firing Methods 0.000 abstract description 12
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 5
- 230000008602 contraction Effects 0.000 abstract 1
- 229940091250 magnesium supplement Drugs 0.000 description 18
- 239000002904 solvent Substances 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- -1 methoxyl group Chemical group 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 12
- 230000008025 crystallization Effects 0.000 description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 10
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 159000000013 aluminium salts Chemical class 0.000 description 3
- 229910000329 aluminium sulfate 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
- 239000002131 composite material Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 150000002500 ions Chemical group 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- RCYJPSGNXVLIBO-UHFFFAOYSA-N sulfanylidenetitanium Chemical compound [S].[Ti] RCYJPSGNXVLIBO-UHFFFAOYSA-N 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-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
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 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
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 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
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-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
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 150000003608 titanium Chemical class 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
- 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
- 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- NDHFYDKYYXSPFR-UHFFFAOYSA-N CC(C)CO[Ti] Chemical compound CC(C)CO[Ti] NDHFYDKYYXSPFR-UHFFFAOYSA-N 0.000 description 1
- RCZPHVPIOWNERS-UHFFFAOYSA-N CCCO[Ti] Chemical compound CCCO[Ti] RCZPHVPIOWNERS-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
- 241000040710 Chela Species 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 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
- 229910020068 MgAl Inorganic materials 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
- 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
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-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
- COASEVWSBFDUAY-UHFFFAOYSA-N acetic acid;silicon Chemical compound [Si].CC(O)=O COASEVWSBFDUAY-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 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
- 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
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- JPNZKPRONVOMLL-UHFFFAOYSA-N azane;octadecanoic acid Chemical class [NH4+].CCCCCCCCCCCCCCCCCC([O-])=O JPNZKPRONVOMLL-UHFFFAOYSA-N 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 235000005822 corn Nutrition 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
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 229950006191 gluconic acid Drugs 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229920005610 lignin Polymers 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
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- PJJZFXPJNUVBMR-UHFFFAOYSA-L magnesium benzoate Chemical compound [Mg+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 PJJZFXPJNUVBMR-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229960005336 magnesium citrate Drugs 0.000 description 1
- 239000004337 magnesium citrate Substances 0.000 description 1
- 235000002538 magnesium citrate Nutrition 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229960000816 magnesium hydroxide Drugs 0.000 description 1
- OVGXLJDWSLQDRT-UHFFFAOYSA-L magnesium lactate Chemical compound [Mg+2].CC(O)C([O-])=O.CC(O)C([O-])=O OVGXLJDWSLQDRT-UHFFFAOYSA-L 0.000 description 1
- 239000000626 magnesium lactate Substances 0.000 description 1
- 229960004658 magnesium lactate Drugs 0.000 description 1
- 235000015229 magnesium lactate Nutrition 0.000 description 1
- 229940105112 magnesium myristate Drugs 0.000 description 1
- UHNWOJJPXCYKCG-UHFFFAOYSA-L magnesium oxalate Chemical compound [Mg+2].[O-]C(=O)C([O-])=O UHNWOJJPXCYKCG-UHFFFAOYSA-L 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 229910000400 magnesium phosphate tribasic Inorganic materials 0.000 description 1
- 229940072082 magnesium salicylate Drugs 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 229940057948 magnesium stearate Drugs 0.000 description 1
- 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
- XDKQUSKHRIUJEO-UHFFFAOYSA-N magnesium;ethanolate Chemical compound [Mg+2].CC[O-].CC[O-] XDKQUSKHRIUJEO-UHFFFAOYSA-N 0.000 description 1
- CRGZYKWWYNQGEC-UHFFFAOYSA-N magnesium;methanolate Chemical compound [Mg+2].[O-]C.[O-]C CRGZYKWWYNQGEC-UHFFFAOYSA-N 0.000 description 1
- DMRBHZWQMKSQGR-UHFFFAOYSA-L magnesium;tetradecanoate Chemical compound [Mg+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O DMRBHZWQMKSQGR-UHFFFAOYSA-L 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
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- 239000001923 methylcellulose Substances 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 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
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000003068 static effect Effects 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
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 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
- 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
- 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 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 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
- 229960004418 trolamine Drugs 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
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Abstract
本发明以提供制造钛酸铝、钛酸铝镁等的钛酸铝系陶瓷的成形体时，可降低钛酸铝系陶瓷的成形体相对于原材料混合物的成形体的收缩率，降低所得的钛酸铝系陶瓷的成形体的热膨胀系数的方法为目的。本发明是将含钛源物质及铝源物质的原材料混合物进行烧成以制造钛酸铝系陶瓷的方法，其中前述铝源物质的BET比表面积为0.1m2/g以上5m2/g以下。
Description
技术领域
本发明涉及钛酸铝系陶瓷的制造方法。
背景技术
已知钛酸铝系陶瓷是含钛及铝作为构成元素，在X射线衍射光谱中具有钛酸铝的结晶花样的陶瓷，为耐热性优异的陶瓷。该钛酸铝系陶瓷一直以来作为构成如坩埚的烧成用具等的材料使用。另外，近年来作为构成捕捉柴油发动机所排出的废气中所含的微细的碳粒子用的陶瓷滤器的材料，产业上的利用价值升高。
作为该钛酸铝系陶瓷的制造方法，已知将混合二氧化钛等的成为钛源的化合物粉末及氧化铝等的成为铝源的化合物粉末所得的粉末状原材料混合物，进行烧成的方法（专利文献1）。
专利文献1：WO2005/105704号公报。
发明内容
然而，传统的方法，将原材料混合物的成形体烧成以得到陶瓷成形体时，有时陶瓷的成形体相对于原材料混合物的成形体的收缩率变大，所得陶瓷的热膨胀系数变大。
本发明提供将含钛源物质及铝源物质的原材料混合物进行烧成以制造钛酸铝系陶瓷的方法，其中前述铝源物质的BET比表面积为0.1m2/g以上，5m2/g以下。
前述铝源物质的BET比表面积以0.3m2/g以上3m2/g以下为优选。
本发明的方法中，将前述原材料混合物成形，得到原材料成形体，烧成所得的原材料成形体为优选。
另外，本发明中，换算为二氧化钛的钛源物质的使用量相对于合计100质量份的换算为二氧化钛的钛源物质的使用量及换算为氧化铝的铝源物质的使用量以30质量份以上，70质量份以下为优选，另外，钛源物质的BET比表面积以0.1m2/g以上，100m2/g以下为优选。
前述原材料混合物以进一步含镁源物质为优选，换算为氧化镁的镁源物质的使用量相对于合计100质量份的换算为二氧化钛的钛源物质的使用量及换算为氧化铝的铝源物质的使用量以0.1质量份以上，10质量份以下为优选。
前述原材料混合物以还含硅源物质为优选，前述硅源物质以长石或玻璃料为优选。另外，前述玻璃料的屈服点以700℃以上为优选。
本发明中，对前述原材料混合物，以进一步使用振动磨进行混合为优选，使用振动磨进行混合时，以使用粒径为1mm以上，100mm以下的氧化铝球或氧化锆球作为粉碎介质为优选。另外，前述振动磨以2mm以上，20mm以下的振幅振动为优选。
依据本发明的方法，将原材料混合物的成形体进行烧成以制造钛酸铝系陶瓷的成形体时，可降低钛酸铝系陶瓷的成形体相对于原材料混合物的成形体的收缩率，可降低所得的钛酸铝系陶瓷的成形体的热膨胀系数。
具体实施方式
本发明的方法中，使用含1种以上的钛源物质及1种以上的铝源物质的原材料混合物。前述的原材料混合物以进一步含1种以上的镁源物质及/或1种以上的硅源物质为优选。
本发明中所谓钛源物质是指含钛元素的物质，可举例如氧化钛。作为氧化钛，可举例如氧化钛（Ⅳ）、氧化钛（Ⅲ）、氧化钛（Ⅱ）等，以使用氧化钛（Ⅳ）为优选。氧化钛（Ⅳ）可为结晶，也可为非晶态。氧化钛（Ⅳ）为结晶时，可列举作为结晶型的锐钛矿型、金红石型、板钛矿型等，以锐钛矿型、金红石型为优选。
作为钛源物质，也可举例如可通过在空气中进行烧成衍生为二氧化钛（氧化钛）的物质。作为该物质，可举例如钛盐、烷氧基钛、氢氧化钛、氮化钛、硫化钛、钛等。
作为钛盐，具体可举例如三氯化钛、四氯化钛、硫化钛（Ⅳ）、硫化钛（Ⅵ）、硫酸钛（Ⅳ）等。作为烷氧基钛，具体可举例如乙氧基钛（Ⅳ）、甲氧基钛（Ⅳ）、叔丁氧基钛（Ⅳ）、异丁氧基钛（Ⅳ）、正丙氧基钛（Ⅳ）、四异丙氧基钛（Ⅳ）及其螯合化物等。
作为钛源物质，可举例如含钛与其他金属元素的复合氧化物。作为含钛与其他金属元素的复合氧化物，可举例如钛酸铝、钛酸铝镁等。
本发明使用的钛源物质的BET比表面积通常为0.1m2/g以上，100m2/g以下，以0.2m2/g以上，50m2/g以下为优选。钛源物质的表面也可被覆由氧化铝、二氧化硅、氧化锆、氢氧化铝等的无机酸构成的薄的表面层。
另外，钛源物质也可含原料来源或制造步骤中混入的不可避免的杂质。
本发明中所谓铝源物质，是指物质所含金属元素的实质上全部为铝的物质。但是也可含原料来源或制造步骤中混入的不可避免的杂质。作为铝源物质，可举例如氧化铝。氧化铝可为结晶，也可为非晶态。氧化铝为结晶时，可列举其结晶型为γ型、δ型、θ型、α型等。铝源物质以α型氧化铝为优选。
另外，作为铝源物质，也可列举可通过在空气中进行烧成衍生为氧化铝的物质，例如铝盐、烷氧基铝、氢氧化铝、金属铝等。
铝盐可为与无机酸的盐（无机盐），也可为与有机酸的盐（有机盐）。作为铝无机盐，具体可举例如硝酸铝、硝酸铵铝等的硝酸盐、碳酸铵铝等的碳酸盐等。作为铝有机盐，可举例如草酸铝、醋酸铝、硬脂酸铝、乳酸铝、月桂酸铝等。
作为烷氧基铝，可举例如异丙氧基铝、乙氧基铝、仲丁氧基铝、叔丁氧基铝等。
氢氧化铝可为结晶，也可为非晶态。氢氧化铝为结晶时，其结晶型可举例如水铝矿型、三羟铝石型、norstrandite型、勃姆石型、假勃姆石型等。作为非晶态的氢氧化铝，可举例如将铝盐、烷氧基铝等的水溶性铝化合物的水溶液水解所得的铝水解物。
其中，适合的铝源物质是氧化铝、氢氧化铝。
本发明使用的铝源物质的BET比表面积为0.1m2/g以上，5m2/g以下，以0.3m2/g以上，3m2/g以下为优选，以0.4m2/g以上，2m2/g以下为更优选。若BET比表面积小时，钛酸铝化的反应时，与钛源物质的反应不足，所以有反应性降低的趋势。另一方面，BET比表面积过大时，粒子间空隙率变大，其结果是原材料混合物的体积变大，钛酸铝化时，进行烧成而消灭空隙，所以收缩率增加。收缩率大时，在烧成后的钛酸铝系陶瓷成形体上除了容易发生破裂或裂纹之外，尺寸精度变差。本发明中所谓的收缩率是指烧成前的原材料成形体与烧成后的钛酸铝系陶瓷成形体的尺寸变化率，由后述实施例详述的方法所算出。
通过晶析制作铝源物质时（例如氢氧化铝），铝源物质的比表面积是通过控制晶析条件（制作铝为过饱和状态的水溶液（以下称为过饱和水溶液）用的溶剂及溶质的种类、过饱和水溶液中的铝浓度、已添加种子的过饱和水溶液中的种子浓度、使铝源物质结晶析出时的反应温度及反应时间等）而可调整。例如，通常作为铝源物质的氢氧化铝虽可通过バイヤー法而合成，但比表面积特别小的氢氧化铝是可通过添加作为种子的平均二次粒径为1μm以上，70μm以下的氢氧化铝至铝的过饱和水溶液而得。过饱和水溶液中，铝浓度换算为氧化铝以50g/L以下为优选。另外，为使过饱和水溶液中铝浓度为50g/L以下，以提高过饱和水溶液的液温为优选，以50℃以上至沸点以下为优选。已添加种子的过饱和水溶液中，种子浓度以低为优选，但以在10g/L以上，300g/L以下为优选。另外，通过烧成而得铝源物质时（例如氧化铝），铝源物质的比表面积是通过控制烧成前原料的BET比表面积或烧成温度而可调整，通常烧成温度愈高，铝源物质的比表面积愈小。另外，通过控制最终调整粒度时的粉碎条件，可调整铝源物质的比表面积，可通过形成弱粉碎条件以减小铝源物质的比表面积。
另外，就反应性的观点，铝源物质的二次粒径以10μm以上，100μm以下为优选，以20μm以上，70μm以下为更优选。
钛源物质及铝源物质的使用量基于换算成二氧化钛[TiO2]及氧化铝[Al2O3]的结果所决定。相对于100质量份的换算为二氧化钛的钛源物质的使用量及换算为氧化铝的铝源物质的使用量的合计量（以下称为总二氧化钛·氧化铝量），换算为二氧化钛的钛源物质的使用量通常为30质量份以上，70质量份以下，以40质量份以上，60质量份以下为优选。换算为氧化铝的铝源物质的使用量通常为30质量份以上，70质量份以下，以40质量份以上，60质量份以下为优选。
本发明中所谓镁源物质是指含镁元素的物质。作为镁源物质，可举例如氧化镁。作为镁源物质，也可举例如可通过在空气中进行烧成而衍生为氧化镁的物质。作为可通过在空气中进行烧成而衍生为氧化镁的物质，可举例如镁盐、烷氧基镁、氢氧化镁、氮化镁、金属镁等。
作为镁盐，具体可举例如氯化镁、高氯酸镁、磷酸镁、焦磷酸镁、草酸镁、硝酸镁、碳酸镁、醋酸镁、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。
作为烷氧基镁，具体可举例如甲氧基镁、乙氧基镁等。
作为镁源物质也可使用含镁与其他金属元素的物质。作为这种物质，可举例如镁氧尖晶石[MgAl2O4]或钛酸铝镁。
另外，镁源物质也可含原料来源或制造步骤中混入的不可避免的杂质。
前述原材料混合物进一步含镁源物质时，以氧化镁[MgO]换算的镁源物质的使用量是每100质量份的总二氧化钛·氧化铝量通常为0.1质量份以上，10质量份以下，以8质量份以下为优选。
所谓硅源物质是指含硅元素的物质。作为硅源物质，可举例如二氧化硅、一氧化硅等的氧化硅。另外，通过在空气中进行烧成可衍生为氧化硅的物质也可作为硅源物质使用。作为该物质，可举例如硅酸、碳化硅、氮化硅、硫化硅、四氯化硅、醋酸硅、硅酸钠、原硅酸钠、长石、含硅及铝的复合氧化物、玻璃料等。就工业上容易取得而言，以长石、玻璃料等为优选。使用玻璃料作为硅源物质时，从提高所制造的钛酸铝系陶瓷的耐热分解性的观点，以使用屈服点为700℃以上的玻璃料为优选。
每100质量份的总二氧化钛·氧化铝量，换算为氧化硅的硅源物质的使用量以0.1质量份以上，20质量份以下为优选，以1质量份以上，10质量份以下为更优选。
本发明的方法中，可通过混合前述钛源物质及前述铝源物质而得原材料混合物。本发明的方法中，以通过混合前述钛源物质、前述铝源物质、前述镁源物质及/或硅源物质而得原材料混合物为优选。
混合时，可使用通常所使用的混合机，例如可使用如诺塔混合机、Lodige混合机的搅拌混合机、如快速搅拌器等的气体混合机、球磨机、振动磨等。混合方法可为干式混合、湿式混合中任一种。
为了干式气氛下进行混合，例如混合钛源物质、铝源物质等的原材料，不使分散在液体溶剂中，在粉碎容器内搅拌即可，通常是在粉碎介质共存下在粉碎容器内进行搅拌。
作为粉碎容器，通常是使用不锈钢等的金属材料所构成的容器，也可在内表面被覆氟树脂、硅树脂、聚氨酯树脂等。粉碎容器的内容积相对于原材料混合物及粉碎介质的合计容积，通常为1体积倍以上，4体积倍以下，以1.2体积倍以上，3体积倍以下为优选。
作为粉碎介质，可举例如粒径为1mm以上，100 mm以下，以5mm以上，50 mm以下为优选的氧化铝球、氧化锆球等。粉碎介质的使用量相对于原材料混合物的使用量，通常为1质量倍以上，1000质量倍以下，以5质量倍以上，100质量倍以下为优选。
粉碎是例如加入原材料混合物及粉碎介质至粉碎容器内后，通过使粉碎容器振动、旋转或二者均有来进行。通过使粉碎容器振动或旋转，一同搅拌、混合原材料混合物及粉碎介质，同时进行粉碎。为使粉碎容器振动或旋转，可使用例如振动磨、球磨机、行星式磨机、针磨机（pin mill）等的高速旋转粉碎机等的通常的粉碎机，以工业规模容易实施而言，以使用振动磨为优选。使粉碎容器振动时，其振幅通常为2mm以上，20 mm以下，以12 mm以下为优选。粉碎可连续式进行，也可以批次式进行，但就工业规模容易实施而言，以连续式进行为优选。粉碎需要的时间通常为1分钟以上，6小时以下，以1.5分钟以上，2小时以下为优选。
干式粉碎原材料混合物时，也可加入粉碎助剂、解胶剂等的1种以上的添加剂。作为粉碎助剂，可举例如甲醇、乙醇、丙醇等的醇类、丙二醇、聚丙二醇、乙二醇等的二醇类、三乙醇胺等的胺类、棕榈酸、硬脂酸、油酸等的高级脂肪酸类、碳黑、石墨等的碳材料等。
使用添加剂时，其合计使用量是每100质量份的原材料混合物使用量，通常为0.1质量份以上，10质量份以下，以0.5质量份以上，5质量份以下为优选，进而以0.75质量份以上，2质量份以下为更优选。
另一方面，湿式混合时，例如可混合这些原材料混合物，使其分散在液体溶剂中进行。混合在通常的液体溶剂中仅进行搅拌处理即可，也可在粉碎介质共存下在粉碎容器内进行搅拌。
粉碎容器可使用与干式混合用容器相同的容器。粉碎容器的内容积相对于原材料混合物、粉碎介质、及液体溶剂的合计容积，通常为1体积倍以上，4体积倍以下，以1.2体积倍以上，3体积倍以下为优选。
作为湿式混合的溶剂，可使用水、离子交换水、甲醇、乙醇、丁醇、丙醇等的一元醇类、或丙二醇、聚丙二醇、乙二醇等的二元醇类等的有机溶剂。其中，因杂质少，以离子交换水为优选。溶剂的使用量是相对于100质量份的前述原材料混合物量，通常为20质量份以上，1000质量份以下，以30质量份以上，300质量份以下为优选。
作为粉碎介质，可使用与干式混合时相同的粉碎介质，其使用量是相对于原材料混合物的使用量，通常为1质量倍以上，1000质量倍以下，以5质量倍以上，100质量倍以下为优选。
将原材料混合物以湿式粉碎时，也可添加粉碎助剂，粉碎是例如加入原材料混合物、粉碎介质、液体溶剂、及粉碎助剂至粉碎容器内后，通过使粉碎容器振动、旋转或二者均有来进行。通过使粉碎容器振动或旋转，一同搅拌、混合原材料混合物及粉碎介质，同时进行粉碎。粉碎容器可使用与干式粉碎相同的容器，粉碎条件（粉碎容器的振幅、粉碎需要的时间等）可与干式粉碎相同。
湿式混合时，也可添加分散剂至溶剂。作为分散剂，可举例如硝酸、盐酸、硫酸等的无机酸、草酸、柠檬酸、醋酸、苹果酸、乳酸等的有机酸、甲醇、乙醇、丙醇等的醇类、聚羧酸铵等的表面活性剂等。使用分散剂时，其使用量是每100质量份的溶剂，通常为0.1质量份以上，20质量份以下，以0.2质量份以上，10质量份以下为优选。
混合后，通过除去（例如馏去）溶剂，可得到均匀混合的原材料混合物。
除去溶剂时，不局限温度、压力条件，可将原材料混合物在室温风干，也可真空干燥，也可加热干燥。另外，也不局限干燥条件，可静置干燥，也可流动干燥。加热干燥时的温度虽无特别规定，但通常为50℃以上，250℃以下。加热干燥时可使用的机器，可举例如柜式干燥机、淤浆干燥机、喷雾干燥机等。
另外，湿式混合时，有时根据所使用的铝源物质等的原材料混合物的种类，溶解在溶剂中，但溶解在溶剂中的铝源物质等的原材料混合物通过馏去溶剂，再次成为固体物而析出。
所得的粉末状的原材料混合物也可成形成原材料成形体。成形后进行烧成，由此可抑制烧成中成形体收缩，可防止成形体破裂。作为成形用的成形机，可举例如单轴压机、挤出成形机（单轴挤出成形机等）、压片机、造粒机等。
将原材料混合物成形，得到原材料成形体时，可添加成孔剂、粘结剂、润滑剂或增塑剂、分散剂、溶剂等至原材料混合物。
作为成孔剂，可举例如石墨等的碳材料、聚乙烯、聚丙烯、聚甲基丙烯酸甲酯等的树脂类、淀粉、坚果壳、核桃壳、玉米等的植物系材料、冰、干冰等。
作为粘结剂，可举例如甲基纤维素、羧甲基纤维素、羧甲基纤维素钠等的纤维素类、聚乙烯醇等的醇类、木素磺酸盐等的盐、石蜡、微晶蜡等的蜡、EVA、聚乙烯、聚苯乙烯、液晶聚合物、工程塑料等的热塑性树脂等。另外，根据物质不同有时也担任成孔剂及粘结剂二者的功能。作为担任成孔剂及粘结剂二者功能的物质，可举例如成形时粒子彼此粘结，可使成形体保形，其后烧成时，该物质本身燃烧可形成孔隙的物质，具体可举例如聚乙烯等。
作为润滑剂，可举例如甘油等的醇系润滑剂、辛酸、月桂酸、棕榈酸、花生酸、油酸、硬脂酸等的高级脂肪酸、硬脂酸铝等的硬脂酸金属盐等。该润滑剂通常也作为增塑剂发挥功能。
溶剂通常可使用离子交换水、甲醇、乙醇等的醇类。
将前述原材料混合物或其成形体进行烧成，得到钛酸铝或钛酸铝镁等的钛酸铝系陶瓷的烧成体时，烧成温度通常为1300℃以上，以1400℃以上为优选。另一方面，为使所产生的钛酸铝系陶瓷的烧成体容易加工，烧成温度通常为1650℃以下，以1600℃以下为优选，以1550℃以下为更优选。至烧成温度的升温速度虽非特别限定，但通常为1℃/小时以上，500℃/小时以下，以2℃/小时以上，500℃/小时以下为优选。另外，烧成中途也可设有保持一定温度的过程。
烧成通常是在大气中进行，但依原材料混合物的成分或成分量比，可在氮气、氩气等的惰性气体中进行烧成，也可在如一氧化碳气体、氢气等的还原性气体中进行烧成。另外，也可降低烧成气氛中的水蒸气分压进行烧成。
烧成通常可使用管状电炉、箱形电炉、隧道窑、远红外线炉、微波加热炉、竖炉、反射炉、旋转炉、辊底炉等通常的烧成炉进行。烧成可以间歇式进行，也可连续式进行。另外，烧成可以静态式进行，也可以流动式进行。
烧成时间可以是前述混合物转变成钛酸铝系陶瓷所需的时间以上，虽依前述混合物的量、烧成炉的形式、烧成温度、烧成气氛等而异，但通常为10分钟以上，72小时以下。
这样一来，可得到钛酸铝系陶瓷的烧成体。
以本发明的制造方法所得的钛酸铝系陶瓷是在X射线衍射光谱中，含钛酸铝的结晶花样，除此之外也可含例如氧化硅、氧化铝、氧化钛等的结晶花样。钛酸铝系陶瓷是钛酸铝镁[Al2（1-x）MgxTi（1+x）O5]时，前述x值可根据换算为二氧化钛的钛源物质的使用量、换算为氧化铝的铝源物质的使用量、及换算为氧化镁的镁源物质的使用量而控制。前述x值为0.01以上，以0.01以上，0.7以下为优选，以0.02以上，0.5以下为更优选。
实施例
以下用实施例详细地说明本发明，但本发明不限于以下的实施例的方式。
另外，各实施例、比较例所得的钛酸铝系陶瓷中的钛酸铝化率（以下称为「AT化率」）通过求出粉末X射线衍射光谱中2θ=27.4°的位置上出现的峰[对应于氧化钛·金红石相（110）面]的积分强度（IT）及2θ=33.7°的位置上出现的峰[相当于钛酸铝相（230）面及钛酸铝镁相（230）面]的积分强度（IAT），由式（1）算出。
AT化率（%）=100×IAT/（IAT+ IT） …（1）
另外，各实施例、比较例所得的钛酸铝系陶瓷的粒子形状是通过扫描式电子显微镜[SEM]进行观察。
钛酸铝系陶瓷烧成体的热膨胀系数的值[K-1]是自实施例、比较例所得的烧成体切出试样，将其以200℃/h的速度升温至600℃。之后，使用热机械分析装置[TMA]（SII Technology（株）社制「TMA6300」），自室温以600℃/h的速度升温至1000℃，测定其间的热膨胀系数[K-1]。
钛酸铝系陶瓷的收缩率设烧成前的原材料成形体的直径为A0，厚度为H0，烧成后所得的烧成体的直径为A，厚度为H，由式（2）求出。
收缩率（%）=100×（（H- H0）+（A- A0））/2 …（2）
实施例、比较例中作为原材料物质使用的铝源物质的BET比表面积是指由BET 1点测定法求出的比表面积。另外，二次粒径是通过激光衍射式粒度分布测定装置[日机装社制Microtrac HRA（X-100）]，以体积基准作为累计百分率50%等效粒径（D50）计算。
实施例1
一同加入4810g的BET比表面积为15.2m2/g的氧化钛粉末[Dupont（株）制，「R-900」]、4093g的BET比表面积为0.6m2/g的二次粒径为43μm的α氧化铝粉末、405g的氧化镁粉末[宇部兴产（株）制，「UC-95S」]及693g的屈服点为852℃（目录值）的玻璃料[Takara Standard（株）制，「CF-0043M2」]与80kg的直径为15mm的氧化铝球至内容量为50L的氧化铝制粉碎容器。原料混合物的合计体积为10L。之后，将粉碎容器通过振动磨，以振幅为10mm，振动频率为1200次/分，功率为5.5kW，振动30分钟，由此一边粉碎粉碎容器内的原料混合物，一边进行混合。将3g的此原料混合物用单轴成形机，以0.3t/cm2的成形压力进行成形，得到直径约20mm（A0）及厚度约5mm（H0）的原材料成形体。将此原材料成形体，在大气中，通过箱型电炉，以升温速度为300℃/小时，升温至1450℃，保持该温度4小时而进行烧成。之后，放冷至室温，得到实施例1的陶瓷烧成体。另外，将原材料混合物以相同条件进行烧成，对于所得的烧成物，以粉末X射线衍射法求出衍射光谱时，AT化率为100%。另外，实施例1的陶瓷烧成体的收缩率及热膨胀率分别为8.6%、-0.72×10-6[K-1]，可实现低热膨胀率及低收缩率。另外，以[Al2(1-x)MgxTi(1+x)O5]表示所得的钛酸铝镁时的x值为0.20。
比较例1
除了使用BET比表面积为6.2m2/g的α氧化铝粉末[住友化学（株）制，「AES-12」]以取代实施例1使用的α氧化铝粉末以外，以与实施例1相同条件得到比较例1的陶瓷烧成体。以粉末X射线衍射法求出衍射光谱时，AT化率为100%。另外，比较例1的陶瓷烧成体的收缩率及热膨胀率分别为11.4%、-0.14×10-6[K-1]，收缩率变大。另外，上述x值为0.20。
产业实用性
本发明的制造方法所得的钛酸铝或钛酸铝镁等的钛酸铝系陶瓷可使用于产业上各种用途。作为用途可举例如坩埚、耐火架子、烧箱、炉材等的烧成炉用具、柴油发动机、汽油发动机等内燃机的排气净化所使用的滤器或催化剂载体、啤酒等的食品过滤用滤器、使石油精制时产生的气体成分、一氧化碳、二氧化碳、氮、氧等选择性地透过用的选择透过滤器等所使用的陶瓷滤器、基板、电容器等的电子部件等。
Claims (13)
1. 一种方法，是将含钛源物质及铝源物质的原材料混合物进行锻烧以制造钛酸铝系陶瓷的方法，其特征在于前述铝源物质的BET比表面积为0.1m2/g以上至5m2/g以下。
2. 如权利要求1的方法，其中前述铝源物质的BET比表面积为0.3m2/g以上至3m2/g以下。
3. 如权利要求1或2的方法，其中将前述原材料混合物成形，得到原材料成形体，并锻烧所得的原材料成形体。
4. 如权利要求1至3中任一项的方法，其中相对于合计100质量份换算为二氧化钛的钛源物质的使用量以及换算为氧化铝的铝源物质的使用量，换算为二氧化钛的钛源物质的使用量为30质量份以上至70质量份以下。
5. 如权利要求1至4中任一项的方法，其中前述钛源物质的BET比表面积为0.1m2/g以上至100m2/g以下。
6. 如权利要求1至5中任一项的方法，其中前述原材料混合物还含镁源物质。
7. 如权利要求6的方法，其中相对于合计100质量份换算为二氧化钛的钛源物质的使用量以及换算为氧化铝的铝源物质的使用量，换算为氧化镁的镁源物质的使用量为0.1质量份以上至10质量份以下。
8. 如权利要求1至7中任一项的方法，其中前述原材料混合物还含硅源物质。
9. 如权利要求8的方法，其中前述硅源物质是长石或玻璃料。
10. 如权利要求9的方法，其中前述玻璃料的屈服点为700℃以上。
11. 如权利要求1至10中任一项的方法，其中对前述原材料混合物进一步进行使用振动磨的混合。
12. 如权利要求11的方法，其中前述使用振动磨进行混合时，使用粒径为1mm以上至100mm以下的氧化铝球或氧化锆球作为粉碎介质。
13. 如权利要求11或12的方法，其中前述振动磨以2mm以上至20mm以下的振幅振动。
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| CN112979307A (zh) * | 2021-04-06 | 2021-06-18 | 济南大学 | 钛酸铝陶瓷前体料和钛酸铝致密陶瓷及其制造方法 |
Also Published As
| Publication number | Publication date |
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| US20110156323A1 (en) | 2011-06-30 |
| EP2322492A4 (en) | 2011-10-05 |
| JP2010138060A (ja) | 2010-06-24 |
| WO2010026982A1 (ja) | 2010-03-11 |
| KR20110053313A (ko) | 2011-05-20 |
| TW201026631A (en) | 2010-07-16 |
| EP2322492A1 (en) | 2011-05-18 |
| JP4929327B2 (ja) | 2012-05-09 |
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