JP5485765B2 - チタン酸アルミニウム系セラミックス体の製造方法 - Google Patents
チタン酸アルミニウム系セラミックス体の製造方法 Download PDFInfo
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- JP5485765B2 JP5485765B2 JP2010078002A JP2010078002A JP5485765B2 JP 5485765 B2 JP5485765 B2 JP 5485765B2 JP 2010078002 A JP2010078002 A JP 2010078002A JP 2010078002 A JP2010078002 A JP 2010078002A JP 5485765 B2 JP5485765 B2 JP 5485765B2
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- raw material
- powder
- aluminum titanate
- aluminum
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- 239000000919 ceramic Substances 0.000 title claims description 134
- 229910000505 Al2TiO5 Inorganic materials 0.000 title claims description 132
- 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 description 132
- 238000004519 manufacturing process Methods 0.000 title claims description 67
- 239000000843 powder Substances 0.000 claims description 218
- 239000002994 raw material Substances 0.000 claims description 142
- 239000004927 clay Substances 0.000 claims description 72
- 238000010304 firing Methods 0.000 claims description 64
- 239000000203 mixture Substances 0.000 claims description 61
- 239000010936 titanium Substances 0.000 claims description 59
- 239000011777 magnesium Substances 0.000 claims description 54
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 53
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 53
- 229910052782 aluminium Inorganic materials 0.000 claims description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 47
- 239000010703 silicon Substances 0.000 claims description 47
- 229910052710 silicon Inorganic materials 0.000 claims description 47
- 229910052719 titanium Inorganic materials 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 229910052749 magnesium Inorganic materials 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 42
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000011521 glass Substances 0.000 claims description 24
- 239000011230 binding agent Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 19
- 239000000314 lubricant Substances 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 239000012634 fragment Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 238000004898 kneading Methods 0.000 claims description 9
- 239000010433 feldspar Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 64
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 45
- 229940091250 magnesium supplement Drugs 0.000 description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 29
- 235000010215 titanium dioxide Nutrition 0.000 description 26
- 239000000395 magnesium oxide Substances 0.000 description 20
- 229910010413 TiO 2 Inorganic materials 0.000 description 18
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000000126 substance Substances 0.000 description 16
- 238000005238 degreasing Methods 0.000 description 15
- 239000000654 additive Substances 0.000 description 14
- 239000013078 crystal Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 13
- -1 polyethylene Polymers 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 11
- 229910004298 SiO 2 Inorganic materials 0.000 description 10
- 238000001125 extrusion Methods 0.000 description 8
- 238000005979 thermal decomposition reaction Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 238000013001 point bending Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 230000002950 deficient Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000010010 raising Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 150000005215 alkyl ethers Chemical class 0.000 description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 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
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229920000609 methyl cellulose Polymers 0.000 description 3
- 239000001923 methylcellulose Substances 0.000 description 3
- 235000010981 methylcellulose Nutrition 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000000930 thermomechanical effect Effects 0.000 description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 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
- 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
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 2
- 239000004698 Polyethylene 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
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 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
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 2
- 229940063655 aluminum stearate Drugs 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-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
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 239000004570 mortar (masonry) Substances 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
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920001592 potato starch Polymers 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 229960004274 stearic acid Drugs 0.000 description 2
- RCYJPSGNXVLIBO-UHFFFAOYSA-N sulfanylidenetitanium Chemical compound [S].[Ti] RCYJPSGNXVLIBO-UHFFFAOYSA-N 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-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
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-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
- SDTMFDGELKWGFT-UHFFFAOYSA-N 2-methylpropan-2-olate Chemical compound CC(C)(C)[O-] SDTMFDGELKWGFT-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
- RVDLHGSZWAELAU-UHFFFAOYSA-N 5-tert-butylthiophene-2-carbonyl chloride Chemical compound CC(C)(C)C1=CC=C(C(Cl)=O)S1 RVDLHGSZWAELAU-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 229920001732 Lignosulfonate 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
- 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
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 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
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002472 Starch Polymers 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
- 235000011054 acetic acid 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
- 239000000783 alginic acid Substances 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 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
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- IOGARICUVYSYGI-UHFFFAOYSA-K azanium (4-oxo-1,3,2-dioxalumetan-2-yl) carbonate Chemical compound [NH4+].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O IOGARICUVYSYGI-UHFFFAOYSA-K 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 235000015165 citric acid Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids 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
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- FZFYOUJTOSBFPQ-UHFFFAOYSA-M dipotassium;hydroxide Chemical compound [OH-].[K+].[K+] FZFYOUJTOSBFPQ-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010332 dry classification Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000010354 integration Effects 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
- 238000007561 laser diffraction method Methods 0.000 description 1
- 229940033355 lauric acid Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 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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- 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
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
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- 239000001755 magnesium gluconate Substances 0.000 description 1
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- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 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
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- 229960004658 magnesium lactate Drugs 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
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 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
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 229960003390 magnesium sulfate Drugs 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- IAKLPCRFBAZVRW-XRDLMGPZSA-L magnesium;(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanoate;hydrate Chemical compound O.[Mg+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O IAKLPCRFBAZVRW-XRDLMGPZSA-L 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
- 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
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- YQXQWFASZYSARF-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC YQXQWFASZYSARF-UHFFFAOYSA-N 0.000 description 1
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- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000014571 nuts Nutrition 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 229960002969 oleic acid Drugs 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 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 1
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- 229920000642 polymer Polymers 0.000 description 1
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- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002459 porosimetry Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- IKNCGYCHMGNBCP-UHFFFAOYSA-N propan-1-olate Chemical compound CCC[O-] IKNCGYCHMGNBCP-UHFFFAOYSA-N 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000005368 silicate glass 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
- 229910052814 silicon oxide Inorganic materials 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
- 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
- 238000005245 sintering Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 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
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 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
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-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
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 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
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
- MDDPTCUZZASZIQ-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] MDDPTCUZZASZIQ-UHFFFAOYSA-N 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 238000010333 wet classification Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
(i)上記未焼成の再生原料から直径1mm以下の粉砕物を得る工程、
(ii)該粉砕物と水とを含む再生粘土を調製する工程、
(iii)該再生粘土を成形して成形体を得る工程、および、
(iv)該成形体を焼成する工程。
(i)未焼成の再生原料から直径1mm以下の粉砕物を得る工程、
(ii)該粉砕物と水とを含む再生粘土を調製する工程、
(iii)該再生粘土を成形して成形体を得る工程、および、
(iv)該成形体を焼成する工程。
(i)粉砕工程
本工程において、未焼成の再生原料から直径1mm以下の粉砕物を得る。このように適切に粒度調整がなされた未焼成物を再生原料として用いることにより、粘土に戻しやすくなり、均一な再生粘土の調製が容易になるため、効率的にチタン酸アルミニウム系セラミックス体を製造できるとともに、機械的強度および低熱膨張性、耐熱性等の熱特性に優れるチタン酸アルミニウム系セラミックス体を得ることが可能となる。本発明において直径とは粉砕物の短径を意味し、例えば後述するように篩別する場合は目開き1mmの篩をパスするものを意味する。
本工程において、上記工程(i)で得られた直径1mm以下の粉砕物と水とを含む再生粘土を調製する。再生粘土は、該粉砕物に、必要に応じて水を加え、混練することにより得ることができる。たとえば、該粉砕物が、「回収対象の製造工程」における原料の成形時や成形体の形状調整時に生じた不良成形体およびその破片などの再生原料から得られたものである場合には、水を添加することなく、あるいは少量の水の添加のみで再生粘土を調製することができる。また、該粉砕物が、水分量が5質量%以下となるように150℃未満の温度範囲で熱処理された再生原料から得られたものである場合には、基本的に、該粉砕物に水のみを加えることによって(バインダー、潤滑剤、造孔剤等の添加剤を新たに加えることなく)、再生粘土を調製することができる。混練には通常用いられる混練機を用いることができる。
式(A)中、N10はAl2O3の式量を表し、x10はアルミナ〔Al2O3〕換算のアルミニウム源粉末のモル量を表す。アルミナ〔Al2O3〕換算のアルミニウム源粉末のモル量x10は、下記式(A−1)により求められる。
式(A−1)中、w1はアルミニウム源粉末の使用量(g)を表し、M1はアルミニウム源粉末1モル中のアルミニウムのモル数を表し、N1は使用したアルミニウム源粉末の式量を表す。本発明において2種以上のアルミニウム源粉末を使用する場合、式(A−1)によって各アルミニウム源粉末のアルミナ〔Al2O3〕換算のモル量を求め、各モル量を合計することによって、使用するアルミニウム源粉末のアルミナ〔Al2O3〕換算のモル量を求めることができる。
式(B)中、N20はTiO2の式量を表し、x20はチタニア〔TiO2〕換算のチタニウム源粉末のモル量を表す。チタニア〔TiO2〕換算のチタニウム源粉末のモル量x20は、下記式(B−1)により求められる。
式(B−1)中、w2はチタニウム源粉末の使用量(g)を表し、M2はチタニウム源粉末1モル中のチタニウムのモル数を表し、N2は使用したチタニウム源粉末の式量を表す。本発明において2種以上のチタニウム源粉末を使用する場合、式(B−1)によって各チタニウム源粉末のチタニア〔TiO2〕換算のモル量を求め、各モル量を合計することによって、使用するチタニウム源粉末のチタニア〔TiO2〕換算のモル量を求めることができる。
式(C)中、N30はMgOの式量を表し、x30はマグネシア〔MgO〕換算のマグネシウム源粉末のモル量を表す。マグネシア〔MgO〕換算のマグネシウム源粉末のモル量x30は、下記式(C−1)により求められる。
式(C−1)中、w3はマグネシウム源粉末の使用量(g)を表し、M3はマグネシウム源粉末1モル中のマグネシウムのモル数を表し、N3は使用したマグネシウム源粉末の式量を表す。本発明において2種以上のマグネシウム源粉末を使用する場合、式(C−1)によって各マグネシウム源粉末のマグネシア〔MgO〕換算のモル量を求め、各モル量を合計することによって、使用するマグネシウム源粉末のマグネシア〔MgO〕換算のモル量を求めることができる。
式(D)中、N40はSiO2の式量を表し、x40はシリカ〔SiO2〕換算のケイ素源粉末のモル量を表す。シリカ〔SiO2〕換算のケイ素源粉末のモル量x40は、下記式(D−1)により求められる。
式(D−1)中、w4はケイ素源粉末の使用量(g)を表し、M4はケイ素源粉末1モル中のケイ素のモル数を表し、N4は使用したケイ素源粉末の式量を表す。本発明において2種以上のケイ素源粉末を使用する場合、式(D−1)によって各ケイ素源粉末のシリカ〔SiO2〕換算のモル量を求め、各モル量を合計することによって、使用するケイ素源粉末のシリカ〔SiO2〕換算のモル量を求めることができる。
本工程において、上記再生粘土を成形して、成形体を得る。成形体の形状は特に制限されないが、たとえば、ハニカム形状、棒状、チューブ状、板状、るつぼ形状等を挙げることができる。なかでも、得られるチタン酸アルミニウム系セラミックス体をDPF等のセラミックスフィルタに適用する場合には、ハニカム形状とすることが好ましい。再生粘土の成形に用いる成形機としては、一軸プレス、押出成形機、打錠機、造粒機などが挙げられる。
本工程において、上記再生粘土の成形体を焼成し、チタン酸アルミニウム系セラミックス体を得る。成形体の焼成における焼成温度は、通常、1300℃以上、好ましくは1400℃以上である。また、焼成温度は、通常、1650℃未満、好ましくは1550℃以下である。焼成温度までの昇温速度は特に限定されるものではないが、通常、1℃/時間〜500℃/時間である。再生粘土が新原料のケイ素源粉末や、粉砕物および/または新原料のチタン酸アルミニウム系セラミックス粉末が含有するケイ素元素に由来するケイ素分を含む場合には、焼成工程の前に、1100〜1300℃の温度範囲で3時間以上保持する工程を設けることが好ましい。これにより、チタン酸アルミニウム系セラミックス体中でのケイ素分の融解、拡散を促進させることができる。
チタン酸アルミニウム系セラミックス体を、押出成形時の押出方向に長さ50mm、幅5mm、厚さ5mmの直方体形状に切り出す。この切り出したセラミックス体の外表面を紙やすり(#1500)を用いて、目視で凹凸がなくなるまで研磨する。得られるサンプルの三点曲げ強度を、JIS R 1601に準拠した方法により測定する。
チタン酸アルミニウム化率(AT化率)は、乳鉢にて解砕したチタン酸アルミニウム系セラミックス体について測定した粉末X線回折スペクトルにおける2θ=27.4°の位置に現れるピーク〔チタニア・ルチル相(110)面に帰属される〕の積分強度(IT)と、2θ=33.7°の位置に現れるピーク〔チタン酸アルミニウムマグネシウム相(230)面に帰属される〕の積分強度(IAT)とから、下記式:
AT化率=IAT/(IT+IAT)×100(%)
により算出する。
チタン酸アルミニウム系セラミックス体を解砕して粉末とし、アルミナルツボに入れ、箱型電気炉にて1100℃で48時間保持することによって、熱分解評価用チタン酸アルミニウム系セラミックスを得た。得られた熱分解評価用チタン酸アルミニウム系セラミックスの粉末X線回折スペクトル(XRD)における、2θ=27.4°の位置に現れるピーク〔チタニア・ルチル相(110)面に帰属される〕の積分強度(IT2)と、2θ=33.7°の位置に現れるピーク〔チタン酸アルミニウム相(230)面およびチタン酸アルミニウムマグネシウム相(230)面に帰属される〕の積分強度(IAT2)を求め、下記式:
熱分解率(%)=100−100×(IAT2)/(IAT2+IT2)
により熱分解率を算出する。
チタン酸アルミニウム系セラミックス体を、押出成形時の押出方向に長さ50mm、幅5mm、厚さ5mmの直方体形状に切り出し、さらに長さ12mmの平行端面となるように正確に切り出す。ついで、この試験片に対して、200℃/hの昇温速度で1000℃まで昇温し、切り出し作業に用いた固定用樹脂を焼失させ、室温(25℃)まで冷却する。熱処理を施した試験片について、熱機械的分析装置(SIIテクノロジー(株)製 TMA6300)を用いて、室温(25℃)から1000℃まで600℃/hで昇温させた際の試験片の膨張率から、下記式に基づき、熱膨張係数〔K-1〕を算出する。
ここで、試験片の膨張率とは、
(1000℃まで昇温させたときの試験片の押出方向の長さ−昇温前(25℃)における試験片の押出方向の長さ)/(昇温前(25℃)における試験片の押出方向の長さ)
を意味する。
JIS R1634に準拠した、水中浸漬によるアルキメデス法により、チタン酸アルミニウム系セラミックス体の水中重量M2(g)、飽水重量M3(g)および乾燥重量M1(g)を測定し、下記式:
開気孔率(%)=100×(M3−M1)/(M3−M2)
により開気孔率を算出する。
0.4gのチタン酸アルミニウム系セラミックス体を砕き、得られる約2mm角の小片を、120℃で4時間、空気中で、乾燥させた後、水銀圧入法により、細孔半径測定範囲0.001〜100.0μmまで測定する。細孔容積基準でみたときの最大頻度を示す細孔半径を2倍した値を細孔径(モード径)とする。測定装置には、Micromeritics社製の「オートポアIII9420」を用いる。
原料粉末の平均粒子径〔体積基準の累積百分率50%相当粒子径(D50)〕は、レーザ回折式粒度分布測定装置〔日機装社製「Microtrac HRA(X−100)」〕を用いて測定する。
試料(粉砕した熱処理品)約5gをガラス容器に計り採り、該試料の初期質量(W0)を計測する。次に、ガラス容器ごと110℃で2時間熱処理した後、室温まで冷却する。冷却後の試料の質量(W1)を計測し、下記式:
水分量(質量%)=100×(W0−W1)/W0
により水分量を算出する。
試料(粉砕した熱処理品)をあらかじめ110℃で2時間熱処理し、得られた熱処理後の試料の約5gを白金容器に計り採り、該試料の初期質量(W2)を計測する。次に、白金容器ごと1100℃で2時間熱処理した後、室温まで冷却する。冷却後の試料の質量(W3)を計測し、下記式:
強熱減量(質量%)=100×(W2−W3)/W2
により強熱減量を算出する。
原料粉末として以下のものを用いる。下記の原料粉末の仕込み組成は、アルミナ〔Al2O3〕、チタニア〔TiO2〕、マグネシア〔MgO〕およびシリカ〔SiO2〕換算の質量比で、〔Al2O3〕/〔TiO2〕/〔MgO〕/〔SiO2〕=47%/47%/2%/4%である。
D50が29μmの酸化アルミニウム粉末(α−アルミナ粉末)
47質量部
(2)チタニウム源粉末
D50が0.5μmの酸化チタン粉末(ルチル型結晶)
47質量部
(3)マグネシウム源粉末
D50が2.5μmの酸化マグネシウム粉末
2質量部
(4)ケイ素源粉末
D50が5.4μmのガラスフリット(タカラスタンダード社製「CK0160M1」、SiO2分70%)
4質量部
上記アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびケイ素源粉末からなる混合物に、該混合物100質量部に対して、造孔剤として馬鈴薯でんぷんを14質量部、バインダーとしてメチルセルロースを9質量部、界面活性剤としてポリオキシアルキレンアルキルエーテルを5質量部、および潤滑剤としてグリセリンを0.5質量部加え、さらに、分散媒として水を32質量部加えた後、混練機を用いて混練することにより、成形用粘土を調製する。ついで、この成形用粘土を押出成形することにより、ハニカム形状の成形体を作製する。得られる成形体を、大気雰囲気下、120℃で5時間熱処理し、成形体の熱処理品を得る。この熱処理品の水分量は、5質量%以下である。
実施例1と同様にして、成形用粘土を押出成形することにより、ハニカム形状の成形体を作製する。得られる成形体を、大気雰囲気下、500℃で10時間熱処理し、成形体の熱処理品を得る。この熱処理品の強熱減量は、5質量%以下である。該熱処理品を直径2cm以下程度となるように粗砕し、さらにロールクラッシャー(ロール間隔2mm)を用いて粉砕を行なう。目開き1mmの篩を用いて篩別を行ない、篩下を回収して粉砕物を得る。
実施例1と同様にして、ハニカム形状の成形体を、大気雰囲気下、120℃で5時間熱処理し、成形体の熱処理品を得る。該熱処理品を直径2cm以下程度となるように粗砕し、さらにロールクラッシャー(ロール間隔2mm)を用いて粉砕を行なう。得られる粉砕物は、直径1mmを越える粒子を多く含む。
Claims (22)
- チタン酸アルミニウム系セラミックス体の製造工程において回収される、未焼成の再生原料を用いて、チタン酸アルミニウム系セラミックス体を製造する方法であって、
(i)前記未焼成の再生原料から直径1mm以下の粉砕物を得る工程と、
(ii)前記粉砕物と水とを含む再生粘土を調製する工程と、
(iii)前記再生粘土を成形して成形体を得る工程と、
(iv)前記成形体を焼成する工程と、
を含み、
前記直径1mm以下の粉砕物を得る工程(i)は、前記未焼成の再生原料を粉砕および/または分級する工程を含み、
前記分級は、篩別により行なわれ、
前記未焼成の再生原料または前記粉砕物は、1300℃未満の温度で熱処理されたものであり、
前記未焼成の再生原料は、アルミニウム源粉末、チタニウム源粉末、マグネシウム源粉末およびガラスフリットを含む、チタン酸アルミニウム系セラミックス体の製造方法。 - 前記未焼成の再生原料は、未焼成の成形体もしくはその破片、または焼成温度に至るまでの昇温を途中で停止した中間物である請求項1に記載の方法。
- 前記粉砕物の直径は、200μm以下である請求項1又は2に記載の方法。
- 前記未焼成の再生原料または前記粉砕物は、1体積%以上の酸素を含む雰囲気下または、1体積%以上の酸素を含む酸素含有ガスの気流下で熱処理されたものである請求項1〜3のいずれか1項に記載の方法。
- 前記未焼成の再生原料または前記粉砕物は、その水分量が5質量%以下となるように熱処理されたものである請求項1〜4のいずれか1項に記載の方法。
- 熱処理温度が150℃未満である請求項5に記載の方法。
- 前記再生粘土を調製する工程(ii)は、前記粉砕物に、少なくとも水を加えて混練する工程を含む請求項5または6に記載の方法。
- 前記未焼成の再生原料または前記粉砕物は、その強熱減量が5質量%以下となるように熱処理されたものである請求項1〜4のいずれか1項に記載の方法。
- 熱処理温度が300℃以上、1000℃未満である請求項8に記載の方法。
- 前記再生粘土を調製する工程(ii)は、前記粉砕物に、少なくとも水と、バインダー、潤滑剤および造孔剤からなる群から選択されるいずれか1種以上の成分とを加えて混練する工程を含む請求項8または9に記載の方法。
- 前記未焼成の再生原料は、チタン酸アルミニウム系セラミックスをさらに含む請求項1〜10のいずれか1項に記載の方法。
- 前記チタン酸アルミニウム系セラミックスは、マグネシウム元素を含む請求項11に記載の方法。
- 前記チタン酸アルミニウム系セラミックスは、ケイ素元素を含む請求項11または12に記載の方法。
- 前記再生粘土は、バインダー、潤滑剤および造孔剤からなる群から選択されるいずれか1種以上の成分をさらに含む請求項1〜13のいずれか1項に記載の方法。
- 前記再生粘土は、チタン酸アルミニウム系セラミックス粉末および/または焼成によりチタン酸アルミニウム系セラミックスに導かれる粉末混合物からなる新原料をさらに含む請求項1〜14のいずれか1項に記載の方法。
- 前記新原料を構成するチタン酸アルミニウム系セラミックス粉末は、マグネシウム元素を含む請求項15に記載の方法。
- 前記新原料を構成するチタン酸アルミニウム系セラミックス粉末は、ケイ素元素を含む請求項15または16に記載の方法。
- 前記新原料を構成する粉末混合物は、マグネシウム源粉末を含む請求項15に記載の方法。
- 前記新原料を構成する粉末混合物は、ケイ素源粉末を含む請求項15または16に記載の方法。
- 前記ケイ素源粉末は、長石あるいはガラスフリット、またはそれらの混合物からなる粉末である請求項19に記載の方法。
- 前記新原料を構成するチタン酸アルミニウム系セラミックス粉末および/または粉末混合物に含まれる粉末の平均粒子径は、100μm以下である請求項15〜20のいずれか1項に記載の方法。
- 前記成形体を焼成する工程(iv)における焼成温度は、1300℃以上1650℃未満である請求項1〜21のいずれか1項に記載の方法。
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