JP6407887B2 - 多孔質材料及び断熱膜 - Google Patents
多孔質材料及び断熱膜 Download PDFInfo
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- JP6407887B2 JP6407887B2 JP2015550914A JP2015550914A JP6407887B2 JP 6407887 B2 JP6407887 B2 JP 6407887B2 JP 2015550914 A JP2015550914 A JP 2015550914A JP 2015550914 A JP2015550914 A JP 2015550914A JP 6407887 B2 JP6407887 B2 JP 6407887B2
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- 239000011148 porous material Substances 0.000 title claims description 127
- 239000000463 material Substances 0.000 claims description 106
- 239000002245 particle Substances 0.000 claims description 105
- 238000009413 insulation Methods 0.000 claims description 23
- 239000011159 matrix material Substances 0.000 claims description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 14
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 description 17
- 239000002002 slurry Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 7
- 229910052753 mercury Inorganic materials 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 239000008199 coating composition Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010191 image analysis Methods 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 229920000592 inorganic polymer Polymers 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000004698 Polyethylene 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
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- SXQXMCWCWVCFPC-UHFFFAOYSA-N aluminum;potassium;dioxido(oxo)silane Chemical compound [Al+3].[K+].[O-][Si]([O-])=O.[O-][Si]([O-])=O SXQXMCWCWVCFPC-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000404 calcium aluminium silicate Substances 0.000 description 1
- 235000012215 calcium aluminium silicate Nutrition 0.000 description 1
- WNCYAPRTYDMSFP-UHFFFAOYSA-N calcium aluminosilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WNCYAPRTYDMSFP-UHFFFAOYSA-N 0.000 description 1
- 229940078583 calcium aluminosilicate Drugs 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910002078 fully stabilized zirconia Inorganic materials 0.000 description 1
- 229920000876 geopolymer Polymers 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920003257 polycarbosilane Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000002491 polymer binding agent Substances 0.000 description 1
- 229920001709 polysilazane Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920000734 polysilsesquioxane polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910000077 silane Inorganic materials 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
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/009—Porous or hollow ceramic granular materials, e.g. microballoons
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/02—Shape or form of insulating materials, with or without coverings integral with the insulating materials
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/02—Shape or form of insulating materials, with or without coverings integral with the insulating materials
- F16L59/028—Composition or method of fixing a thermally insulating material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/16—Pore diameter
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- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
Description
ZrO2粒子は、平均粒子径が10nm〜1μmであることが好ましく、10nm〜500nmであることが更に好ましく、10nm〜100nmであることが特に好ましい。上記平均粒子径は、小さいほど熱伝導率が低くなるために好ましいが、10nm未満であると製造コストが高くなるおそれがある。一方、1μm超であると、熱伝導率が高くなるおそれがある。なお、「ZrO2粒子の平均粒子径」は、以下のように測定した値である。TEMを用いた観察によって得た微構造の画像を用い、10個以上のZrO2粒子の粒子径を計測し、その平均値を算出した。また、ZrO2粒子は他の元素(例えば、Mg,Ca,Yなど)を固溶していてもよく、部分安定化ジルコニアや完全安定化ジルコニアであってもよい。
異種材料の含有割合は、0.1〜30体積%であることが好ましく、0.1〜20体積%であることが更に好ましく、0.1〜15体積%であることが特に好ましい。上記範囲内であることにより、ZrO2の特性を維持したまま、熱伝導率をさらに低減できるという利点がある。異種材料の含有割合が上記下限値未満であると、熱伝導率の低減効果が不十分であるおそれがある。上記上限値超であると、ZrO2の有する耐熱性や強度などの材料特性において不具合が生じるおそれがある。
本発明の多孔質材料の製造方法の一実施形態は、グリーンシート形成用スラリーを調製するスラリー調製工程と、グリーンシートを形成するグリーンシート形成工程と、焼成体を作製する焼成体作製工程と、焼成体を解砕して多孔質材料を得る解砕工程と、を有する。上記スラリー調製工程は、ZrO2粒子、異種材料、及び造孔材を含むグリーンシート形成用スラリーを調製する工程である。上記グリーンシート形成工程は、グリーンシート形成用スラリーを膜状に形成してグリーンシートを形成する工程である。上記焼成体作製工程は、形成したグリーンシートを焼成して膜状の焼成体を作製する工程である。上記解砕工程は、焼成体を解砕して多孔質材料を得る工程である。
グリーンシート形成用スラリーに含まれるZrO2粒子及び異種材料は、上述した本発明の多孔質材料のZrO2粒子及び異種材料と同様のものである。
グリーンシートは、焼成後の厚さが10〜50μmとなるような膜状であることが好ましい。
グリーンシートの焼成条件は、適宜設定することができるが、例えば、800〜2300℃で0.5〜20時間とすることが好ましく、800〜1800℃で5〜20時間であることが更に好ましく、800〜1300℃で5〜20時間であることが特に好ましい。
焼成体を解砕する方法としては、例えば、乾式ビーズミル、ローラーミルなどを用いて焼成体を室温で解砕することができる。特に、「アスペクト比が3以上の板状で、最小長が0.1〜50μmである」多孔質粒子を得るためには、気流式分級機を用い、整粒(分級)することが好ましい。
本発明の断熱膜は、本発明の多孔質材料を材料として含むものである。このような断熱膜は、断熱性能に優れている。
ZrO2原料(ZrO2粒子)であるジルコニア粉末に、異種材料としてSiO2、造孔材としてカーボンブラック、バインダーとしてポリビニルブチラール樹脂(PVB)、可塑剤としてフタル酸ジオクチル(DOP)、及び、溶剤としてキシレンと1−ブタノールを加えた。これを原料組成物とした。原料組成物中の各成分の添加量は、ジルコニア粉末10.8体積%、SiO21.2体積%、バインダー10.8体積%、可塑剤6体積%、溶剤71.2体積%であった。なお、表1中、各成分の「体積%」は、ZrO2粒子、異種材料、及び造孔材の合計に対する各成分の「体積%」を示している。
異種材料の含有割合は、多孔質材料を化学分析することにより得た。得られた分析結果をもとに、異種材料として添加した化合物(実施例1の場合はSiO2)に換算した含有量を体積%として算出した。
多孔質材料の熱伝導率は、以下のように測定する。まず、多孔質材料と同材料を別途、0.5mm×5mm×30mmに成形したものを焼成し、光交流法により熱拡散率を、同材料をDSC法により比熱を測定し、熱拡散率、比熱、密度(見かけ粒子密度)の積を多孔質材料の熱伝導率とした。見かけ粒子密度は、水銀を用いた液浸法により測定した。
多孔質材料の熱容量は、以下のように測定する。まず、多孔質材料と同材料を別途、0.5mm×5mm×30mmに成形したものを焼成し、DSC法により比熱を測定し、比熱、密度(見かけ粒子密度)の積を多孔質材料の熱容量とした。見かけ粒子密度は、水銀を用いた液浸法により測定した。
断熱膜の熱伝導率は、レーザーフラッシュ2層モデルにて断熱膜の厚さ方向に平行な断面における熱伝導率を測定した。断熱膜の熱容量は、断熱膜を粉砕した後、DSC法で比熱を測定し、比熱×密度(見かけ粒子密度)の積から算出した。
まず、実施例1と同様にして表1に示す条件で多孔質材料を得た。次に、実施例1と同様にして上記各測定を行った。結果を表1に示す。
Claims (8)
- 複数の細孔が形成された多孔質構造を有し、ZrO2粒子と、前記ZrO2粒子の表面に存在する異種材料と、を前記多孔質構造の骨格として有し、
前記異種材料が、第1群より選択される少なくとも一種、第2群より選択される少なくとも一種、または、前記第1群より選択される少なくとも一種と前記第2群より選択される少なくとも一種との両方、を含むものであり、
前記第1群が、SiO2、TiO2、La2O3、Al2O3、SrO、Gd2O3、Nb2O5、Y2O3、及び、これらの2種以上からなる複合酸化物からなる群であり、
前記第2群が、SiO2、TiO2、La2O3、Al2O3、SrO、Gd2O3、Nb2O5、Y2O3からなる群より選択される少なくとも一種とZrO2との複合酸化物からなる群であり、
前記異種材料の含有割合が、0.1〜15体積%であり、
前記異種材料は、少なくともZrO2粒子間に介在している多孔質材料。 - 前記異種材料が、SiO2、TiO2、La2O3、及びLa2Zr2O7からなる群より選択される少なくとも2種以上である請求項1に記載の多孔質材料。
- 前記異種材料の直径は、前記ZrO2粒子の直径よりも小さい請求項1または2に記載の多孔質材料。
- 前記異種材料の直径が、0.1〜300nmである請求項1〜3のいずれか一項に記載の多孔質材料。
- 熱伝導率が1W/mK以下である請求項1〜4のいずれか一項に記載の多孔質材料。
- 1mm以下の大きさの粒子状である請求項1〜5のいずれか一項に記載の多孔質材料。
- アスペクト比が3以上の板状で、最小長が0.1〜50μmである請求項1〜6のいずれか一項に記載の多孔質材料。
- 請求項1〜7のいずれか一項に記載の多孔質材料と、前記多孔質材料が分散されたマトリックスと、を有する断熱膜。
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