JP2016088819A - Powder, molded body thereof and packaged body - Google Patents
Powder, molded body thereof and packaged body Download PDFInfo
- Publication number
- JP2016088819A JP2016088819A JP2014227299A JP2014227299A JP2016088819A JP 2016088819 A JP2016088819 A JP 2016088819A JP 2014227299 A JP2014227299 A JP 2014227299A JP 2014227299 A JP2014227299 A JP 2014227299A JP 2016088819 A JP2016088819 A JP 2016088819A
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- JP
- Japan
- Prior art keywords
- powder
- particles
- mass
- silica
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 144
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 142
- 239000002245 particle Substances 0.000 claims abstract description 124
- 239000012784 inorganic fiber Substances 0.000 claims abstract description 91
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052742 iron Inorganic materials 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims description 54
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 44
- 239000011162 core material Substances 0.000 claims description 28
- 239000011810 insulating material Substances 0.000 claims description 26
- 230000006835 compression Effects 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 abstract description 41
- 238000013019 agitation Methods 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 34
- 239000000835 fiber Substances 0.000 description 34
- 238000000034 method Methods 0.000 description 34
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 26
- 238000003756 stirring Methods 0.000 description 20
- -1 is selected Substances 0.000 description 19
- 238000000465 moulding Methods 0.000 description 18
- 239000004744 fabric Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 16
- 238000002156 mixing Methods 0.000 description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000009413 insulation Methods 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 10
- 239000003365 glass fiber Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 239000011490 mineral wool Substances 0.000 description 9
- 239000005871 repellent Substances 0.000 description 9
- 230000002940 repellent Effects 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000011049 filling Methods 0.000 description 8
- 239000011888 foil Substances 0.000 description 8
- 238000012546 transfer Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000004745 nonwoven fabric Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 5
- 239000004917 carbon fiber Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 150000002484 inorganic compounds Chemical class 0.000 description 5
- 229910010272 inorganic material Inorganic materials 0.000 description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 229920002748 Basalt fiber Polymers 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 239000001993 wax Substances 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229960000892 attapulgite Drugs 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 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 3
- 239000008393 encapsulating agent Substances 0.000 description 3
- 229910021485 fumed silica Inorganic materials 0.000 description 3
- 239000011491 glass wool Substances 0.000 description 3
- 235000013980 iron oxide Nutrition 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910052625 palygorskite Inorganic materials 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229910021487 silica fume Inorganic materials 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 210000002268 wool Anatomy 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 239000002781 deodorant agent Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 229920006284 nylon film Polymers 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 2
- 229910052624 sepiolite Inorganic materials 0.000 description 2
- 235000019355 sepiolite Nutrition 0.000 description 2
- 238000009958 sewing Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 229910005438 FeTi Inorganic materials 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910021260 NaFe Inorganic materials 0.000 description 1
- 229910021314 NaFeO 2 Inorganic materials 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920006243 acrylic copolymer Polymers 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- BULLHNJGPPOUOX-UHFFFAOYSA-N chloroacetone Chemical compound CC(=O)CCl BULLHNJGPPOUOX-UHFFFAOYSA-N 0.000 description 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- 229940090961 chromium dioxide Drugs 0.000 description 1
- IAQWMWUKBQPOIY-UHFFFAOYSA-N chromium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Cr+4] IAQWMWUKBQPOIY-UHFFFAOYSA-N 0.000 description 1
- AYTAKQFHWFYBMA-UHFFFAOYSA-N chromium(IV) oxide Inorganic materials O=[Cr]=O AYTAKQFHWFYBMA-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- ORXJMBXYSGGCHG-UHFFFAOYSA-N dimethyl 2-methoxypropanedioate Chemical compound COC(=O)C(OC)C(=O)OC ORXJMBXYSGGCHG-UHFFFAOYSA-N 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 description 1
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- KEHCHOCBAJSEKS-UHFFFAOYSA-N iron(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Fe+2] KEHCHOCBAJSEKS-UHFFFAOYSA-N 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 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
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 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
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Silicon Compounds (AREA)
Abstract
Description
本発明は、粉体、その成形体及び被包体に関する。 The present invention relates to a powder, a molded body thereof, and an encapsulated body.
室温では、空気分子の平均自由行程は、約100nmである。そのため、直径100nm以下の空隙を有する多孔質体は、その中で空気による対流と伝導による伝熱とが抑制され、断熱作用を示す。 At room temperature, the mean free path of air molecules is about 100 nm. Therefore, a porous body having a void having a diameter of 100 nm or less suppresses convection by air and heat transfer by conduction, and exhibits a heat insulating action.
この断熱作用に従い、超微粒子を断熱材に用いることで、熱伝導率の低い断熱材が得られる。例えば、特許文献1に、シリカ及び/又はアルミナを含み、粒子径DSが5nm以上30nm以下である複数の小粒子を含んで成形されており、圧縮率0〜5%における最大荷重が0.7MPa以上であり、30℃における熱伝導率が0.05W/m・K以下である、断熱材とその製造方法が開示されている。 In accordance with this heat insulating action, a heat insulating material with low thermal conductivity can be obtained by using ultrafine particles for the heat insulating material. For example, Patent Document 1 is formed by including a plurality of small particles containing silica and / or alumina and having a particle diameter D S of 5 nm to 30 nm, and the maximum load at a compression rate of 0 to 5% is 0.00. A heat insulating material having a thermal conductivity of 30 MPa or more and 0.05 W / m · K or less and a method for producing the same are disclosed.
しかしながら、上記の断熱材を実用化しようとする場合には、熱伝導率以外も取扱性等の問題がある。まず、熱伝導率を制御する場合は、断熱材の構造のみを特定のものとすればよい。例えば、シリカのような熱伝導性が低い素材を選択し、粉体を作製し、さらに多孔質体として、その中の空隙が100nmより短くなるようにすれば、所望の熱伝導率が得られる。 However, when the above-described heat insulating material is to be put into practical use, there are problems such as handleability other than thermal conductivity. First, when controlling the thermal conductivity, only the structure of the heat insulating material may be specified. For example, if a material with low thermal conductivity, such as silica, is selected, powder is produced, and the porous body is made to have voids shorter than 100 nm, the desired thermal conductivity can be obtained. .
ただし、上記の粉体を、製造後一定時間保管する場合には、粉体の組成にばらつきが生じたり、粉体の自重によりかさ密度に分布が生じたりする。そうすると、施工前又は成形前に、再度の撹拌混合が必要となる。また、上記特許文献1に開示する粉体も、帯電しやすく、付着力が高くなるという問題がある。 However, when the above powder is stored for a certain period of time after manufacture, the composition of the powder varies, or the bulk density is distributed due to the weight of the powder. If it does so, before construction or before shaping | molding, another stirring and mixing will be needed. In addition, the powder disclosed in Patent Document 1 also has a problem that it is easily charged and has high adhesion.
さらに、上記特許文献1の粉体を成形してなる成形体、及びその焼成硬化体も、上記の粉体と同様に帯電しやすい。その成形体又は焼成硬化体が帯電すると、付着力が高くなり、それが原因で断熱材の表面が滑りやすくなる等の取扱性の問題と、被包体の製造の際に付着した粉体が外被材に付着しシール不良を起こし、歩留まりが低下したりする等の製造上の問題とを生じる。 Furthermore, the molded body formed by molding the powder of Patent Document 1 and the fired and cured body thereof are also easily charged similarly to the above powder. When the molded body or the baked cured body is charged, the adhesive force is increased, and due to this, the problem of handling properties such as the surface of the heat insulating material being slippery and the powder adhering during the manufacture of the encapsulant are reduced. This causes problems in manufacturing such as adhesion to the jacket material, causing a sealing failure, and a decrease in yield.
そこで、本発明は、撹拌時の帯電性が低く、付着力が低い、粉体を提供することを目的とする。 In view of the above, an object of the present invention is to provide a powder having low chargeability during stirring and low adhesion.
本発明者らは、上記従来技術の課題を解決するために鋭意研究を重ねた結果、シリカ粒子と、特定の無機繊維と、を含む、粉体が、上記従来技術の課題を解決できることを見出し、本発明を完成するに至った。 As a result of intensive studies in order to solve the problems of the conventional technique, the present inventors have found that a powder containing silica particles and specific inorganic fibers can solve the problems of the conventional technique. The present invention has been completed.
すなわち、本発明は下記の通りである。
[1]シリカ粒子と、無機繊維と、を含み、
前記無機繊維は、前記無機繊維100質量%に対して、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維である、粉体。
[2]前記シリカ粒子は、粒子径DSが5nm以上30nm以下である複数の小粒子を含む、[1]に記載の粉体。
[3]赤外線不透明化粒子をさらに含む、[1]又は[2]に記載の粉体。
[4]アルミナ粒子をさらに含む、[1]から[3]のいずれか1に記載の粉体。
[5]断熱材に用いられる、[1]から[4]のいずれか1に記載の粉体。
[6][1]から[5]のいずれか1に記載の粉体を含む、成形体。
[7]0%以上5%以下の圧縮率における最大荷重が、0.7MPa以上である、[6]に記載の成形体。
[8][1]から[5]のいずれか1に記載の粉体及び/又は[6]又は[7]に記載の成形体を含むコア材と、前記コア材を収容する外被材と、を備える、被包体。
That is, the present invention is as follows.
[1] containing silica particles and inorganic fibers,
The inorganic fibers, with respect to the inorganic fibers 100 wt%, an inorganic fiber comprising Fe 2 O 3 40 wt% or more 1 wt% of iron in terms of the following powder.
[2] The powder according to [1], wherein the silica particles include a plurality of small particles having a particle diameter D S of 5 nm to 30 nm.
[3] The powder according to [1] or [2], further comprising infrared opaque particles.
[4] The powder according to any one of [1] to [3], further comprising alumina particles.
[5] The powder according to any one of [1] to [4], which is used for a heat insulating material.
[6] A molded article comprising the powder according to any one of [1] to [5].
[7] The molded article according to [6], wherein the maximum load at a compression rate of 0% or more and 5% or less is 0.7 MPa or more.
[8] A core material including the powder according to any one of [1] to [5] and / or the molded body according to [6] or [7], and a jacket material that accommodates the core material; An enveloping body.
本発明の粉体によれば、撹拌時における低い帯電性と、低い付着力を得ることができる。 According to the powder of the present invention, low chargeability during stirring and low adhesion can be obtained.
以下、本発明を実施するための形態(以下、「本実施形態」という。)について詳細に説明する。以下の本実施形態は、本発明を説明するための例示であり、本発明を以下の本実施形態に限定するものではない。本発明は、その要旨の範囲内で種々変形して実施することができる。 Hereinafter, a mode for carrying out the present invention (hereinafter referred to as “the present embodiment”) will be described in detail. The following embodiment is an exemplification for explaining the present invention, and the present invention is not limited to the following embodiment. The present invention can be implemented with various modifications within the scope of the gist.
〔粉体〕
本実施形態の粉体は、シリカ粒子と、無機繊維と、を含み、前記無機繊維は、前記無機繊維100質量%に対して、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維である。
〔powder〕
The powder of the present embodiment includes silica particles and inorganic fibers, and the inorganic fibers contain iron in an amount of 1% by mass to 40% by mass in terms of Fe 2 O 3 with respect to 100% by mass of the inorganic fibers. Inorganic fiber containing.
<シリカ粒子>
本実施形態の粉体は、シリカ粒子を含む。本実施形態のシリカ粒子とは、組成式SiO2で表される成分からなる粒子、及びSiO2を含む材料を指し、SiO2に加えて金属成分、無機化合物等を含む粒子を包含するものである。つまり、シリカ粒子は、純粋な二酸化ケイ素に加えて、Si又は種々の他元素との塩及び複合酸化物を含んでもよいし、水酸化物のような含水酸化物を含んでもよい。また、シリカ粒子がシラノール基を有していてもよい。シリカ粒子中のシリカは、結晶質であっても、非晶質であっても、それらの混合体であってもよい。シリカ粒子のシリカが非晶質であると、断熱材として用いる場合の固体伝導による伝熱が小さく、断熱性能が向上する傾向にあるため、好ましい。
<Silica particles>
The powder of this embodiment contains silica particles. The silica particles of the present embodiment refer to particles composed of components represented by the composition formula SiO 2 and materials containing SiO 2 , including particles containing metal components, inorganic compounds, etc. in addition to SiO 2. is there. That is, in addition to pure silicon dioxide, the silica particles may contain a salt with Si or various other elements and a composite oxide, or may contain a hydrated oxide such as a hydroxide. Moreover, the silica particle may have a silanol group. Silica in the silica particles may be crystalline, amorphous, or a mixture thereof. It is preferable that the silica of the silica particles is amorphous because heat transfer due to solid conduction is small when used as a heat insulating material, and the heat insulating performance tends to be improved.
シリカ粒子として、具体的には、「シリカ」、「石英」等のケイ素の酸化物;ケイ素の部分酸化物;シリカアルミナ、ゼオライト等のケイ素の複合酸化物;Na、Ca、K、Mg、Ba、Ce、B、Fe、及びAlのいずれかのケイ酸塩(ガラス);ケイ素以外の元素の酸化物、部分酸化物、塩、又は複合酸化物(アルミナ、チタニア等)と、ケイ素の酸化物、部分酸化物、塩、又は複合酸化物との混合体;SiC、SiN等の酸化物等が挙げられる。 Specific examples of silica particles include silicon oxides such as “silica” and “quartz”; silicon partial oxides; silicon composite oxides such as silica alumina and zeolite; Na, Ca, K, Mg, Ba Silicate (glass) of any one of Ce, B, Fe, and Al; oxides, partial oxides, salts, or complex oxides (alumina, titania, etc.) of elements other than silicon, and oxides of silicon , Partial oxides, salts, or mixtures with complex oxides; oxides such as SiC and SiN.
粉体100質量%に対して、シリカを50質量%以上含むことが好ましく、75質量%以上含むことがより好ましい。シリカを50質量%以上含むことで、粉体の固体伝導による伝熱が小さくなり、断熱材としての用途に好適な傾向にある。シリカを75質量%以上含むことで、粉体間の凝集力が高まり、粉体の飛散が少なくなる傾向にある。 Silica is preferably contained in an amount of 50% by mass or more and more preferably 75% by mass or more with respect to 100% by mass of the powder. By including 50 mass% or more of silica, heat transfer due to solid conduction of the powder becomes small, and it tends to be suitable for use as a heat insulating material. By including 75% by mass or more of silica, the cohesive force between the powders is increased and the powder scattering tends to be reduced.
粉体の用途によっては、粉体がシリカ粒子及び無機繊維以外の材料を含んでもよい。シリカ粒子以外の材料については後で詳述するが、粉体がシリカ粒子及び無機繊維以外の材料を含む場合には、粉体100質量%に対して、シリカを50質量%以上99.9質量%以下であることが好ましく、50質量%以上97.5質量%以下がより好ましく、60質量%以上97.5質量%以下がさらに好ましい。シリカ粒子が50質量%以上97.5質量%以下であることで、赤外線不透明化粒子等を含む粉体の場合は、粉体の飛散が抑制され、高い温度での断熱性能の向上といった効果があらわれる傾向にある。また、シリカ粒子が60質量%以上97.5重量%以下であることで、粉体のかさ密度がより小さくなる傾向にある。 Depending on the application of the powder, the powder may contain materials other than silica particles and inorganic fibers. Materials other than silica particles will be described in detail later. When the powder contains materials other than silica particles and inorganic fibers, silica is contained in an amount of 50% by mass or more and 99.9% by mass with respect to 100% by mass of the powder. % Is preferably 50% by mass or more and 97.5% by mass or less, and more preferably 60% by mass or more and 97.5% by mass or less. When the silica particles are 50% by mass or more and 97.5% by mass or less, in the case of a powder containing infrared opaque particles and the like, the scattering of the powder is suppressed, and the effect of improving the heat insulation performance at a high temperature is obtained. It tends to appear. Moreover, it exists in the tendency for the bulk density of powder to become smaller because a silica particle is 60 to 97.5 weight%.
粉体を断熱材として用いる場合は、その使用される温度において、シリカ粒子が熱的に安定であることが好ましい。具体的には、断熱材の使用最高温度において1時間保持したときに、シリカ粒子の質量が10%以上減少しないことが好ましい。また、シリカ粒子は耐水性を有することが好ましい。具体的には、25℃の水100gに対するシリカ粒子の溶解量が0.1g未満であることが好ましく、0.01g未満であることがより好ましい When using a powder as a heat insulating material, it is preferable that a silica particle is thermally stable in the temperature used. Specifically, it is preferable that the mass of the silica particles does not decrease by 10% or more when held at the maximum use temperature of the heat insulating material for 1 hour. The silica particles preferably have water resistance. Specifically, the amount of silica particles dissolved in 100 g of water at 25 ° C. is preferably less than 0.1 g, more preferably less than 0.01 g.
シリカ粒子の比重は、粉体を断熱材とする場合に断熱材のかさ密度が小さくなる傾向にあるため、2.0以上4.0以下であることが好ましく、2.0以上3.0以下であることがより好ましく、2.0以上2.5以下であることがさらに好ましい。ここで、シリカを含む無機化合物粒子の比重は、ピクノメーター法により求まる真比重を指す。 The specific gravity of the silica particles is preferably 2.0 or more and 4.0 or less, and preferably 2.0 or more and 3.0 or less because the bulk density of the heat insulating material tends to be small when the powder is used as a heat insulating material. More preferably, it is 2.0 or more and 2.5 or less. Here, the specific gravity of the inorganic compound particles containing silica refers to the true specific gravity determined by the pycnometer method.
本実施形態の粉体は、シリカ粒子を一種のみ含有してもよいし、2種類以上を含んでもよく、粒子径の異なる2種類のシリカ粒子、すなわちシリカからなる小粒子と大粒子とを含むことが好ましい。粒子径の異なる2種類のシリカ粒子を含むことで、小粒子と大粒子の帯電性及び熱伝導率が異なるため、2種類のシリカ粒子を適当な割合とすることで、帯電性及び熱伝導率を調整することができる。 The powder of the present embodiment may contain only one kind of silica particles or two or more kinds, and includes two kinds of silica particles having different particle diameters, that is, small particles and large particles made of silica. It is preferable. By including two types of silica particles with different particle sizes, the chargeability and thermal conductivity of small particles and large particles differ. Can be adjusted.
本実施形態のシリカ粒子は、粒子径DSが5nm以上30nm以下である、複数の小粒子を含むことがより好ましく、5nm以上25nm以下である複数の小粒子を含むことがさらに好ましく、5nm以上20nm以下である複数の小粒子を含むことが特に好ましい。粒子径DSが5nm以上であることで、小粒子であるシリカ粒子が化学的に安定し、断熱性能が安定しやすい傾向にある。粒子径DSが30nm以下であることで、小粒子であるシリカ粒子同士の接触面積が小さく、粉体の固体伝導による伝熱が少なくなり、熱伝導率が小さくなる傾向にある。粒子径DSが25nm以下であることで、熱伝導率がより小さくなる傾向にある。 The silica particles of the present embodiment more preferably include a plurality of small particles having a particle diameter D S of 5 nm to 30 nm, more preferably a plurality of small particles of 5 nm to 25 nm. It is particularly preferred to include a plurality of small particles that are 20 nm or less. By particle diameter D S is 5nm or more, the silica particles are small particles chemically stable, heat insulating performance is in a stable prone. By particle diameter D S is 30nm or less, small contact area between the silica particles are small particles, heat transfer is reduced by the powder of the solid conduction, tends to thermal conductivity is reduced. By particle diameter D S is 25nm or less, there is a tendency that the thermal conductivity becomes smaller.
シリカ粒子の粒子径は、電界放射型走査型電子顕微鏡(FE−SEM)で観察し、その等面積円相当径を求めることにより測定できる。平均粒子径は、粒子100個をFE−SEMで観察し、その等面積円相当径を求めて数平均を算出することにより、確認することができる。このとき、等面積円相当径が35nm未満の粒子を小粒子として測定し、小粒子の粒子径を粒子径DS、小粒子の粒子径の平均をDS平均、とし、等面積円相当径が35nm以上の粒子を大粒子として測定し、大粒子の粒子径を粒子径DL、大粒子の粒子径の平均をDL平均とする。 The particle diameter of the silica particles can be measured by observing with a field emission scanning electron microscope (FE-SEM) and determining the equivalent area equivalent circle diameter. The average particle diameter can be confirmed by observing 100 particles with FE-SEM, obtaining the equivalent area equivalent circle diameter, and calculating the number average. At this time, particles having an equivalent area circle equivalent diameter of less than 35 nm are measured as small particles, the particle diameter of the small particles is taken as the particle diameter D S , and the average of the particle diameters of the small particles is taken as the D S average . There the more particles 35nm measured as large particles, large particle size particles size of the particles D L, the average particle diameter of the large particles and D L average.
本実施形態のシリカ粒子は、DL平均が、DS平均<DL平均を満たし、40nm以上60μm以下である複数の小粒子を含むことがより好ましく、40nm以上10μm以下である複数の小粒子を含むことがさらに好ましく、40nm以上5μm以下である複数の小粒子を含むことが特に好ましい。DL平均が40nm以上であることで、粉体を成形した場合におけるスプリングバックが小さい傾向にある。DL平均が60μm以下であることで、熱伝導率が小さい傾向にある。DL平均が10μm以下であることで、粉体中の無機繊維及び赤外線不透明化粒子等とが均一に混合される傾向にある。DL平均が5μm以下であることで、粒子の付着力が大きく、粉体からの粒子の脱落が少なくなる傾向にある。 Silica particles of the present embodiment, D L mean, D S mean <D L average satisfied, more preferably comprising a plurality of small particles is 40nm or more 60μm or less, a plurality of small particles is 40nm or more 10μm or less Is more preferable, and it is particularly preferable to include a plurality of small particles having a size of 40 nm to 5 μm. When the DL average is 40 nm or more, the spring back tends to be small when the powder is molded. When the DL average is 60 μm or less, the thermal conductivity tends to be small. When the DL average is 10 μm or less, the inorganic fibers and infrared opaque particles in the powder tend to be uniformly mixed. When the DL average is 5 μm or less, the adhesion force of the particles is large, and the dropout of the particles from the powder tends to be reduced.
DL平均は、DS平均の2倍以上であることが好ましく、3倍以上であることがより好ましく、4倍以上であることがさらに好ましい。2倍以上であることで、粉体を成形した場合にスプリングバックが小さくなる傾向にある。3倍以上であることで、小粒子のシリカ粒子と大粒子のシリカ粒子が混合する粉体のかさ比重が大きく、粉体体積が小さく、作業性が高くなる傾向にある。4倍以上であることで、小粒子のシリカ粒子と大粒子のシリカ粒子の粒径の差が大きく、大粒子のシリカ粒子が小粒子のシリカ粒子に対して分散が容易である傾向がある。シリカ粒子の分散性が良好であると、粉体を断熱材として用いる場合に、固体伝熱性が小さくなる傾向にある。 The D L average is preferably at least twice the DS average , more preferably at least 3 times, and even more preferably at least 4 times. When it is twice or more, the springback tends to be small when the powder is molded. By being 3 times or more, the bulk specific gravity of the powder in which the small particles and the large particles are mixed tends to be large, the powder volume is small, and the workability tends to be high. By being 4 times or more, the difference in particle size between the small silica particles and the large silica particles is large, and the large silica particles tend to be easily dispersed with respect to the small silica particles. When the dispersibility of the silica particles is good, the solid heat conductivity tends to be small when the powder is used as a heat insulating material.
<無機繊維>
本実施形態の粉体は、無機繊維100質量%に対して、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維を含む。Fe2O3換算で鉄を1質量%以上40質量%以下含有する無機繊維を含むことで、粉体の帯電性が抑制され、撹拌時に撹拌容器への付着が少なくなる。この理由は明らかではないが、鉄として酸化鉄であるFeO及びFeOと比較して還元状態のFe化合物等が存在するため、これが粉体と電気的に相互作用し、撹拌時の帯電を抑制すると推測される。また、無機繊維はアスペクト比が高い形状を有することで、撹拌時に粉体及び撹拌容器と効率良く接触できるため、撹拌による粉体の帯電と容器への付着を抑制する優れた性能を示すとも推測される。
<Inorganic fiber>
Powder of the present embodiment, the inorganic fibers 100 wt%, including inorganic fibers containing iron 1 mass% to 40 mass% in terms of Fe 2 O 3. By including inorganic fibers containing 1% by mass or more and 40% by mass or less of iron in terms of Fe 2 O 3 , the chargeability of the powder is suppressed, and adhesion to the stirring vessel is reduced during stirring. The reason for this is not clear, but there is a reduced Fe compound, etc., as compared with FeO and FeO, which are iron oxides. As a result, this interacts electrically with the powder and suppresses charging during stirring. Guessed. In addition, since the inorganic fiber has a shape with a high aspect ratio, it can be efficiently contacted with the powder and the stirring container at the time of stirring. Is done.
本実施形態の鉄として、具体的には、Fe;FeO、Fe2O3、Fe3O4等の酸化鉄;Fe(OH)2、Fe(OH)3等の水酸化鉄;FeOOH等のオキシ水酸化鉄;硫化鉄、硫酸鉄、硝酸鉄、酢酸鉄、シュウ酸鉄、炭酸鉄、塩化鉄、リン酸鉄等の鉄塩;NaFeO2、NaFe2O3、KFeO2、K2FeO4、CaFeO2、CaFe2O4、MgFe2O4等の酸化鉄の塩;NaFeSiO3、FeSiO4等のケイ酸鉄類;NaFeSi2O6、KFeSi2O6、CaFeSi2O6、MgFeSi2O6等のケイ酸鉄塩類;FeAl2O4等のアルミン酸鉄類;Na(Fe0.75Al0.25)O2、Ca2FeAlO5、MgFeAlO4等のアルミン酸鉄塩類;FeTiO3等のFeとTiの複合酸化物;NaTiFeO4、KFeTi3O8、CaFeTi2O6、MgFeTi4O10等のFeとTiの複合酸化物の塩等が挙げられる。 Specifically, as iron of this embodiment, Fe; FeO, Fe 2 O 3 , iron oxide such as Fe 3 O 4 ; iron hydroxide such as Fe (OH) 2 and Fe (OH) 3 ; FeOOH, etc. Iron oxyhydroxide; iron salts such as iron sulfide, iron sulfate, iron nitrate, iron acetate, iron oxalate, iron carbonate, iron chloride, iron phosphate; NaFeO 2 , NaFe 2 O 3 , KFeO 2 , K 2 FeO 4 , CaFeO 2 , CaFe 2 O 4 , MgFe 2 O 4 and other iron oxide salts; NaFeSiO 3 , FeSiO 4 and other iron silicates; NaFeSi 2 O 6 , KFeSi 2 O 6 , CaFeSi 2 O 6 , MgFeSi 2 O Iron silicates such as 6 ; iron aluminates such as FeAl 2 O 4 ; iron aluminates such as Na (Fe 0.75 Al 0.25 ) O 2 , Ca 2 FeAlO 5 , MgFeAlO 4 ; Fe and Ti such as FeTiO 3 Composite oxide of NaTiFeO 4 , K Examples thereof include salts of complex oxides of Fe and Ti such as FeTi 3 O 8 , CaFeTi 2 O 6 , and MgFeTi 4 O 10 .
本実施形態の鉄は、無機繊維100質量%に対してFe2O3換算で、1質量%以上30質量%以下であることがより好ましく、1質量%以上25質量%以下であることがさらに好ましく、2質量%以上25質量%以下であることが特に好ましく、5質量%以上25質量%以下であることがより特に好ましい。鉄が30質量%以下であることで断熱性能に優れる傾向にあるり、25質量%以下であることで無機繊維が切れにくくなり強度に優れる傾向にあり、2重量%以上であることで粉体への分散性が向上する傾向にあり、5質量%以上であることで粉体との凝集力が増し粉体の飛散が抑えられる傾向にある。 The iron of this embodiment is more preferably 1% by mass to 30% by mass and more preferably 1% by mass to 25% by mass in terms of Fe 2 O 3 with respect to 100% by mass of the inorganic fibers. It is particularly preferably 2% by mass or more and 25% by mass or less, and particularly preferably 5% by mass or more and 25% by mass or less. When the amount of iron is 30% by mass or less, heat insulation performance tends to be excellent. When the amount is 25% by mass or less, inorganic fibers are difficult to cut and the strength tends to be excellent. The dispersibility tends to be improved, and when it is 5% by mass or more, the cohesive force with the powder is increased and the scattering of the powder tends to be suppressed.
Fe2O3換算とは、無機繊維に含まれる各組成を酸化物として換算した合計量を無機繊維100質量%とし、それに対する本実施形態の鉄をFe2O3に換算した質量としたものである。具体的には、実施例に記載する測定方法により求める。 With Fe 2 O 3 conversion, the total amount of each component contained in the inorganic fiber converted as an oxide is 100% by mass of the inorganic fiber, and the iron according to this embodiment is converted into the mass converted to Fe 2 O 3. It is. Specifically, it calculates | requires by the measuring method described in an Example.
無機繊維中の鉄の質量割合は、無機繊維を粉体から分級できる場合には、蛍光X線測定により、次の方法に従い求める。無機繊維1gと、結晶セルロース粉末のフナセルII粉末(商品名、フナコシ株式会社製)1gを、乳鉢で30分間混合後、混合粉末2gを内径25mm、厚さ5mm、幅3mmの塩化ビニル製のリング内に充填し、プレス機により厚さ3mmに加圧成形し、測定試料とする。この試料の全定性分析を行い、成分形態は酸化物として、ファンダメンタルパラメーター法により、FeのFe2O3換算の質量%を求める。フナセルII粉末はフラックスとして、計算から除外する。例えば、蛍光X線測定装置として、走査型蛍光X線分析装置ZSX PrimusII(商品名、株式会社リガク製)を使用する場合は、あらかじめフナセルII粉末を、組成C6H10O5のフラックスとして化合物登録しておき、試料モデルはバルク、成分形態は酸化物、フラックスはフナセルII粉末、希釈率は1を選択し、SQX計算を実施することにより、Fe2O3の質量%を求める。 When the inorganic fiber can be classified from the powder, the mass ratio of iron in the inorganic fiber is determined by fluorescent X-ray measurement according to the following method. After mixing 1 g of inorganic fiber and 1 g of Fungusel II powder of crystalline cellulose powder (trade name, manufactured by Funakoshi Co., Ltd.) for 30 minutes in a mortar, 2 g of the mixed powder is a ring made of vinyl chloride having an inner diameter of 25 mm, a thickness of 5 mm, and a width of 3 mm. The sample is filled in and pressed into a thickness of 3 mm with a press machine to obtain a measurement sample. A total qualitative analysis of this sample is performed, and the mass of Fe in terms of Fe 2 O 3 is determined by the fundamental parameter method, with the component form being an oxide. Funacell II powder is excluded from the calculation as flux. For example, when a scanning fluorescent X-ray analyzer ZSX Primus II (trade name, manufactured by Rigaku Corporation) is used as the fluorescent X-ray measuring device, the compound as a flux of composition C 6 H 10 O 5 is used in advance. By registering, the sample model is bulk, the component form is oxide, the flux is Funasel II powder, the dilution rate is 1, and the SQX calculation is performed to determine the mass% of Fe 2 O 3 .
また、断熱材中の無機繊維が焼結等の理由により粉体から分級できない場合には、断熱材の断面中に見られる無機繊維の鉄の含有量をSEM−EDX測定することにより、求める。 Moreover, when the inorganic fiber in a heat insulating material cannot be classified from powder for reasons, such as sintering, it calculates | requires by measuring the iron content of the inorganic fiber seen in the cross section of a heat insulating material by SEM-EDX.
本実施形態の無機繊維とは、無機繊維の平均太さに対する無機繊維の平均長さの比(アスペクト比)が、10以上であるものが好ましく、50以上であるものがより好ましく、100以上であるものがさらに好ましい。アスペクト比が10以上であることで、粉体を成形する場合に小さい圧力で成形が可能である傾向にある。また、アスペクト比が50以上であることで、成形体の生産性を向上する傾向にある。さらに、アスペクト比が100以上であることで、成形体の曲げ強度が優れたものとなる傾向にある。 The inorganic fiber of the present embodiment preferably has a ratio (aspect ratio) of the average length of the inorganic fiber to the average thickness of the inorganic fiber of 10 or more, more preferably 50 or more, and 100 or more. Some are more preferred. When the aspect ratio is 10 or more, the powder tends to be molded with a small pressure when it is molded. Moreover, it exists in the tendency which improves the productivity of a molded object because an aspect-ratio is 50 or more. Furthermore, when the aspect ratio is 100 or more, the bending strength of the molded product tends to be excellent.
無機繊維のアスペクト比は、FE−SEMにより測定した無機繊維100本の太さ及び長さの平均値から求める。 The aspect ratio of the inorganic fiber is determined from the average value of the thickness and length of 100 inorganic fibers measured by FE-SEM.
無機繊維は、粉体中で単分散して混合されていることが好ましいが、無機繊維が互いに絡まった状態、又は複数の無機繊維が同一方向で揃った束の状態で混合されていてもかまわない。また、無機繊維は、単分散状態において、無機繊維の向きが同一方向で揃った状態であってもかまわない。ただし、熱伝導率を小さくする観点から、無機繊維は、伝熱方向に対して垂直方向に配向していることが好ましい。 The inorganic fibers are preferably monodispersed and mixed in the powder. However, the inorganic fibers may be mixed in a state where the inorganic fibers are entangled with each other or a bundle in which a plurality of inorganic fibers are aligned in the same direction. Absent. In addition, the inorganic fibers may be in a monodispersed state in which the directions of the inorganic fibers are aligned in the same direction. However, from the viewpoint of reducing the thermal conductivity, the inorganic fibers are preferably oriented in a direction perpendicular to the heat transfer direction.
無機繊維として、具体的には、ガラス長繊維(フィラメント)(SiO2−Al2O3−B2O3−CaO)、グラスウール(SiO2−Al2O3−CaO−Na2O)、耐アルカリガラス繊維(SiO2−ZrO2−CaO−Na2O)、ロックウール(バサルトウール)(SiO2−Al2O3−Fe2O3−MgO−CaO)、スラグウール(SiO2−Al2O3−MgO−CaO)、セラミックファイバー(ムライト繊維)(Al2O3−SiO2)、シリカ繊維(SiO2)、アルミナ繊維(Al2O3−SiO2)、バサルト繊維(SiO2−Al2O3−Fe2O3−MgO−CaO)、チタン酸カリウム繊維、アルミナウィスカー、炭化ケイ素ウィスカー、窒化ケイ素ウィスカー、炭酸カルシウムウィスカー、塩基性硫酸マグネシウムウィスカー、硫酸カルシウムウィスカー(セッコウ繊維)、酸化亜鉛ウィスカー、ジルコニア繊維、炭素繊維、黒鉛ウィスカー、フォスフェート繊維、AES(Alkaline Earth Silicate)ファイバー(SiO2−CaO−MgO);天然鉱物のウォラストナイト、セピオライト、アタパルジャイト、ブルーサイト等が挙げられる。これらの無機繊維は、Fe2O3換算で鉄を1質量%以上40質量%以下含むものであれば、特に限定されない。 Specific examples of inorganic fibers include long glass fibers (filaments) (SiO 2 —Al 2 O 3 —B 2 O 3 —CaO), glass wool (SiO 2 —Al 2 O 3 —CaO—Na 2 O), Alkali glass fiber (SiO 2 —ZrO 2 —CaO—Na 2 O), rock wool (basalt wool) (SiO 2 —Al 2 O 3 —Fe 2 O 3 —MgO—CaO), slag wool (SiO 2 —Al 2) O 3 —MgO—CaO), ceramic fiber (mullite fiber) (Al 2 O 3 —SiO 2 ), silica fiber (SiO 2 ), alumina fiber (Al 2 O 3 —SiO 2 ), basalt fiber (SiO 2 —Al 2 O 3 -Fe 2 O 3 -MgO -CaO), potassium titanate fibers, alumina whiskers, silicon carbide whiskers, silicon nitride whiskers, calcium carbonate whiskers, basic sulfate Magnesium whisker, calcium sulfate whisker (gypsum fiber), zinc oxide whisker, zirconia fiber, carbon fiber, graphite whisker, phosphate fibers, AES (Alkaline Earth Silicate) fiber (SiO 2 -CaO-MgO); natural mineral wollastonite , Sepiolite, attapulgite, brucite and the like. These inorganic fibers are not particularly limited as long as they contain 1% by mass or more and 40% by mass or less of iron in terms of Fe 2 O 3 .
これらの無機繊維を調製する際に、鉄を含む原料を使用したり、その使用量を調整することで、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維を得ることができる。 When preparing these inorganic fibers, by using a raw material containing iron or adjusting the amount used, an inorganic fiber containing 1 mass% or more and 40 mass% or less of iron in terms of Fe 2 O 3 is obtained. Can do.
無機繊維としては、断熱性能の観点から、SiO2を含むものが好ましい。無機繊維がSiO2を含むことは、上述のXRFにより確認することができる。SiO2を含むものとして、具体的には、ガラス長繊維(フィラメント)(SiO2−Al2O3−B2O3−CaO)、グラスウール(SiO2−Al2O3−CaO−Na2O)、耐アルカリガラス繊維(SiO2−ZrO2−CaO−Na2O)、ロックウール(バサルトウール)(SiO2−Al2O3−Fe2O3−MgO−CaO)、スラグウール(SiO2−Al2O3−MgO−CaO)、セラミックファイバー(ムライト繊維)(Al2O3−SiO2)、シリカ繊維(SiO2)、アルミナ繊維(Al2O3−SiO2)、バサルト繊維(SiO2−Al2O3−Fe2O3−MgO−CaO)、AES(Alkaline Earth Silicate)ファイバー(SiO2−CaO−MgO)、天然鉱物のウォラストナイト、セピオライト、アタパルジャイト等が挙げられる。 Inorganic fibers are preferably those containing SiO 2 from the viewpoint of heat insulation performance. It can be confirmed by the above-mentioned XRF that the inorganic fiber contains SiO 2 . Specific examples of the material containing SiO 2 include long glass fibers (filaments) (SiO 2 —Al 2 O 3 —B 2 O 3 —CaO), glass wool (SiO 2 —Al 2 O 3 —CaO—Na 2 O). ), Alkali-resistant glass fiber (SiO 2 —ZrO 2 —CaO—Na 2 O), rock wool (basalt wool) (SiO 2 —Al 2 O 3 —Fe 2 O 3 —MgO—CaO), slag wool (SiO 2 —) Al 2 O 3 —MgO—CaO), ceramic fiber (mullite fiber) (Al 2 O 3 —SiO 2 ), silica fiber (SiO 2 ), alumina fiber (Al 2 O 3 —SiO 2 ), basalt fiber (SiO 2 — Al 2 O 3 —Fe 2 O 3 —MgO—CaO), AES (Alkaline Earth Silicate) fiber (SiO 2 —CaO—MgO), natural mineral wallus Tonite, sepiolite, attapulgite and the like can be mentioned.
無機繊維としては、耐熱性の観点から、Al2O3を含むものが好ましい。無機繊維がAl2O3を含むことは、上述のXRFにより確認することができる。Al2O3を含むものとして、具体的には、ガラス長繊維(フィラメント)(SiO2−Al2O3−B2O3−CaO)、グラスウール(SiO2−Al2O3−CaO−Na2O)、ロックウール(バサルトウール)(SiO2−Al2O3−Fe2O3−MgO−CaO)、スラグウール(SiO2−Al2O3−MgO−CaO)、セラミックファイバー(ムライト繊維)(Al2O3−SiO2)、アルミナ繊維(Al2O3−SiO2)、バサルト繊維(SiO2−Al2O3−Fe2O3−MgO−CaO)、天然鉱物のアタパルジャイト等が挙げられる。 The inorganic fibers, from the viewpoint of heat resistance, those containing Al 2 O 3 is preferred. It can be confirmed by the above-mentioned XRF that the inorganic fiber contains Al 2 O 3 . As including al 2 O 3, specifically, long glass fibers (filaments) (SiO 2 -Al 2 O 3 -B 2 O 3 -CaO), glass wool (SiO 2 -Al 2 O 3 -CaO -Na2O ), Rock wool (basalt wool) (SiO 2 —Al 2 O 3 —Fe 2 O 3 —MgO—CaO), slag wool (SiO 2 —Al 2 O 3 —MgO—CaO), ceramic fiber (mullite fiber) ( Al 2 O 3 —SiO 2 ), alumina fibers (Al 2 O 3 —SiO 2 ), basalt fibers (SiO 2 —Al 2 O 3 —Fe 2 O 3 —MgO—CaO), natural mineral attapulgite and the like. .
無機繊維の平均太さは、飛散を防ぐ観点から、1μm以上が好ましい。断熱材として用いる場合には、固体伝導による伝熱を抑える観点から、20μm以下であることが好ましい。無機繊維の平均太さは、FE−SEMにより、無機繊維100本の太さを求めて、これを平均して求める。 The average thickness of the inorganic fibers is preferably 1 μm or more from the viewpoint of preventing scattering. When using as a heat insulating material, it is preferable that it is 20 micrometers or less from a viewpoint of suppressing the heat transfer by solid conduction. The average thickness of the inorganic fibers is determined by calculating the thickness of 100 inorganic fibers by FE-SEM and averaging them.
本実施形態の無機繊維は、粉体100質量%に対して、0.1質量%以上20質量%以下が好ましく、0.5質量%以上15質量%以下がより好ましく、0.5質量%以上10質量%以下がさらに好ましい。無機繊維が0.1質量%以上であることで、帯電性が抑制される傾向にある。また、無機繊維が20質量%以下であることで、熱伝導率が小さくなる傾向にある。さらに、0.5質量%以上20質量%以下であることで、混合容器璧への繊維の付着の影響が小さくなり、繊維含有量の再現性が良くなる傾向にあり、0.5質量%以上15質量%以下であることで、ダマの発生等無く混合が容易となる傾向にあり、0.5質量%以上10質量%以下であることで、成形時のスプリングバックが小さくなり、成形欠が起こりにくくなり、生産性が良好となる傾向にある。 The inorganic fiber of the present embodiment is preferably 0.1% by mass or more and 20% by mass or less, more preferably 0.5% by mass or more and 15% by mass or less, and more preferably 0.5% by mass or more with respect to 100% by mass of the powder. 10 mass% or less is still more preferable. When the inorganic fiber is 0.1% by mass or more, the chargeability tends to be suppressed. Moreover, it exists in the tendency for heat conductivity to become small because inorganic fiber is 20 mass% or less. Furthermore, when the content is 0.5% by mass or more and 20% by mass or less, the influence of the adhesion of fibers to the mixing container wall is reduced, and the reproducibility of the fiber content tends to be improved. When it is 15% by mass or less, there is a tendency that mixing does not occur and the mixing becomes easy. It tends to occur less easily and productivity tends to be good.
無機繊維によっては、絶縁性の高い表面処理が施されている場合もあるが、無機繊維を洗浄する等の絶縁性の高い表面処理剤を除去する等の後に、粉体の原料することも可能である。 Depending on the inorganic fiber, a surface treatment with a high insulating property may be applied, but after removing the surface treatment agent with a high insulating property such as washing the inorganic fiber, it is also possible to use it as a raw material for powder. It is.
<赤外線不透明化粒子>
本実施形態の粉体は、赤外線不透明化粒子をさらに含むことが、高い温度での断熱性能を得られる点から、好ましい。赤外線不透明化粒子とは、赤外線を反射、散乱又は吸収する材料を含む粒子を指す。粉体に赤外線不透明化粒子を含むと、輻射による伝熱が抑制されるため、特に200℃以上の高い温度領域での断熱性能が高い傾向にある。
<Infrared opaque particles>
It is preferable that the powder of this embodiment further contains infrared opaque particles from the viewpoint of obtaining heat insulation performance at a high temperature. An infrared opaque particle refers to a particle containing a material that reflects, scatters, or absorbs infrared light. When infrared opaque particles are included in the powder, heat transfer due to radiation is suppressed, so that the heat insulation performance particularly in a high temperature region of 200 ° C. or higher tends to be high.
赤外線不透明化粒子として、具体的には、酸化ジルコニウム、ケイ酸ジルコニウム、二酸化チタン、鉄チタン酸化物、酸化鉄、酸化銅、炭化ケイ素、金鉱石、二酸化クロム、二酸化マンガン、グラファイト等の炭素質物質、炭素繊維、スピネル顔料、アルミニウム等の粒子、ステンレス鋼の粒子、青銅の粒子、銅/亜鉛合金の粒子、銅/クロム合金の粒子等が挙げられる。これらの金属粒子又は非金属粒子を、単独で用いてもよく、2種類以上を併用してもよい。 Specific examples of infrared opaque particles include zirconium oxide, zirconium silicate, titanium dioxide, iron titanium oxide, iron oxide, copper oxide, silicon carbide, gold ore, chromium dioxide, manganese dioxide, graphite and other carbonaceous materials. , Carbon fiber, spinel pigment, aluminum particles, stainless steel particles, bronze particles, copper / zinc alloy particles, copper / chromium alloy particles, and the like. These metal particles or non-metal particles may be used alone or in combination of two or more.
これらの赤外線不透明化粒子の中で、酸化ジルコニウム、ケイ酸ジルコニウム、二酸化チタン、炭化ケイ素の粒子が好ましい。赤外線不透明化粒子の組成は、FE−SEM EDXにより求められる。 Of these infrared opaque particles, zirconium oxide, zirconium silicate, titanium dioxide, and silicon carbide particles are preferred. The composition of the infrared opaque particles is determined by FE-SEM EDX.
赤外線不透明化粒子の平均粒子径は、0.5μm以上30μm以下が好ましく、0.5μm以上10μm以下がより好ましい。平均粒子径が0.5μm以上であることで、200℃以上での断熱性能に優れる傾向にあり、平均粒子径が30μm以下であることで、固体伝導の抑制による200℃未満での断熱性能に優れる傾向にある。また、無機繊維とシリカ粒子のサイズにもよるが、シリカ粒子の平均粒子径DS及びDLが5nm以上50μm以下の場合には、赤外線不透明化粒子の平均粒子径は0.5μm以上10μm以下であることで、シリカ粒子との混合が容易となる傾向にある。なお、赤外線不透明化粒子の平均粒子径は、上述のシリカ粒子と同じ方法により求められる。 The average particle size of the infrared opaque particles is preferably 0.5 μm or more and 30 μm or less, and more preferably 0.5 μm or more and 10 μm or less. When the average particle diameter is 0.5 μm or more, the heat insulation performance at 200 ° C. or more tends to be excellent, and when the average particle diameter is 30 μm or less, the heat insulation performance at less than 200 ° C. due to suppression of solid conduction. It tends to be excellent. Also, depending on the size of the inorganic fibers and silica particles, when the average particle diameter D S and D L of the silica particles is 5nm or more 50μm or less, an average particle diameter of the infrared opacifying particles 0.5μm or 10μm or less Therefore, mixing with silica particles tends to be easy. The average particle size of the infrared opaque particles is determined by the same method as that for the silica particles described above.
赤外線不透明化粒子は、粉体100質量%に対して、0質量%超49.5質量%以下であることが好ましく、2質量%以上30質量%以下であることがより好ましい。赤外線不透明化粒子が49.5質量%以下であることで、固体伝導による伝熱が小さく、200℃未満での断熱性能が高い傾向にある。赤外線不透明化粒子が2質量%以上であることで、200℃以上での断熱性能が向上する傾向にあり、赤外線不透明化粒子が30質量%以下であることで、シリカ粒子との混合が容易となる傾向にある。 The infrared opaque particles are preferably more than 0% by mass and 49.5% by mass or less, and more preferably 2% by mass to 30% by mass with respect to 100% by mass of the powder. When the infrared opaque particles are 49.5% by mass or less, heat transfer due to solid conduction is small, and heat insulation performance at less than 200 ° C. tends to be high. When the infrared opaque particles are 2% by mass or more, the heat insulation performance at 200 ° C. or higher tends to be improved, and when the infrared opaque particles are 30% by mass or less, mixing with silica particles is easy. Tend to be.
赤外線不透明化粒子の質量割合は、赤外線不透明化粒子の組成をSEM−EDX測定し、赤外線不透明化粒子のみが含有する元素を調べた後、その元素を蛍光X線分析法により定量することで、求めることができる。 The mass ratio of the infrared opaque particles is determined by measuring the composition of the infrared opaque particles by SEM-EDX, examining the elements contained only in the infrared opaque particles, and then quantifying the elements by fluorescent X-ray analysis. Can be sought.
<アルミナ粒子>
本実施形態の粉体は、アルミナ粒子をさらに含むことが、高い耐熱性を得られる観点から好ましい。アルミナ粒子は、組成式Al2O3で表される材料を含む粒子を指す。粉体に含まれるアルミナ粒子は、純粋なAl2O3で表される材料を含む粒子でもよく、Al及び種々の他元素との塩又は複合酸化物の材料を含む粒子であってもよい。具体的には、アルミニウムの酸化物(α−アルミナ、γ−アルミナ、β−アルミナ、θ−アルミナ、ヒュームドアルミナ、非晶質のアルミナなど)、水酸化アルミニウム、アルミニウム等を含む複合酸化物(シリカアルミナ、ゼオライト等)、炭化アルミニウム、窒化アルミニウム等の表面を酸化して得られた酸化物の材料を含む粒子等が挙げられる。
<Alumina particles>
The powder of the present embodiment preferably further contains alumina particles from the viewpoint of obtaining high heat resistance. Alumina particles refer to particles containing a material represented by the composition formula Al 2 O 3 . The alumina particles contained in the powder may be particles containing a material represented by pure Al 2 O 3 , or may be a particle containing a salt of Al and various other elements or a composite oxide material. Specifically, composite oxides containing aluminum oxide (α-alumina, γ-alumina, β-alumina, θ-alumina, fumed alumina, amorphous alumina, etc.), aluminum hydroxide, aluminum, and the like ( And particles containing an oxide material obtained by oxidizing the surface of silica alumina, zeolite, etc.), aluminum carbide, aluminum nitride and the like.
これらのアルミナ粒子の中では、断熱性能と耐熱性を両立する観点から、α−アルミナ、γ−アルミナ、θ−アルミナ、ヒュームドアルミナの材料を含む粒子が好ましい。また、成形時に粉体のかさ密度が大きくなり、成形が容易となる傾向にあることから、α−アルミナの材料を含む粒子がより好ましい。 Among these alumina particles, particles containing materials of α-alumina, γ-alumina, θ-alumina, and fumed alumina are preferable from the viewpoint of achieving both heat insulation performance and heat resistance. In addition, particles containing α-alumina material are more preferred because the bulk density of the powder increases during molding and the molding tends to be easy.
成形体に、α−アルミナ、γ−アルミナ、θ−アルミナの材料を含む粒子が含まれていることは、多孔質体の粉末X線回折測定(XRD)を測定することで確認できる。具体的には、そのXRDパターンが、α−アルミナではJCPDSカード番号46−1212、γ−アルミナではJCPDSカード番号23−1009、θ−アルミナではJCPDSカード番号35−0121が、示すd値の位置にピークを有することにより、確認できる。なお、α−アルミナではd値が2.5508(Å)、1.6016(Å)、2.0853(Å)、3.4797(Å)であることで確認でき、γ−アルミナではd値が1.3883(Å)、2.8370(Å)、2.7300(Å)、2.4440(Å)であることで確認でき、θ−アルミナではd値が2.7300(Å)、1.3880(Å)、2.8400(Å)、2.3120(Å)であることで確認できる。 It can confirm that the particle | grains containing the material of (alpha)-alumina, (gamma) -alumina, and (theta) -alumina are contained in the molded object by measuring the powder X-ray-diffraction measurement (XRD) of a porous body. Specifically, the XRD pattern has a JCPDS card number 46-1212 for α-alumina, a JCPDS card number 23-1009 for γ-alumina, and a JCPDS card number 35-0121 for θ-alumina. This can be confirmed by having a peak. In addition, in α-alumina, it can be confirmed that the d value is 2.5508 (Å), 1.6016 (Å), 2.0853 (Å), 3.49797 (Å), and in γ-alumina, the d value is 1.3883 (Å), 2.8370 (Å), 2.7300 (Å), 2.4440 (Å), and θ-alumina has a d value of 2.7300 (Å), 1. 3880 (Å), 2.8400 (Å), and 2.3120 (Å).
アルミナ粒子は、粉体100質量%に対して、Al2O3換算でアルミニウムを1質量%以上80質量%以下含むことが好ましく、1質量%以上40質量%以下含むことがより好ましく、1質量%以上25質量%以下含むことがさらに好ましい。アルミナ粒子が1質量%以上含むことで、900℃を超える温度にさらされた時に、成形体の断熱性能の変化が抑制される傾向にある。アルミナ粒子が80質量%以下含むことで、成形体の質量の増加と断熱性能の低下を抑制できる傾向にある。アルミナ粒子を25質量%以下含むことで、粉体の付着が小さくなる傾向にある。 The alumina particles preferably contain 1% by mass to 80% by mass of aluminum in terms of Al 2 O 3 with respect to 100% by mass of the powder, more preferably 1% by mass to 40% by mass. More preferably, the content is from 25% to 25% by mass. When the alumina particles are contained in an amount of 1% by mass or more, a change in the heat insulating performance of the molded body tends to be suppressed when exposed to a temperature exceeding 900 ° C. When the alumina particles are contained in an amount of 80% by mass or less, an increase in the mass of the molded body and a decrease in heat insulation performance tend to be suppressed. By containing 25% by mass or less of alumina particles, the adhesion of powder tends to be reduced.
アルミナ粒子の質量割合は、上述のシリカ粒子の含有量の測定と同じ方法で、蛍光X線測定により求められる。 The mass ratio of the alumina particles is determined by fluorescent X-ray measurement by the same method as that for measuring the content of silica particles.
粉体は、水が粉体又は成形体に浸み込み、ハンドリング性の低下、成形体の変形、及びひび割れ等が起こるのを抑制する観点から、撥水剤をさらに含むことが好ましい。撥水剤として、具体的には、パラフィンワックス、ポリエチレンワックス、アクリル・エチレン共重合体ワックス等のワックス系撥水剤;シリコーン樹脂、ポリジメチルシロキサン、アルキルアルコキシシラン等のシリコン系撥水剤;パーフロロアルキルカルボン酸塩、パーフロロアルキルリン酸エステル、パーフロロアルキルトリメチルアンモニウム塩等のフッ素系撥水剤、アルキル基やパーフルオロ基を含むアルコキシシラン等のシランカップリング剤、トリメチルシリルクロライドや1,1,1,3,3,3−ヘキサメチルジシラザン等のシリル化剤等が挙げられる。これらは1種または2種以上で使用することができる。これらはそのまま用いてもよいし、溶液やエマルジョンの形態で用いてもよい。これらの中で、ワックス系撥水剤、シリコン系撥水剤が好ましい。 The powder preferably further contains a water repellent from the viewpoint of preventing water from penetrating into the powder or the molded body to reduce handling properties, deformation of the molded body, cracking, and the like. Specific examples of water repellents include wax-based water repellents such as paraffin wax, polyethylene wax, and acrylic / ethylene copolymer wax; silicon-based water repellents such as silicone resin, polydimethylsiloxane, and alkylalkoxysilane; Fluorine-based water repellents such as fluoroalkylcarboxylates, perfluoroalkyl phosphates, perfluoroalkyltrimethylammonium salts, silane coupling agents such as alkoxysilanes containing alkyl groups and perfluoro groups, trimethylsilyl chloride and 1,1 Silylating agents such as 1,3,3,3-hexamethyldisilazane and the like. These can be used alone or in combination of two or more. These may be used as they are or in the form of a solution or an emulsion. Among these, a wax-based water repellent and a silicon-based water repellent are preferable.
十分な撥水効果を付与する観点から、撥水剤の質量に対する粉体全体の質量の比は、100/30以上100/0.1以下が好ましく、100/20以上100/0.5以下がより好ましく、100/10以上100/1以下がさらに好ましい。 From the viewpoint of imparting a sufficient water repellent effect, the ratio of the mass of the entire powder to the mass of the water repellent is preferably from 100/30 to 100 / 0.1, and preferably from 100/20 to 100 / 0.5. More preferably, it is 100/10 or more and 100/1 or less.
〔粉体の製造方法〕
本実施形態の粉体の製造方法は、シリカ粒子を含む粉体と、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維と、を混合する混合工程を有することが好ましい。
[Production method of powder]
The method for producing a powder according to the present embodiment preferably includes a mixing step of mixing a powder containing silica particles and an inorganic fiber containing 1 mass% or more and 40 mass% or less of iron in terms of Fe 2 O 3. .
シリカ粒子としては、従来の製法で製造されるシリカ成分を有する粒子を原料とすることができる。具体的には、原料となるシリカ粒子として、酸性又はアルカリ性の条件下での湿式法により、ケイ酸イオンを縮合して製造された粒子、湿式法でアルコキシシランを加水分解・縮合して製造されたシリカを含む無機化合物粒子、湿式法で製造されたシリカ成分を焼成して製造されたシリカ粒子等が挙げられる。また、シリカを含む無機化合物粒子としては、塩化物などケイ素の化合物を気相で燃焼して製造されたものでもよい。さらに、シリカ粒子は、ケイ素金属やケイ素を含む原料を加熱して得られたケイ素ガスを酸化、燃焼して製造されたものでも、ケイ石などを溶融して製造されたものでもよい。 As the silica particles, particles having a silica component produced by a conventional production method can be used as a raw material. Specifically, the silica particles used as a raw material are produced by condensing silicate ions by a wet method under acidic or alkaline conditions, and produced by hydrolyzing and condensing alkoxysilane by a wet method. Inorganic compound particles containing silica, silica particles produced by firing a silica component produced by a wet method, and the like. The inorganic compound particles containing silica may be produced by burning a silicon compound such as chloride in the gas phase. Further, the silica particles may be produced by oxidizing and burning silicon gas obtained by heating a raw material containing silicon metal or silicon, or may be produced by melting silica.
シリカを含む無機化合物粒子として、天然のケイ酸塩鉱物を使用することができる。天然の鉱物として、具体的には、カンラン石類、緑簾石類、石英、長石類、沸石類等が挙げられる。 A natural silicate mineral can be used as the inorganic compound particles containing silica. Specific examples of natural minerals include olivine, chlorite, quartz, feldspar, and zeolite.
シリカ粒子に含まれるシリカ成分以外の成分は、上記の製法において原料中に不純物として存在しているものを利用しても、シリカの製造プロセス中に添加してもよい。 Components other than the silica component contained in the silica particles may be used as impurities in the raw material in the above production method, or may be added during the silica production process.
公知のシリカの製法としては、以下のものが挙げられる。
(湿式法で合成されるシリカ)
ケイ酸ナトリウムを原料に酸性で製造されるゲル法シリカ。
ケイ酸ナトリウムを原料にアルカリ性で製造される沈降法シリカ。
アルコキシシランの加水分解・縮合で合成されるシリカ。
(乾式法で合成されるシリカ)
ケイ素の塩化物を燃焼して製造されるヒュームドシリカ。
ケイ素金属ガスを燃焼して製造されるシリカ。
フェロシリコン製造時等に副生するシリカヒューム。
アーク法やプラズマ法で製造されるシリカ。
粉砕したシリカ粉末を火炎中で溶融、球状化する溶融シリカ。
The following are mentioned as a manufacturing method of a well-known silica.
(Silica synthesized by wet method)
Gel silica produced with sodium silicate as a raw material.
Precipitated silica produced with alkalinity from sodium silicate.
Silica synthesized by hydrolysis and condensation of alkoxysilanes.
(Silica synthesized by dry method)
Fumed silica produced by burning silicon chloride.
Silica produced by burning silicon metal gas.
Silica fume by-produced during ferrosilicon production.
Silica produced by the arc method or plasma method.
Fused silica that melts and spheroidizes pulverized silica powder in a flame.
上記のシリカの中で、生産性とコストの観点から、ヒュームドシリカ、ケイ素金属ガスを燃焼して作られるシリカ、シリカヒューム、溶融シリカを用いることがより好ましい。 Among the above silica, fumed silica, silica produced by burning silicon metal gas, silica fume, and fused silica are more preferable from the viewpoint of productivity and cost.
〔混合工程〕
本実施形態の混合工程は、少なくともシリカ粒子と無機繊維とを混合し、さらに赤外線不透明化粒子とアルミナ粒子とを混合してもよい。シリカ粒子、及び無機繊維は、混合機(具体的には、改訂六版 化学工学便覧(丸善)に掲載されているもの等)を使用して混合することができる。混合機として、具体的には、容器回転型(容器自体が回転、振動、揺動する)として水平円筒型、V型(攪拌羽根が付いていてもよい)、ダブルコーン型、立方体型及び揺動回転型;機械撹拌型(容器は固定され、羽根などで撹拌する)として、単軸リボン型、複軸パドル型、回転鋤型、二軸遊星攪拌型、円錐スクリュー型、高速撹拌型、回転円盤型、ローラー付き回転容器型、撹拌付き回転容器型、高速楕円ローター型;流動撹拌型(空気、ガスによって撹拌する)として、気流撹拌型、重力による無撹拌型等が挙げられる。これらの混合機は、組み合わせて使用してもよい。
[Mixing process]
In the mixing step of the present embodiment, at least silica particles and inorganic fibers may be mixed, and infrared opaque particles and alumina particles may be further mixed. Silica particles and inorganic fibers can be mixed using a mixer (specifically, those listed in the revised sixth edition Chemical Engineering Handbook (Maruzen), etc.). Specifically, as a mixer, a container rotating type (the container itself rotates, vibrates and swings) is a horizontal cylindrical type, a V type (which may be equipped with a stirring blade), a double cone type, a cubic type and a shaking type. Dynamic rotating type; mechanical stirring type (container is fixed and stirred with blades, etc.), single axis ribbon type, double axis paddle type, rotary saddle type, biaxial planetary stirring type, conical screw type, high speed stirring type, rotation As a disk type, a rotating container type with a roller, a rotating container type with stirring, a high-speed elliptical rotor type; a flow stirring type (stirring by air or gas), an airflow stirring type, a non-stirring type by gravity and the like can be mentioned. These mixers may be used in combination.
混合工程は、粉砕機(具体的には、改訂六版 化学工学便覧(丸善)に掲載されているもの等)を使用して、粒子を粉砕したり、無機繊維を裁断したり、粒子や無機繊維の分散性を向上させながら混合してもよい。 The mixing process uses a pulverizer (specifically, those listed in the Revised Sixth Edition Chemical Engineering Handbook (Maruzen), etc.) to pulverize particles, cut inorganic fibers, You may mix, improving the dispersibility of a fiber.
粉砕機として、具体的には、ロールミル(高圧圧縮ロールミル、ロール回転ミル)、スタンプミル、エッジランナー(フレットミル、チリアンミル)、切断・せん断ミル(カッターミルなど)、ロッドミル、自生粉砕機(エロフォールミル、カスケードミルなど)、竪型ローラーミル(リングローラーミル、ローラーレスミル、ボールレースミル)、高速回転ミル(ハンマーミル、ケージミル、ディスインテグレーター、スクリーンミル、ディスクピンミル)、分級機内蔵型高速回転ミル(固定衝撃板型ミル、ターボ型ミル、遠心分級型ミル、アニュラー型ミル)、容器駆動媒体ミル(転動ボールミル(ポットミル、チューブミル、コニカルミル)、振動ボールミル(円形振動ミル、旋動振動ミル、遠心ミル)、遊星ミル、遠心流動化ミル)、媒体撹拌式ミル(塔式粉砕機、撹拌槽式ミル、横型流通槽式ミル、竪型流通槽式ミル、アニュラーミル)、気流式粉砕機(気流吸込型、ノズル内通過型、衝突型、流動層ジェット吹込型)、圧密せん断ミル(高速遠心ローラーミル、インナーピース式)、乳鉢、石臼等が挙げられる。これらの粉砕機は、組み合わせて使用してもよい。 Specific examples of pulverizers include roll mills (high-pressure compression roll mills, roll rotating mills), stamp mills, edge runners (fret mills, Chillian mills), cutting and shearing mills (cutter mills, etc.), rod mills, and self-pulverizing mills (Erofol). Mill, cascade mill, etc.), vertical roller mill (ring roller mill, rollerless mill, ball race mill), high-speed rotary mill (hammer mill, cage mill, disintegrator, screen mill, disc pin mill), high-speed rotary mill with built-in classifier (Fixed impact plate mill, turbo mill, centrifugal classification mill, annular mill), container drive media mill (rolling ball mill (pot mill, tube mill, conical mill)), vibration ball mill (circular vibration mill, rotational vibration mill, Centrifugal mill), planetary mill, centrifugal fluidizing mill) Medium agitation mill (tower crusher, agitation tank mill, horizontal flow tank mill, vertical flow tank mill, annular mill), airflow crusher (airflow suction type, nozzle passage type, collision type, flow) Layer jet blowing type), compaction shear mill (high-speed centrifugal roller mill, inner piece type), mortar, stone mill and the like. These pulverizers may be used in combination.
これらの混合機と粉砕機の中で、撹拌羽根を有する粉体混合機、高速回転ミル、分級機内蔵型高速回転ミル、容器駆動媒体ミル、圧密せん断ミルが、シリカ粒子等の粒子と無機繊維の分散性が向上する傾向にあるため、好ましい。シリカ粒子等の粒子と無機繊維の分散性をより向上させる観点から、撹拌羽根、回転板、ハンマープレート、ブレード、ピン等の先端の周速は、100km/h以上にすることが好ましく、200km/h以上がより好ましく、300km/h以上にすることがさらに好ましい。 Among these mixers and pulverizers, powder mixers with stirring blades, high-speed rotary mills, high-speed rotary mills with built-in classifiers, container drive media mills, compaction shear mills, particles such as silica particles and inorganic fibers This is preferable because the dispersibility tends to be improved. From the viewpoint of further improving the dispersibility of particles such as silica particles and inorganic fibers, the peripheral speed at the tips of stirring blades, rotating plates, hammer plates, blades, pins, etc. is preferably 100 km / h or more, and 200 km / h. h or higher is more preferable, and 300 km / h or higher is further preferable.
複数の種類の粒子を混合する場合には、かさ比重が小さい順に粒子を攪拌機又は粉砕機に投入することが好ましい。赤外線不透明化粒子を用いる場合は、シリカ粒子を混合した後に赤外線不透明化粒子を添加して混合し、その後無機繊維を添加して混合することが好ましい。 When mixing a plurality of types of particles, it is preferable to introduce the particles into a stirrer or a pulverizer in ascending order of bulk specific gravity. When using infrared opaque particles, it is preferable to add and mix infrared opaque particles after mixing silica particles, and then add and mix inorganic fibers.
粉体を断熱材として用いる場合は、成形等の工程を経ることなく、粉体を使用する箇所に充填しただけでそのまま用いてもよいし、粉体を加圧成形したものを断熱材として用いてもよい。 When using the powder as a heat insulating material, it may be used as it is without filling the part where the powder is used without going through a molding process or the like. May be.
本実施形態の粉体を含む成形体は、本実施形態の粉体を加圧成型することによって得ることができる。粉体を加圧成形する方法として、具体的には、金型プレス成形法(ラム式加圧成形法)、ラバープレス法(静水圧成形法)、押出成形法、従来から知られるセラミックス加圧成形法等が挙げられる。これらの中で、生産性の観点から、金型プレス成形法が好ましい。 The compact containing the powder of the present embodiment can be obtained by pressure molding the powder of the present embodiment. Specific examples of methods for pressure forming powders include: die press molding method (ram type pressure molding method), rubber press method (hydrostatic pressure molding method), extrusion molding method, and conventionally known ceramic pressing. Examples include molding methods. Among these, the die press molding method is preferable from the viewpoint of productivity.
金型プレス成形法又はラバープレス法で粉体を型に充填する場合には、粉体に振動を与えるなどして均一に充填することが、成形体の厚みが均一となる傾向にあるため、好ましい。また、型内を減圧、脱気しながら粉体を型に充填することは、短時間で成形できるため、生産性の観点から好ましい。 When filling a mold with powder by a mold press molding method or a rubber press method, it is likely that the thickness of the molded body tends to be uniform, such as by giving vibration to the powder uniformly. preferable. Moreover, filling the mold with the powder while reducing the pressure and degassing the mold is preferable from the viewpoint of productivity because it can be molded in a short time.
成形体のかさ密度は、0.25g/cm3以上2.0g/cm3以下が好ましく、0.25g/cm3以上1.7g/cm3以下がより好ましく、0.25g/cm3以上1.5g/cm3以下がさらに好ましい。かさ密度が0.25g/cm3以上2.0g/cm3以下であることで、運搬時の負担が軽減される傾向にある。具体的な測定方法は、後述の実施例に記載する方法により測定する。 The bulk density of the molded body is preferably from 0.25 g / cm 3 or more 2.0 g / cm 3 or less, more preferably 0.25 g / cm 3 or more 1.7 g / cm 3 or less, 0.25 g / cm 3 or more 1 More preferably, it is 5 g / cm 3 or less. When the bulk density is 0.25 g / cm 3 or more and 2.0 g / cm 3 or less, the burden during transportation tends to be reduced. A specific measuring method is measured by the method described in the examples described later.
成形は、加圧の圧力で制御してもよく、成形体のかさ密度により制御してもよい。ただし、成形の条件を加圧の圧力で制御する場合は、使用する粉体のすべり性、粉体の粒子間や細孔への空気の取り込み量等によって、加圧した状態で保持する時間の経過に伴って圧力値が変化する。それに対して、成形体のかさ密度により制御する場合は、時間の制御を要することなく、得られる成形体の最大荷重を目標値にし易く、生産管理が容易となる傾向にあるため好ましい。 Molding may be controlled by the pressure of pressurization, or may be controlled by the bulk density of the molded body. However, when the molding conditions are controlled by the pressure of the pressurization, the time of holding in the pressurized state depends on the slipperiness of the powder used, the amount of air taken in between the particles of the powder and the pores, etc. The pressure value changes with time. On the other hand, when controlling by the bulk density of the molded body, it is preferable because the maximum load of the obtained molded body can be easily set to the target value without requiring time control, and production management tends to be facilitated.
本実施形態の成形体は、0%以上5%以下の圧縮率における最大荷重が、0.7MPa以上であることが好ましい。具体的な測定方法は、後述の実施例に記載する方法により測定する。 In the molded body of the present embodiment, the maximum load at a compression rate of 0% or more and 5% or less is preferably 0.7 MPa or more. A specific measuring method is measured by the method described in the examples described later.
粉体、又は加圧成形中若しくは加圧成形後の成形体を、粉体又は成形体の耐熱性が十分である温度と時間の条件の範囲内で、加熱乾燥し、粉体又は成形体の吸着水を除去した後に実用に供すると、熱伝導率が低くなるため好ましい。さらに、加熱処理を施してもよい。 The powder or the molded body during or after pressure molding is heat-dried within the temperature and time conditions within which the heat resistance of the powder or molded body is sufficient, and the powder or molded body It is preferable to put it to practical use after removing the adsorbed water because the thermal conductivity is lowered. Furthermore, you may heat-process.
成形は、加圧成形のみでもよいが、加圧成形したものを加熱処理するのが好ましい。粉体を加圧成形したものに加熱処理を施すと、圧縮強度が向上する傾向にあり、特に成形体に対する荷重が大きい用途において好適に使用することができる傾向にある。 The molding may be performed only by pressure molding, but it is preferable to heat-treat the pressure molded product. When heat treatment is performed on a powder-molded powder, the compressive strength tends to be improved, and in particular, it tends to be suitably used in applications where the load on the molded body is large.
寸法安定性の観点から、加熱処理の温度は、その粉体又は成形体の使用最高温度より高温が好ましい。粉体又は成形体の用途により様々であるが、400℃以上1200℃以下が好ましく、500℃以上1200℃以下がより好ましく、600℃以上1200℃以下がさらに好ましい。 From the viewpoint of dimensional stability, the temperature of the heat treatment is preferably higher than the maximum use temperature of the powder or molded product. Although it varies depending on the use of the powder or molded product, it is preferably 400 ° C. or higher and 1200 ° C. or lower, more preferably 500 ° C. or higher and 1200 ° C. or lower, and further preferably 600 ° C. or higher and 1200 ° C. or lower.
粉体又は成形体の加熱処理の雰囲気としては、具体的には、空気中(又は大気中)、酸化性雰囲気中(酸素、オゾン、窒素酸化物、二酸化炭素、過酸化水素、次亜塩素酸、無機・有機過酸化物等)、及び不活性ガス雰囲気中(ヘリウム、アルゴン、窒素等)等が挙げられる。加熱処理時間は、加熱処理温度及び断熱材の量に応じて適宜選択すればよい。加熱処理は、上記粉体を使用する箇所に充填した後に施してもよいし、粉体を加圧成形したものに施してもよい。 Specifically, the atmosphere for the heat treatment of the powder or molded body is in the air (or in the air), in an oxidizing atmosphere (oxygen, ozone, nitrogen oxide, carbon dioxide, hydrogen peroxide, hypochlorous acid) And inorganic / organic peroxides), and in an inert gas atmosphere (helium, argon, nitrogen, etc.). The heat treatment time may be appropriately selected according to the heat treatment temperature and the amount of the heat insulating material. The heat treatment may be performed after filling the portion where the powder is used, or may be performed on a pressure-molded powder.
〔被包体〕
本実施形態の被包体は、上述の粉体及び/又は上述の成形体を含むコア材と、コア材を収容する外被材とを備える。なお、粉体又は成形体をコア材という場合がある。
[Encapsulation]
The enveloping body of this embodiment is provided with the core material containing the above-mentioned powder and / or the above-mentioned molded object, and the outer covering material which accommodates a core material. Note that the powder or the molded body may be referred to as a core material.
<外被材>
本実施形態の外被材としては、粉体及び/又は成形体を含むコア材を収容可能な限り、特に限定されないが、具体的には、ガラスクロス、アルミナ繊維クロス、シリカクロス等の無機繊維織物、無機繊維編物、ポリエステルフィルム、ポリエチレンフィルム、ポリプロピレンフィルム、ナイロンフィルム、ポリエチレンテレフタレートフィルム、フッ素系樹脂フィルム等の樹脂フィルム、プラスチック−金属フィルム、アルミニウム箔、ステンレス箔、銅箔等の金属箔、セラミックペーパー、無機繊維不織布、有機繊維不織布、ガラス繊維紙、炭素繊維紙、ロックウール紙、無機充填紙、有機繊維紙、セラミックコーティング、フッ素樹脂コーティング、シロキサン樹脂コーティング等の樹脂コーティング等が挙げられる。
<Coating material>
The jacket material of the present embodiment is not particularly limited as long as it can accommodate a core material including powder and / or a molded body, and specifically, inorganic fibers such as glass cloth, alumina fiber cloth, silica cloth, and the like. Woven fabric, inorganic fiber knitted fabric, polyester film, polyethylene film, polypropylene film, nylon film, polyethylene terephthalate film, resin film such as fluororesin film, plastic-metal film, metal foil such as aluminum foil, stainless steel foil, copper foil, ceramic Examples include paper, inorganic fiber nonwoven fabric, organic fiber nonwoven fabric, glass fiber paper, carbon fiber paper, rock wool paper, inorganic filler paper, organic fiber paper, ceramic coating, fluororesin coating, siloxane resin coating, and other resin coatings.
外被材の厚みは、被包体を断熱材として用いる場合には、外被材の熱容量を小さくする観点から、薄い方が好ましいが、使用状況や必要な強度等に応じて適宜選択することが可能である。 The thickness of the jacket material is preferably selected from the viewpoint of reducing the heat capacity of the jacket material when the enveloping body is used as a heat insulating material. Is possible.
外被材がコア材を使用する温度でも安定なものからなる場合には、使用時においても、外被材がコア材である粉体又は成形体を収容した状態であることができる。高温で使用される被包体の場合には、使用後のコア材の取扱いがし易い観点から、耐熱性の高い外被材が好ましい。ただし、本明細書中の「外被材」は、コア材の使用時にコア材を収容しているものの他、コア材の運搬や施工の工程でコア材を収容しているものを包含する。つまり、外被材は運搬時や施工時にのみコア材を保護し、使用時には溶融及び/又は揮発してしまうものを包含するので、外被材そのもの及び外被材に含まれる有機成分は、コア材の使用温度で溶融又は消失をしてもよい。 When the outer cover material is stable even at the temperature at which the core material is used, the outer cover material can be in a state of containing powder or a molded body that is the core material even during use. In the case of an enveloping body used at a high temperature, an outer covering material having high heat resistance is preferable from the viewpoint of easy handling of the core material after use. However, the “cover material” in the present specification includes not only the core material that is accommodated when the core material is used, but also the material that accommodates the core material in the process of transporting or constructing the core material. In other words, the jacket material protects the core material only during transportation and construction, and includes those that melt and / or volatilize during use, so the jacket material itself and the organic components contained in the jacket material are It may melt or disappear at the use temperature of the material.
外被材としては、被覆工程が容易である観点から、ガラスクロス、アルミナ繊維クロス、シリカクロス等の無機繊維織物、無機繊維編物、ポリエステルフィルム、ポリエチレンフィルム、ポリプロピレンフィルム、ナイロンフィルム、ポリエチレンテレフタレートフィルム、フッ素系樹脂フィルム等の樹脂フィルム、プラスチック−金属フィルム、アルミニウム箔、ステンレス箔、銅箔等の金属箔、セラミックペーパー、無機繊維不織布、有機繊維不織布、ガラス繊維紙、炭素繊維紙、ロックウール紙、無機充填紙、有機繊維紙等のようなシート形状のものが好ましい。 As the covering material, from the viewpoint that the coating process is easy, inorganic fiber fabrics such as glass cloth, alumina fiber cloth, silica cloth, inorganic fiber knitted fabric, polyester film, polyethylene film, polypropylene film, nylon film, polyethylene terephthalate film, Resin film such as fluorine resin film, plastic-metal film, aluminum foil, stainless steel foil, metal foil such as copper foil, ceramic paper, inorganic fiber nonwoven fabric, organic fiber nonwoven fabric, glass fiber paper, carbon fiber paper, rock wool paper, Sheet-shaped paper such as inorganic filled paper, organic fiber paper and the like is preferable.
被包体が高温で使用される場合には、外被材としては、熱的な安定性の観点から、ガラスクロス、アルミナ繊維クロス、シリカクロス等の無機繊維織物、無機繊維編物、セラミックペーパー、無機繊維不織布がより好ましい。外被材としては、強度の観点から、無機繊維織物がさらに好ましい。 When the enveloping body is used at a high temperature, as the covering material, from the viewpoint of thermal stability, inorganic fiber fabrics such as glass cloth, alumina fiber cloth, silica cloth, inorganic fiber knitted fabric, ceramic paper, An inorganic fiber nonwoven fabric is more preferable. As the jacket material, an inorganic fiber fabric is more preferable from the viewpoint of strength.
被包体は、シリカ粒子と無機繊維とを含み、使用状況に応じてさらに、径が比較的大きなシリカ粒子、赤外線不透明化粒子、アルミナ粒子を添加して形成した粉体を、コア材として、袋状又はチューブ状に加工した外被材に充填したものでもよい。また、当該粉体を加圧成形して成形体とした後にコア材とし、外被材で被覆したものでもよい。 The encapsulant includes silica particles and inorganic fibers, and further, depending on the use situation, a powder formed by adding silica particles having a relatively large diameter, infrared opaque particles, and alumina particles, as a core material, What was filled in the jacket material processed into the bag shape or the tube shape may be used. Further, the powder may be formed by pressing the powder into a molded body, which is then used as a core material and covered with a jacket material.
外被材が形成する容積に対する粉体の充填率は、粉体をコア材とする場合に、粉体を使用する対象物に応じて適宜設定することが可能である。成形体をコア材とする場合には、後述するように、粉体と外被材を共に加圧成形してもよいし、粉体を加圧成形した後に外被材で被覆することも可能である。 When the powder is used as the core material, the filling rate of the powder with respect to the volume formed by the jacket material can be set as appropriate according to the object using the powder. When using the molded body as a core material, as described later, both the powder and the jacket material may be pressure-molded, or the powder may be pressure-molded and covered with the jacket material. It is.
コア材を外被材で被覆する方法は特に限定されず、コア材の調製や成形と外被材での被覆を同時に実施してもよいし、コア材を調製又は成形後に外被材で被覆してもよい。 The method of coating the core material with the jacket material is not particularly limited, and the core material may be prepared or molded and coated with the jacket material at the same time, or the core material may be coated with the jacket material after preparation or molding. May be.
外被材が、無機繊維織物、樹脂フィルム、プラスチック−金属フィルム、金属箔、セラミックペーパー、無機繊維不織布、有機繊維不織布、ガラス繊維紙、炭素繊維紙、ロックウール紙、無機充填紙、有機繊維紙等のシート状の形態である場合には、具体的には、無機繊維糸又は樹脂繊維糸等での縫合、外被材の接着固定、縫合と接着の両方等で被覆することが可能である。 Cover material is inorganic fiber fabric, resin film, plastic-metal film, metal foil, ceramic paper, inorganic fiber nonwoven fabric, organic fiber nonwoven fabric, glass fiber paper, carbon fiber paper, rock wool paper, inorganic filler paper, organic fiber paper In the case of a sheet-like form such as, specifically, it is possible to cover with sewing with inorganic fiber yarn or resin fiber yarn, adhesive fixing of the jacket material, both sewing and bonding, etc. .
シート状の外被材が、樹脂フィルム、プラスチック−金属フィルム、金属箔等である場合は、被覆工程の容易さの観点から、真空パック、シュリンクパックが好ましい。 When the sheet-shaped outer covering material is a resin film, a plastic-metal film, a metal foil, or the like, a vacuum pack or a shrink pack is preferable from the viewpoint of ease of the coating process.
外被材がセラミックコーティング、樹脂コーティング等で形成される場合には、コア材に刷毛又はスプレーで塗布することにより、コア材を外被材で被覆することが可能である。 When the jacket material is formed by ceramic coating, resin coating, or the like, the core material can be coated with the jacket material by applying the core material with a brush or spray.
加圧成形したコア材と外被材とを備える被包体に、線状のくぼみを設け、被包体に柔軟性を付与することも可能である。線の形態は、被包体の使用状況に応じて直線状、曲線状、破線状等を選ぶことができ、これらのうち2種類以上を組み合わせてもよい。線の太さ、くぼみの深さは被包体の厚み、強度、使用状況に応じて決定される。 It is also possible to provide a linear recess in the enveloping body including the core material and the outer covering material that have been pressure-molded, thereby imparting flexibility to the enveloping body. The form of the line can be selected from a straight line shape, a curved line shape, a broken line shape, and the like according to the usage state of the enveloping body, and two or more of these may be combined. The thickness of the line and the depth of the dent are determined according to the thickness, strength, and usage of the envelope.
外被材は、コア材の表面全体を被覆していてもよいし、コア材を部分的に被覆していてもよい。 The jacket material may cover the entire surface of the core material, or may partially cover the core material.
熱接着性を有する外被材を用いる場合には、製袋充填機を使用することが可能である。製袋充填機として、具体的には、製袋しながら粉体を充填、シール、カッティングを行う機能を有するもの、外被材を製袋しカットした袋に粉体を充填後シールする機能を有するもの等が挙げられる。粉体を袋内に充填するためには、シュート(粉体を高所から低所に流し送るための樋状又は管状の用具)が用いられるが、粉体の帯電が少ないと、シュート内及びシール面への粉体の付着が抑制される傾向にある。 When using a jacket material having thermal adhesiveness, a bag making and filling machine can be used. Specifically, as a bag making and filling machine, it has the function of filling, sealing, and cutting powder while making bags, and the function of sealing the envelope material after making it into a bag that has been cut and filled with powder. And the like. In order to fill the powder into the bag, a chute (a bowl-like or tubular tool for flowing the powder from a high place to a low place) is used. There is a tendency that adhesion of the powder to the sealing surface is suppressed.
本実施形態の被包体は、粉体及び成形体よりも取扱いがより容易となり、施工性にも優れる傾向にある。 The enveloping body of this embodiment becomes easier to handle than powders and molded bodies, and tends to be excellent in workability.
本実施形態の粉体、成形体及び被包体は、断熱材に用いることが好ましい。断熱材に用いられることで、熱伝導率が低く、取扱性及び製造性に優れた断熱材が得られる。本実施形態の粉体、成形体及び被包体は、断熱材の他に、吸音材、防音材、遮音材、反響防止材、消音材、研磨剤、触媒担体、吸着剤、芳香剤又は殺菌剤等の薬剤を吸着する担体、脱臭剤、消臭剤、調湿材、充填剤、顔料等にも好ましく用いることができる。 It is preferable to use the powder, the molded body, and the encapsulated body of this embodiment for a heat insulating material. By being used for a heat insulating material, a heat insulating material having low thermal conductivity and excellent handleability and manufacturability can be obtained. The powder, molded body, and encapsulant of the present embodiment include a heat absorbing material, a sound absorbing material, a sound insulating material, a sound insulating material, an anti-reflection material, a sound deadening material, an abrasive, a catalyst carrier, an adsorbent, an fragrance, or a sterilizer. It can also be preferably used for a carrier that adsorbs a drug such as an agent, a deodorant, a deodorant, a humidity control material, a filler, a pigment, and the like.
以下、具体的な実施例及び比較例を挙げて本実施形態をより詳細に説明するが、本実施形態はその要旨を超えない限り、これらの実施例及び比較例によって何ら限定されるものではない。以下の実施例及び比較例において、粉体、成形体は、以下のとおりに評価した。 Hereinafter, the present embodiment will be described in more detail with specific examples and comparative examples, but the present embodiment is not limited by these examples and comparative examples unless they exceed the gist thereof. . In the following Examples and Comparative Examples, powders and molded products were evaluated as follows.
(1)無機繊維に対するXRFによる組成分析、鉄の含有量測定
無機繊維1gと、結晶セルロース粉末のフナセルII粉末(商品名、フナコシ株式会社製)1gを、乳鉢で30分間混合後、混合粉末2gを内径25mm、厚さ5mm、幅3mmの塩化ビニル製のリング内に充填し、プレス機により厚さ3mmに加圧成形し、蛍光X線分析の測定試料とした。走査型蛍光X線分析装置ZSX PrimusII(商品名、株式会社リガク製)に、あらかじめフナセルII粉末を、組成C6H10O5のフラックスとして化合物登録しておき、測定試料を全定性分析した後、試料モデルはバルク、成分形態は酸化物、フラックスはフナセルII粉末、希釈率は1を選択し、SQX計算を実施して、無機繊維100質量%に対する、無機繊維中に含まれる鉄をFe2O3に換算して含有量(質量%)を測定した。同様に、ケイ素をSiO2に換算して、アルミニウムをAl2O3に換算して含有量(質量%)等により、表1に記載するように各種の組成について含有量を測定した。
(1) Composition analysis by XRF for inorganic fiber, measurement of iron content 1 g of inorganic fiber and 1 g of Funacelle II powder (trade name, manufactured by Funakoshi Co., Ltd.) of crystalline cellulose powder for 30 minutes in a mortar, and then 2 g of mixed powder Was filled in a ring made of vinyl chloride having an inner diameter of 25 mm, a thickness of 5 mm, and a width of 3 mm, and press-molded to a thickness of 3 mm by a press machine to obtain a measurement sample for fluorescent X-ray analysis. A compound model is previously registered as a flux of composition C6H10O5 in a scanning X-ray fluorescence analyzer ZSX Primus II (trade name, manufactured by Rigaku Co., Ltd.), and a sample model is bulky after a qualitative analysis of the measurement sample. The component form is oxide, the flux is Funasel II powder, the dilution rate is 1, and the SQX calculation is performed to convert the iron contained in the inorganic fiber to Fe 2 O 3 with respect to 100% by mass of the inorganic fiber. The content (mass%) was measured. Similarly, the content was measured for various compositions as described in Table 1 by converting silicon to SiO 2 and converting aluminum to Al 2 O 3 and content (% by mass).
(2)粉体の撹拌による帯電量評価、付着性評価
粉体試料50gを、撹拌シールを取り付けた2Lのφ140mmのSUS304製容器に入れ、SUS316製75φmmの4枚角度付きパドルが2つ付いたSUS316撹拌シャフトを、撹拌シールを介して撹拌モーターSM−101(アズワン株式会社製)に取り付け、容器を密封後、3000rpmで1分間回転させた。その後、容器蓋を開け、容器を180度回転させ、内部の粉体を排出した。その際に、粉体の帯電量(nC/g)を、春日電気株式会社製クーロンメーターNK−1001とファラデーケージKQ−1400を使用して測定した。付着性評価は、容器に付着し回収できなかった粉体の質量(g)を測定した。
(2) Charge amount evaluation by powder agitation and adhesion evaluation 50 g of a powder sample was put in a 2 L φ140 mm SUS304 container equipped with a stirring seal, and two SUS316 75 φmm 4-paddles with an angle were attached. A SUS316 agitation shaft was attached to an agitation motor SM-101 (manufactured by As One Co., Ltd.) via an agitation seal, and the container was sealed and rotated at 3000 rpm for 1 minute. Thereafter, the container lid was opened, the container was rotated 180 degrees, and the internal powder was discharged. At that time, the charge amount (nC / g) of the powder was measured using a Coulomb meter NK-1001 and Faraday cage KQ-1400 manufactured by Kasuga Electric Co., Ltd. In the adhesion evaluation, the mass (g) of the powder that adhered to the container and could not be collected was measured.
(3)成形体、焼成硬化体のかさ密度測定
縦約30cm、横約30cm、厚さ約20mmの成形体及びその焼成硬化体の試料の寸法と質量を測定し、質量を体積で割ることにより、かさ密度(g/cm3)を測定した。
(3) Measurement of bulk density of molded body and fired and cured body By measuring the size and mass of a sample of about 30 cm in length, about 30 cm in width and about 20 mm in thickness, and a sample of the fired and cured body, and dividing the mass by the volume. The bulk density (g / cm 3 ) was measured.
(4)成形体、焼成硬化体の30℃の熱伝導率測定
縦約30cm、横約30cm、厚み約20mmの形状に成形した多孔質体である成形体及びその焼成硬化体を試料とし、30℃での熱伝導率(W/m・K)を、ヒートフローメーター HFM 436 Lambda(商品名、NETZSCH社製)を使用して熱伝導率を測定した。較正は、JISA1412−2に従い、密度163.12kg/m3、厚さ25.32mmのNIST SRM 1450c校正用標準板を使用して、高温側と低温側の温度差が20℃の条件において、15、20、24、30、40、50、60、65℃で予め実施した。
(4) Measurement of thermal conductivity at 30 ° C. of molded body and fired and cured body A molded body that is a porous body molded into a shape having a length of about 30 cm, a width of about 30 cm, and a thickness of about 20 mm and its fired and cured body were used as samples. The thermal conductivity (W / m · K) at ° C. was measured using a heat flow meter HFM 436 Lambda (trade name, manufactured by NETZSCH). Calibration is performed according to JIS A1412-2 using a NIST SRM 1450c calibration standard plate having a density of 163.12 kg / m 3 and a thickness of 25.32 mm under the condition that the temperature difference between the high temperature side and the low temperature side is 20 ° C. 20, 24, 30, 40, 50, 60, and 65 ° C. in advance.
(5)成形体、焼成硬化体の帯電性評価
静電気電荷拡散率測定装置NS−D100(商品名、株式会社ナノシーズ社製)を用いて、温度20℃、湿度50%RHの恒温恒湿器内で、直径約4cm10mm厚みの円板状に成形した成形体及びその焼成硬化体である試料に対し、コロナ放電部位、及び表面電位計との距離を10mmにセットした。6kVの針電極からのコロナ放電による帯電を10秒間行い、コロナ帯電を行った1秒後及び10秒後の表面電位(kV)を表面電位計により測定を行った。測定は、JIS C 61340−2−1に準拠して実施した。
(5) Evaluation of chargeability of molded body and fired cured body In a constant temperature and humidity chamber at a temperature of 20 ° C. and a humidity of 50% RH using an electrostatic charge diffusivity measuring device NS-D100 (trade name, manufactured by Nano Seeds Co., Ltd.) Then, the distance from the corona discharge site and the surface potential meter was set to 10 mm with respect to the molded body formed into a disk shape having a diameter of about 4 cm and a thickness of 10 mm and the sample which was the fired and cured body. Charging by corona discharge from a 6 kV needle electrode was performed for 10 seconds, and the surface potential (kV) after 1 second and 10 seconds after corona charging was measured with a surface potentiometer. The measurement was performed according to JIS C 61340-2-1.
(6)焼成硬化体の最大荷重の測定
焼成硬化体である試料から1辺が多孔質体の厚みに等しい立方体を切り出して作製し、精密万能試験機オートグラフAG−100KN(株式会社島津製作所製)を使用して、試料を厚みに対して0%以上5%以下の圧縮率における最大荷重(MPa)を測定した。
(6) Measurement of maximum load of fired and cured body A cube having one side equal to the thickness of the porous body is cut out from a sample that is a fired and cured body, and is produced by a precision universal testing machine Autograph AG-100KN (manufactured by Shimadzu Corporation) ) Was used to measure the maximum load (MPa) at a compression rate of 0% or more and 5% or less of the sample with respect to the thickness.
[実施例1]
平均粒子径が14nmのヒュームドシリカ1600gと、平均粒子径が120nmのシリカヒューム4000gと、ケイ酸ジルコニウム1200gと、αアルミナ800gを、ハンマーミルで均一に混合し、混合粉体を得た。
[Example 1]
1600 g of fumed silica having an average particle diameter of 14 nm, 4000 g of silica fume having an average particle diameter of 120 nm, 1200 g of zirconium silicate, and 800 g of α-alumina were uniformly mixed with a hammer mill to obtain a mixed powder.
この混合粉体3960gと、鉄の含有量がFe2O3換算で26.9%であり、平均繊維径が13μm、平均繊維長が6mmのバサルト繊維40gを、高速せん断ミキサーで混合し、粉体を得た。この粉体の撹拌による帯電量評価、付着性評価(上記(2))を行った。無機繊維の無機繊維中の上記(1)のXRFによる組成分析結果を表1に、帯電性評価、付着性評価の結果を表2に示す。 3960 g of this mixed powder and 40 g of basalt fiber having an iron content of 26.9% in terms of Fe 2 O 3 , an average fiber diameter of 13 μm, and an average fiber length of 6 mm were mixed with a high-speed shear mixer, Got the body. The charge amount evaluation and adhesion evaluation (above (2)) were performed by stirring this powder. Table 1 shows the results of composition analysis by XRF of (1) above in the inorganic fibers of the inorganic fibers, and Table 2 shows the results of chargeability evaluation and adhesion evaluation.
縦30cm、横30cm、厚み2cm、かさ密度が0.40g/cm3の成形体を得られるように、縦30cm、横30cmの金型に上記で得られた粉体を720g充填し、加圧成形し、かさ密度が0.40g/cm3の成形体を得た。この成形体の30℃での上記(4)の熱伝導率を評価した。結果を表2に示す。 In order to obtain a molded body having a length of 30 cm, a width of 30 cm, a thickness of 2 cm, and a bulk density of 0.40 g / cm 3 , 720 g of the above-obtained powder was filled in a 30 cm long and 30 cm wide mold and pressed. Molded to obtain a molded body having a bulk density of 0.40 g / cm 3 . The thermal conductivity of the above (4) at 30 ° C. of this molded body was evaluated. The results are shown in Table 2.
直径4cm、厚み1cm、かさ密度が0.40g/cm3の成形体を得られるように、直径4cmの金型に上記で得られた粉体を5g充填し、加圧成形し、かさ密度が0.40g/cm3の成形体を得た。この成形体の上記(5)の帯電性を評価した。結果を表2に示す。 In order to obtain a molded body having a diameter of 4 cm, a thickness of 1 cm, and a bulk density of 0.40 g / cm 3 , 5 g of the above-obtained powder was filled in a 4 cm diameter mold and pressure-molded. A molded body of 0.40 g / cm 3 was obtained. The chargeability of (5) above of this molded product was evaluated. The results are shown in Table 2.
縦30cm、横30cm、厚み2cm、かさ密度が0.50g/cm3の成形体を得られるように、縦30cm、横30cmの金型に上記で得られた粉体を900g充填し、加圧成形し、かさ密度が0.50g/cm3の成形体を得た。この成形体を1000℃1時間焼成し、厚み1.8cm、かさ密度0.62g/cm3の、焼成硬化体を得た。この焼成硬化体に対して、上記(4)の30℃での熱伝導率と、上記(6)の圧縮強度を評価した。結果を表2に示す。 In order to obtain a molded body having a length of 30 cm, a width of 30 cm, a thickness of 2 cm, and a bulk density of 0.50 g / cm 3 , 900 g of the powder obtained above was filled in a 30 cm long and 30 cm wide mold and pressed. Molded to obtain a molded body having a bulk density of 0.50 g / cm 3 . This molded body was fired at 1000 ° C. for 1 hour to obtain a fired and cured body having a thickness of 1.8 cm and a bulk density of 0.62 g / cm 3 . The thermal conductivity at 30 ° C. of (4) above and the compressive strength of (6) above were evaluated for this fired cured product. The results are shown in Table 2.
直径4cm、厚み1.2cm、かさ密度が0.50g/cm3の成形体を得られるように、直径4cmの金型に上記で得られた粉体を8g充填し、加圧成形し、かさ密度が0.50g/cm3の、円板状の成形体を得た。この成形体を1000℃1時間焼成し、厚み1.0cm、かさ密度0.62g/cm3の、焼成硬化体を得た。この焼成硬化体に対して、上記(5)の帯電性を評価した。結果を表2に示す。 In order to obtain a molded body having a diameter of 4 cm, a thickness of 1.2 cm, and a bulk density of 0.50 g / cm 3 , 8 g of the above-obtained powder was filled in a 4 cm diameter mold, and pressure-molded. A disk-shaped molded body having a density of 0.50 g / cm 3 was obtained. This molded body was fired at 1000 ° C. for 1 hour to obtain a fired and cured body having a thickness of 1.0 cm and a bulk density of 0.62 g / cm 3 . The chargeability of the above (5) was evaluated for this fired and cured product. The results are shown in Table 2.
上記の厚み1.8cm、かさ密度0.62g/cm3の焼成硬化体をさらに2枚調製し、裁断により直径28cm、厚さ1.8cmの2枚の円板状試料を作製した。保護熱板法熱伝導率測定装置(英弘精機株式会社製)により、800℃での熱伝導率を測定したところ、0.115(W/m・K)であった。結果を表2に示す。 Two more fired and cured bodies having a thickness of 1.8 cm and a bulk density of 0.62 g / cm 3 were prepared, and two disk-shaped samples having a diameter of 28 cm and a thickness of 1.8 cm were prepared by cutting. It was 0.115 (W / m * K) when the heat conductivity in 800 degreeC was measured with the protection hot plate method thermal conductivity measuring apparatus (made by Eihiro Seiki Co., Ltd.). The results are shown in Table 2.
[比較例1]
無機繊維として、平均繊維径が10μm、平均繊維長が6mmの、Eガラスファイバーを用いた以外は、実施例1と同様の方法で、粉体を得た。上記(1)の無機繊維のXRFによる組成分析を、結果を表1に示す。この粉体の撹拌による帯電量評価、付着性評価(上記(2))を行った。結果を表2に示す。
[Comparative Example 1]
A powder was obtained in the same manner as in Example 1 except that E glass fiber having an average fiber diameter of 10 μm and an average fiber length of 6 mm was used as the inorganic fiber. The composition analysis by XRF of the inorganic fiber (1) is shown in Table 1. The charge amount evaluation and adhesion evaluation (above (2)) were performed by stirring this powder. The results are shown in Table 2.
得られた粉体以外は実施例1と同様に、縦30cm、横30cm、厚み2cm、かさ密度が0.40g/cm3の成形体を得て、上記(4)の30℃での熱伝導率を評価した。結果を表2に示す。 Except for the obtained powder, a molded body having a length of 30 cm, a width of 30 cm, a thickness of 2 cm, and a bulk density of 0.40 g / cm 3 was obtained in the same manner as in Example 1, and the heat conduction at 30 ° C. of (4) above. Rate was evaluated. The results are shown in Table 2.
得られた粉体以外は実施例1と同様に、直径4cm、厚み1cm、かさ密度が0.40g/cm3の成形体を得て、上記(5)の帯電性を評価した。結果を表2に示す。 Except for the obtained powder, a molded body having a diameter of 4 cm, a thickness of 1 cm, and a bulk density of 0.40 g / cm 3 was obtained in the same manner as in Example 1, and the chargeability of the above (5) was evaluated. The results are shown in Table 2.
得られた粉体以外は実施例1と同様に、縦30cm、横30cm、厚み2cm、かさ密度が0.50g/cm3の成形体を950℃1時間焼成し、厚み1.8cm、かさ密度0.62g/cm3の焼成硬化体を得た。この焼成硬化体に対して、上記(4)の30℃での熱伝導率と、上記(6)の圧縮強度を評価した。結果を表2に示す。 Except for the obtained powder, as in Example 1, a shaped body having a length of 30 cm, a width of 30 cm, a thickness of 2 cm, and a bulk density of 0.50 g / cm 3 was fired at 950 ° C. for 1 hour, and the thickness was 1.8 cm. A fired and cured body of 0.62 g / cm 3 was obtained. The thermal conductivity at 30 ° C. of (4) above and the compressive strength of (6) above were evaluated for this fired cured product. The results are shown in Table 2.
得られた粉体以外は実施例1と同様に、直径4cm、厚み1.2cm、かさ密度が0.50g/cm3の成形体を得られるように、直径4cmの金型に上記で得られた粉体を8g充填し、加圧成形し、かさ密度が0.50g/cm3の、円板状の成形体を得た。この成形体を950℃1時間焼成し、厚み1.0cm、かさ密度0.62g/cm3の焼成硬化体を得た。この焼成硬化体に対して上記(5)の帯電性を評価した。結果を表2に示す。 Except for the obtained powder, it was obtained in the same manner as in Example 1 so that a molded body having a diameter of 4 cm, a thickness of 1.2 cm, and a bulk density of 0.50 g / cm 3 was obtained. 8 g of the obtained powder was filled and pressure-molded to obtain a disk-shaped molded body having a bulk density of 0.50 g / cm 3 . This molded body was fired at 950 ° C. for 1 hour to obtain a fired and cured body having a thickness of 1.0 cm and a bulk density of 0.62 g / cm 3 . The chargeability of the above (5) was evaluated for the fired cured product. The results are shown in Table 2.
Claims (8)
前記無機繊維は、前記無機繊維100質量%に対して、Fe2O3換算で鉄を1質量%以上40質量%以下含む無機繊維である、粉体。 Silica particles and inorganic fibers,
The inorganic fibers, with respect to the inorganic fibers 100 wt%, an inorganic fiber comprising Fe 2 O 3 40 wt% or more 1 wt% of iron in terms of the following powder.
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