WO2002044301A2 - Particles with opalescent effect - Google Patents
Particles with opalescent effect Download PDFInfo
- Publication number
- WO2002044301A2 WO2002044301A2 PCT/EP2001/012788 EP0112788W WO0244301A2 WO 2002044301 A2 WO2002044301 A2 WO 2002044301A2 EP 0112788 W EP0112788 W EP 0112788W WO 0244301 A2 WO0244301 A2 WO 0244301A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particles
- spheres
- monodisperse spheres
- suspension
- monodisperse
- Prior art date
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- 239000002245 particle Substances 0.000 title claims abstract description 51
- 230000000694 effects Effects 0.000 title claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 49
- 239000000758 substrate Substances 0.000 claims description 33
- 239000000725 suspension Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 24
- -1 Sb2O Inorganic materials 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 13
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 13
- 239000000084 colloidal system Substances 0.000 claims description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims description 12
- 150000004706 metal oxides Chemical class 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 230000005693 optoelectronics Effects 0.000 claims description 4
- 239000002861 polymer material Substances 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 150000004770 chalcogenides Chemical class 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 239000011118 polyvinyl acetate Substances 0.000 claims description 2
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 229920000620 organic polymer Polymers 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 16
- 239000007787 solid Substances 0.000 abstract description 9
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 15
- 241000894007 species Species 0.000 description 13
- 230000008569 process Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 10
- 239000003086 colorant Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 239000011022 opal Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 239000004038 photonic crystal Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000007858 starting material Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000003491 array Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 238000012552 review Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000010437 gem Substances 0.000 description 2
- 229910001751 gemstone Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 244000241796 Christia obcordata Species 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229910000003 Lead carbonate Inorganic materials 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Inorganic materials O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- AOPJVJYWEDDOBI-UHFFFAOYSA-N azanylidynephosphane Chemical compound P#N AOPJVJYWEDDOBI-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012053 oil suspension Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920005553 polystyrene-acrylate Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 238000002444 silanisation Methods 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
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3045—Treatment with inorganic compounds
- C09C1/3054—Coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/36—Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/254—Polymeric or resinous material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/256—Heavy metal or aluminum or compound thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/256—Heavy metal or aluminum or compound thereof
- Y10T428/257—Iron oxide or aluminum oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/259—Silicic material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/294—Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
- Y10T428/2942—Plural coatings
- Y10T428/2949—Glass, ceramic or metal oxide in coating
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/2962—Silane, silicone or siloxane in coating
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the field of the invention relates to particles with opalescent effect - especially 3- D structural color pigments - based on solid colloidal crystals of monodispersed spheres and the manufacturing processes suitable for large-scale production of such solid colloidal crystal products.
- the 3-D structural color pigments yield color effects as a result of light diffraction by ordered three-dimensional structures of colloidal monodisperse spheres. They diffract light because the lattice spacings, and therefore, the modulation of refractive index in their structures are in the range of the wavelength of light.
- the color effects are optimized by adjusting the refractive index difference between the monodisperse spheres and the media in between the spheres. This may be accomplished by partially or completely infiltrating the monodisperse spherebased crystal structure with one or more suitable secondary materials.
- the resultant high quality colloidal crystals may also be used as photonic crystals for potential photonic and optoelectronic applications.
- the present invention deals with particles with opalescent effect that contain a sphere based crystal structure (or super-lattice) built up by monodisperse spheres and one or more secondary types of much smaller colloidal particles occupying partially or completely the empty spaces between the monodisperse spheres.
- the smaller colloidal particles in the structure modify the refractive index contrast between the monodisperse spheres and the media in between them. They also act as binding agents to hold the sphere based structure more strongly together.
- the monodisperse spheres suitable for the particles with opalescent effect typically have a standard deviation of the particle size of less than 5 %, preferably about 2 %.
- the existing physical effect pigments or colorants are essentially exclusively based on layered structures with refractive indexes alternating in only one dimension.
- Typical products include, for example, pearlescent pigments based on bismuth oxychlo de or lead carbonate crystalline platelets, interference pigments based mica flakes or alumina flakes, and gonio-chromatic pigments based on silica flakes, metal flakes or liquid crystal platelets. These products have been extensively reviewed by Pfaff and Reynders recently (Chemical Reviews, 1999, 99(7), 1963-1981 ).
- This invention also deals with a method of manufacturing thin layer (flaky) crystals of monodisperse spheres using a substrate coating technology.
- the substrate may be a static, flat surface or a moving belt.
- the latter is known as a web coating process (US 3,138,475) which was expanded to produce silica and titania flakes for layered interference colorants (World Patents 93/08237, 97/43346 and 97/43348).
- This web coating technology is capable of large scale production of 3-D structural color pigments of the current invention.
- the method may also be used to produce photonic crystals based on normal opal or inverse opal structures suitable for photonic and optoelectronic device applications.
- this invention also deals with the use of the particles or of thin layer flaky crystals produced with the method described herein for photonic and optoelectronic device applications.
- Figure 1 schematically presents layer-based 1-D, rod-based 2-D and sphere- based 3-D structures and their possible interaction with light.
- Figure 2 is a schematic flowsheet of a preferred embodiment of the process of the invention.
- Figures 3A and 3B are electron micrographs of silica sphere crystals.
- silica spheres were first synthesized and fractionated into narrow particle size fractions. Then spheres with the desired size uniformity and range were assembled into closely packed arrays by sedimentation or centrifugation. The packed arrays were finally stabilized by heating or by the use of a cement-like material to bond the spheres together.
- a cement-like material to bond the spheres together.
- a second material typically with high refractive index such as metal oxides, carbon or metal was then introduced into the structure by infiltrating the gaps between the spheres with a desired precursor material followed by certain treatments to convert precursor material into desired material. Finally, the polymer or silica spheres were removed from the structure by chemical or thermal processes. In photonics applications, polymer or silica does not have enough high refractive index to provide a strong optical effect. Infiltration with high refractive index material is generally necessary.
- a new type of 3-D structural color pigments is produced via a substrate coating process of the type shown in Figure 2.
- the process involves three production stages.
- the suspension preparation stage a suspension of monodisperse spheres is prepared at a suitable concentration, in an appropriate solvent, and with a suitable amount of one or more colloidal species with much smaller particle size than the monodisperse spheres for refractive index adjustment and structure binding.
- crystallization stage the suspension is brought onto a flat substrate, static or constantly moving with desired thickness of the suspension layer; the spheres are crystallized into closely packed layers along with the evaporation of the solvent; the crystalline layer is then initially dried and removed from the substrate at small pieces of flakes.
- the product finishing stage the crystal flakes are further dried, calcined, milled to reduce the particle size to an appropriate range, and then classified into different fractions of final products.
- the monodisperse spheres may comprise almost any materials which are sufficently transparent for the wavelengths of the desired light reflections, so that this light is able to penetrate several sphere diameters deep into the particle.
- Preferred spheres comprise metal chalcogenides, preferably metal oxides or metal pnictides, preferably nitrides or phosphides.
- Metals in the sense of these terms are all elements which may occur as an electropositive partner in comparison to the counterions, such as the classic metals of the transition groups and the main group metals of main groups one and two, but also including all elements of main group three and also silicon, germanium, tin, lead, phosphorous, arsenic, antimony and bismuth.
- the preferred metal chalcogenides and metal pnictides include, in particular, silicon dioxide, aluminium oxide, titanium dioxide, zirconium dioxide, gallium nitride, boron nitride and aluminum nitride and also silicon nitride and phosphorous nitride.
- Starting material for the production of the particles of the invention preferably comprises monodisperse spheres of silicon dioxide which are obtainable, for example, by the process described in US 4,911 ,903.
- the spheres are produced by hydrolytic polycondensation of tetraalkoxysilanes in an aqueous-ammoniacal medium, a sol of primary particles being produced first of all and then the SiO 2 particles obtained being brought to the desired particle size by continuous, controlled addition of tetraalkoxysilane. With this process it is possible to produce monodisperse Si0 2 spheres having average particle diameters of between 0.05 and 10 ⁇ m with a standard deviation of 5%.
- Further preferred starting material comprises SiO 2 spheres coated with nonabsorbing metal oxides, such as Ti ⁇ 2, Zr0 2 , Zn0 2 , SnO 2 or Al 2 O 3 , for example.
- metal oxides such as Ti ⁇ 2, Zr0 2 , Zn0 2 , SnO 2 or Al 2 O 3 .
- the production of SiO 2 spheres coated with metal oxides is described in more detail in US 5,846,310, DE 198 42 134 and DE 199 29 109, for example.
- Coating with absorbing metal oxides, such as the iron oxides Fe 3 0 4 and/or Fe 2 O 3 also leads to particles which may be used in accordance with the invention.
- monodisperse spheres of nonabsorbing metal oxides such as TiO 2 , ZrO 2 , ZnO 2 , SnO 2 or AI 2 O 3 or metal oxide mixtures. Their preparation is described, for example, in EP 0 644 914. Furthermore, the process according to EP 0 216 278 for producing monodisperse SiO 2 spheres may be transferred readily and with the same result to other oxides.
- tetraethoxysilane, tetrabutoxytitanium, tetrapropoxyzirconium or mixtures thereof are added in one shot with intensive mixing and the resulting mixture is stirred intensively for a further 20 seconds, forming a suspension of monodisperse spheres in the nanometer range.
- the spheres are separated off in a conventional manner, by centrifuging, for example, and are washed and dried.
- Monodisperse polymer spheres as well for example polystyrene or polymethyl methacrylate, may be used as starting material for the production of the particles of the invention.
- Spheres of this kind are available commercially.
- Bangs Laboratories Inc. (Carmel, USA) offer monodisperse spheres of a very wide variety of polymers.
- suitable starting material for producing the pigments of the invention comprises monodisperse spheres of polymers which contain included particles, for example metal oxides.
- Such materials are offered by the company micro capseries- undmaschines GmbH in Rostock, Germany.
- microencapsulations are manufactured on the basis of polyesters, polyamides and natural and modified carbohydrates.
- monodisperse spheres of metal oxides coated with organic materials for example silanes.
- the monodisperse spheres are dispersed in alcohols and modified with common organoalkoxysilanes.
- the silanization of spherical oxide particles is also described in DE 43 16 814.
- the suspension ready for crystallization may be simply prepared by mixing a monodisperse sphere suspension and the sols containing the desired colloid species if they are already in a desired solvent in a desired concentration. However, extra steps may be needed to prepare the suspension.
- a suspension of monodisperse spheres is mixed with desired amounts of one or more smaller particle species regardless of their solvents and concentrations.
- the resultant suspension is centrifuged to separate the particles from their solvents. Then the particle mixture is redispersed in a desired solvent and at a suitable concentration ready for crystallization.
- the redispersion may be done by mechanical mixing and agitation followed by, if necessary, ultrasonic treatment. If necessary, the centrifugation and redispersion may be repeated one or more times before proceeding to the crystallization stage.
- the concentration of the sphere suspension for crystallization may vary from -5% to -65% in weight.
- a preferred concentration is from -20% to -50%.
- a concentration from -40% to -50% is more preferred.
- a large number of different solvents may be used for the preparation of the suspension. Examples include but are not limited to water, ethanol, methanol, 1- or 2-propanol, acetone, acetonitrile, dichloromethane, methyl chloroform, methyl acetate, butyl acetate, ethylene glycol, among many others.
- the preferred solvents are water and ethanol on the ' basis of economic, health, safety and environmental considerations.
- ethanol is more preferred than water.
- a thin layer of the ethanol suspension on an appropriate substrate can be crystallized (solvent removed) rapidly even under normal evaporation conditions. With the help of an infrared heater, the solvent removal may be completed in a couple of minutes without compromising much of the crystalline quality.
- the preferred sphere size ranges from ca. 150 nm to ca. 450 nm.
- the size of the secondary colloid species used for refractive index adjustment and structure stabilization may vary from -5 nm up to about one-third in diameter of the size of the monodisperse spheres used. Preferably, it is from -10 nm to - 50 nm. Too large a size of the colloid species may cause structural distortions and reduce the optical effect.
- colloidal species examples include but are not limited to metal oxide sols e.g. SiO 2 , AI2O3, TiO 2 , SnO 2 , Sb 2 O5, Fe2 ⁇ 3 , Zr ⁇ 2, Ce ⁇ 2 and Y 2 O 3 ; metal colloids e.g. gold, silver and copper; and colloidal polymers such as, for example, poly(methyl methacrylate), poly(vinyl acetate), polyacrylontrile and poly(styrene-co-butadiene).
- metal oxide sols e.g. SiO 2 , AI2O3, TiO 2 , SnO 2 , Sb 2 O5, Fe2 ⁇ 3 , Zr ⁇ 2, Ce ⁇ 2 and Y 2 O 3
- metal colloids e.g. gold, silver and copper
- colloidal polymers such as, for example, poly(methyl methacrylate), poly(vinyl acetate), polyacrylontrile and poly(styrene-co-butadiene).
- colloidal species that can effectively bind the structure together with enough mechanical strength after final treatment. It is possible that one colloidal species does both refractive index adjustment and binding. In this case, only one species is necessary.
- the optimum amount of the colloidal species needed can be determined experimentally by routine experimentation. The optimized amount of the colloids would result in the best crystal quality, the best color quality and highest mechanical stability. Typically, it varies from -5% to -25% in weight with respect to the monodisperse spheres used. In the cases where centrifugation is needed in the suspension preparation, an extra amount of the colloidal species is needed taking into account the possible incomplete isolation of the smaller colloid particles.
- substrate materials that may be used for the production of thin layer crystals of monodisperse spheres include but are not limited to glass, metals, e.g. stainless steel and aluminum, and polymer materials e.g. polypropylene, polystyrene, poly(methyl pentene), polycarbonate, poly(ethylene terephthalate), just to name a few.
- Pretreatment of the substrate surface with dilute acids or bases may be needed in order to make it more wettable for the colloid suspension to be used. If a moving substrate for large scale production is concerned, polymer materials are preferred due to their flexibility and low cost.
- the thickness of the monodisperse spherebased crystal layers may be estimated by taking into account the amount and concentration of the suspension, and surface area of substrate being covered.
- Achievable layer thicknesses by this process ranges from -20 ⁇ m to over 5 mm, preferably, -100 ⁇ m to -1000 ⁇ m.
- Evaporation crystallization and initial stage drying may be accomplished either at room temperature or under heat.
- Preferred heaters are those that use infrared irradiation sources, which may be easily incorporated into a web-coating equipment for the moving substrate process.
- the collection of the layered crystals as millimeter sized flakes may be done by simply brushing them off the substrate. At this stage, the crystals are not fully stabilized and still fragile. Excess mechanical impact should be avoided to keep the sphere based structure intact.
- the crystals undergo finishing treatments and are processed into final products.
- Typical finishing steps include drying, heat treatment or calcination, milling, and classification.
- the calcination temperature ranges from 400°C to 1100°C, preferably from 600°C to 800°C.
- An alternative modified substrate coating method may also be used to produce 3- D color pigments with controlled crystal size and shape. In this way, the milling and classification steps in the product finishing stage described above may not be needed.
- the key modification to the above method is the selection of substrate materials. Unlike the above method, where the substrate and the suspension are compatible so that the suspension can very well wet the substrate, an incompatible substrate is chosen. Instead of a uniform layer, the suspension would stay on the substrate as individual small drops. After evaporation / crystallization, these drops would become solid crystalline particles.
- the size of the crystalline particles may be controlled by controlling the size of the drops and the concentration of the suspension.
- the shape of the crystalline particles may be controlled to certain degrees by changing substrates or by changing the surface nature of a substrate. This way, one may be able to control the contact angle of a suspension on a substrate. By adjusting the contact angle, one may be able to achieve disc-like, ring-like and even ball-like particles.
- micro pipettes or syringes may be used to generate the droplets.
- spraying devices or even inkjet technology may be used.
- Solid substrates are preferred. For example, any hydrophobic polymer substrate may be used for water suspension and a hydrophyllic polymer substrate can be used for oil suspensions.
- a Teflon substrate in particular may be used for both water and ethanol suspensions. This would thus be an improvement over the method of Velev et. al generating shape controlled, polymer sphere based photonic crystals (Science, 2000, 287, 2240) by carrying out crystallization on a surface of a fluorinated oil.
- 3-D structural color pigments include coatings, paints, cosmetic formulations and polymer plastics.
- the pigments would be incorporated in the formulation in an analogous manner to known formulation containing 2-D color pigments.
- a Merck KGaA's silica monospheres were used as raw materials for the production of the 3-D structural color pigment of this invention.
- the sample came as a water suspension at a concentration of 11 % in weight.
- 120 g of silica sphere suspension was mixed with 8 g of a silica sol from Nissan Chemicals (Snowtex-40) having a particle size distribution of 11 - 14 nm and a concentration of 40 - 41 % in water.
- the mixture was centrifuged at 3000 rpm for 30 minutes to separate the solid from the liquid.
- the solid was redispersed in anhydrous ethanol (reagent grade from Alfa Aesar) to the original volume by mechanical stirring and ultrasonic treatment. The solid was separated again by centrifugation and redispersed again in ethanol to the half of the original volume.
- the suspension so prepared was divided into 4 equal parts and each was added to a glass Petri dish having a flat bottom and about 175 cm 2 in surface area. The suspension films in the dishes were left to evaporate / crystallize at room temperature overnight. Then the initially dried crystalline films was collected as small irregular shaped platelets, dried at 110°C for 6 hours and cilcined at 800°C for 8 hours. The platelets were finally ground into smaller sizes and screened to desired size ranges. The product showed a strong greenish diffraction color at a viewing angle close to normal axis of the crystalline surface and reddish color at an angle far away from the normal axis.
- Example 3 Same as in Example 1 , but 8 g of tin(IV) oxide sol was used instead of silica sol.
- the tin oxide sol was purchased from Alfa Aesar having an average particle size of 15 nm and a concentration of 15 wt. % in water dispersion. Both the colors and mechanical strength were comparable to the product from Example 1.
- the resultant products are shown in Figures 3A and 3B.
- Figure 3A the spheres are shown bound together with nanometer sized tin oxide colloids.
- the necks formed by the tin oxide colloid between neighboring spheres are clearly visible.
- Example 2 Same as in Example 1 , but 4 g of the silica sol as in Example 1 and 4 g of Sn ⁇ 2 sol as in Example 2 was used. The product showed both colors and mechanical strength comparable to that from Example 1.
- Example 2 Same as in Example 1 , but Petri dishes made of polymethylpentene instead of glass were used. The evaporation / crystallization was performed under a infrared heater at about 50°C. The process was virtually completed in about 15 minutes. The product shows comparable properties as that from Example 1.
- Example 2 120 g of the silica sphere suspension same as that used in Example 1 was added to glass cylinder and was left undisturbed for 3 days at room temperature. At the bottom of cylinder, a layer of colloidal crystal formed as indicated by strong iridescent colors. The colloidal crystal portion was collected by gently decanting away the upper liquid. Then concentrated suspension collected this way was mixed with 1.5 g of Snowtex-40 as in Example 1. The mixture was added into 2 glass dishes and evaporated at room temperature for about 24 hours. The product was further processed the same way as described in Example 1. It showed comparable color and mechanical strength.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US10/433,000 US20040071965A1 (en) | 2000-11-30 | 2001-11-05 | Particles with opalescent effect |
AU2002229534A AU2002229534A1 (en) | 2000-11-30 | 2001-11-05 | Particles with opalescent effect |
EP01990389A EP1337600A2 (en) | 2000-11-30 | 2001-11-05 | Particles with opalescent effect |
JP2002546650A JP2004514558A (en) | 2000-11-30 | 2001-11-05 | Particles with milky effect |
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US25393200P | 2000-11-30 | 2000-11-30 | |
US60/253,932 | 2000-11-30 |
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WO2002044301A2 true WO2002044301A2 (en) | 2002-06-06 |
WO2002044301A3 WO2002044301A3 (en) | 2003-01-23 |
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PCT/EP2001/012788 WO2002044301A2 (en) | 2000-11-30 | 2001-11-05 | Particles with opalescent effect |
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US (2) | US20040071965A1 (en) |
EP (1) | EP1337600A2 (en) |
JP (1) | JP2004514558A (en) |
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TW (1) | TW567223B (en) |
WO (1) | WO2002044301A2 (en) |
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Also Published As
Publication number | Publication date |
---|---|
EP1337600A2 (en) | 2003-08-27 |
AU2002229534A1 (en) | 2002-06-11 |
US20040071965A1 (en) | 2004-04-15 |
TW567223B (en) | 2003-12-21 |
US20030008771A1 (en) | 2003-01-09 |
WO2002044301A3 (en) | 2003-01-23 |
US6756115B2 (en) | 2004-06-29 |
JP2004514558A (en) | 2004-05-20 |
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