CN1229110A - 带有蓝色主色的干涉颜料 - Google Patents
带有蓝色主色的干涉颜料 Download PDFInfo
- Publication number
- CN1229110A CN1229110A CN99101400A CN99101400A CN1229110A CN 1229110 A CN1229110 A CN 1229110A CN 99101400 A CN99101400 A CN 99101400A CN 99101400 A CN99101400 A CN 99101400A CN 1229110 A CN1229110 A CN 1229110A
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- CN
- China
- Prior art keywords
- pigment
- metal oxide
- oxide
- layer
- value
- 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
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- 239000000049 pigment Substances 0.000 title claims abstract description 61
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 40
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 39
- 238000000576 coating method Methods 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 11
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 239000011521 glass Substances 0.000 claims abstract description 9
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000003513 alkali Substances 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 13
- 229910000765 intermetallic Inorganic materials 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims description 11
- 230000007062 hydrolysis Effects 0.000 claims description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000005321 cobalt glass Substances 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- 229960001866 silicon dioxide Drugs 0.000 claims description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000012634 fragment Substances 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000004040 coloring Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000012876 carrier material Substances 0.000 abstract 1
- 239000010941 cobalt Substances 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 abstract 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- CRHLEZORXKQUEI-UHFFFAOYSA-N dialuminum;cobalt(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Co+2].[Co+2] CRHLEZORXKQUEI-UHFFFAOYSA-N 0.000 abstract 1
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- 239000000243 solution Substances 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012265 solid product Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003086 colorant Substances 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- KGQGQKPCLGRZAZ-UHFFFAOYSA-N oxocobalt;hydrate Chemical compound O.[Co]=O KGQGQKPCLGRZAZ-UHFFFAOYSA-N 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- 241001062009 Indigofera Species 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 150000003608 titanium Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002515 CoAl Inorganic materials 0.000 description 2
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 229940097275 indigo Drugs 0.000 description 2
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 241001599088 Grammica Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 229940103272 aluminum potassium sulfate Drugs 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000009500 colour coating Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- -1 metal oxide compound Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- TWWDDFFHABKNMQ-UHFFFAOYSA-N oxosilicon;hydrate Chemical compound O.[Si]=O TWWDDFFHABKNMQ-UHFFFAOYSA-N 0.000 description 1
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 1
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000012982 x-ray structure analysis Methods 0.000 description 1
Classifications
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- 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
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0024—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index
- C09C1/003—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer
- C09C1/0039—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating high and low refractive indices, wherein the first coating layer on the core surface has the high refractive index comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
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- 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
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- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/02—Amorphous compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- 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
- C01P2004/88—Thick layer coatings
-
- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
- C09C2200/1004—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
- C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/302—Thickness of a layer with high refractive material
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/303—Thickness of a layer with low refractive material
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- C—CHEMISTRY; METALLURGY
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- 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
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/306—Thickness of an absorbing layer
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- 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
- C09C2210/00—Special effects or uses of interference pigments
- C09C2210/60—Interference with laser-light, laser markable pigments
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- 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
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/10—Wet methods, e.g. co-precipitation
- C09C2220/106—Wet methods, e.g. co-precipitation comprising only a drying or calcination step of the finally coated pigment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
本发明公开了一种带有蓝色主色的多层干涉颜料,该颜料由碎片状载体材料和涂层组成,而涂层由以下结构组成;(i)第一层,为高折射率的无色、透明金属氧化物层,(ii)第二层,为低折射率的无色、透明金属氧化物层,(iii)第三层,为铝酸钴、含钴玻璃或氧化钴的外部层。第一层和第三层也可颠倒。所用的高折射率的金属氧化物是二氧化钛、二氧化锆或氧化锡。所用的低折射率的金属氧化物是二氧化硅或氧化铝。
Description
本发明涉及带有蓝色主色的多层干涉颜料。
具有干涉色的颜料是众所周知的。它们含有着色剂或着色金属氧化物,后者也可形成产生干涉色的层。由该方法产生的颜色实际上其作用受到限制。特别是,具有蓝色或浅蓝色的颜料到现在仍未获得满意的色调。另外由于着色剂可大大减少干涉颜料的化学稳定性和热稳定性,所需颜色的选择亦受到限制。
US3951679描述了一种颜料,它以用金属氧化物层涂敷的云母为基础,并可另外载有普鲁土蓝颜色涂层。通过沉淀在基体上的铁化合物与水溶性的六氰基高铁酸盐反应从而形成普鲁土蓝层。该颜料缺点是普鲁土蓝在200-300℃温度下将会分解。
US4968351描述了一种珍珠光泽颜料,它用吸附的着色剂着色,色淀涂敷在着色剂层上以便强化着色剂的吸附。该颜料缺点是当与有机溶剂接触时有机着色剂将从干涉颜料中分离。还有,有机着色剂损害了该颜料的气候稳定性。
US5169442描述了一种由基体和面层组成的蓝-绿颜料,基体包括用金属氧化物涂敷的云母,而面层由氧化镁、氧化钙、氧化钴、和二氧化钛的氧化物混合物组成。然而,该颜料的主色不是纯蓝色。
本发明的目的是提供一种带有蓝色主色的干涉颜料,该颜料具有常规商业干涉颜料的光稳定性、化学稳定性、和气候稳定性。
由带有蓝色主色的多层干涉颜料来实现本发明的目的,该颜料由碎片状载体材料和涂层组成,而涂层由以下结构组成;
(i)第一层,为高折射率的无色、透明金属氧化物层,
(ii)第二层,为低折射率的无色、透明金属氧化物层,
(iii)第三层,为铝酸钴、含钴玻璃或氧化钴的外层。
本发明目的可由另一种由带有蓝色主色的多层干涉颜料来实现,该颜料由碎片状载体材料和涂层组成,而涂层由以下结构组成;
(i)第一层,为铝酸钴、含钴玻璃或氧化钴层,
(ii)第二层,为低折射率的无色、透明金属氧化物层,
(iii)第三层,为高折射率的无色、透明金属氧化物外层。
也可由本发明颜料的制备方法来实现本发明的目的,其中:
-将碎片状载体材料悬浮在水中,并将悬浮液加热到50-100℃,在适合于水解的PH下加入水溶性金属化合物,以便使高折射率的金属氧化物的水合物沉淀在悬浮的颗粒上面,确定各金属氧化物水合物沉淀所需的PH值,并通过同时加入酸或碱使PH保持恒定。
-随后用碱将PH值调整到4-10,并加入水溶性金属化合物,以便使低折射率的金属氧化物水合物沉淀在悬浮的颗粒上面,通过同时加入酸或碱使PH保持恒定。
-随后冲洗所获得的产物,在60-180℃下干燥和在500-1100℃下煅烧。
-随后将产物悬浮在水中,并在3-10的PH值下通过加入相应的水溶性金属化合物并使之水解从而用氧化钴和氧化铝的水合物涂敷产物,通过同时加入碱使PH值保持恒定。
-随后冲洗产物,在60-180℃下干燥和在500-1100℃下煅烧。
也可由本发明颜料的制备方法来实现本发明的目的,其中:
-将碎片状载体材料悬浮在水中,并将悬浮液加热到50-100℃,在3-10的PH值下通过加入相应的水溶性金属化合物并使之水解从而用氧化钴和氧化铝的水合物涂敷载体材料,通过同时加入碱使PH值保持恒定。
-随后用碱将PH值调整到4-10,并加入水溶性金属化合物,以便使低折射率的金属氧化物水合物沉淀在悬浮的颗粒上面,通过同时加入酸或碱使PH保持恒定。
-随后在适合水解的PH值下加入水溶性金属化合物,以便使高折射率的金属氧化物的水合物沉淀在悬浮的颗粒上面,确定各金属氧化物水合物沉淀所需的PH值,并通过同时加入酸或碱使PH值保持恒定。
-随后冲洗产物,在60-180℃下干燥和在500-1100℃下煅烧。
本发明也涉及本发明颜料用于油漆、印刷油墨、塑料、化妆品和陶瓷釉及玻璃釉的应用。
出于这一目的,它们可与常规商业颜料一起作为混合物而使用,其实例是无机和有机吸附颜料、金属-效果的颜料和LCP颜料。
本发明颜料合适的载体材料是天然或合成的、本身无色的碎片状材料,优选的载体材料是层状硅酸盐、金属氧化物碎片状粉末和玻璃碎片及陶瓷碎片。给出特别优选的实例是云母、滑石、高岭土、合成云母、和氧化铝及二氧化硅碎片状粉末。
二氧化硅碎片状粉末按照国际申请WO93/08237通过水玻璃溶液的固化和水解在连续带上进行生产。
载体材料的尺寸不是关键的,并可与特别应用相匹配。通常,碎片状载体材料厚度为0.05-5μm,特别是为0.2-2.0μm,其他两个尺寸长和宽通常为2-100μm,特别是为5-50μm。
颜料各层的厚度对于颜料的光学性能是重要的,对于具有强干涉色的颜料来说,各层的厚度必须彼此相适应。还有,通过合适地选择层的厚度,颜色可获得特别强烈的变化,而这种变化又是目测角的函数。例如,这可通过沉淀较厚的SiO2层(厚度大于100nm)从而形成干涉色强烈地取决于所说目测角的颜料来达到。
本发明颜料各层的厚度如下:
高折射率金属氧化物:70-110nm
低折射率金属氧化物:60-110nm
着色层: 50-90nm
例如,这使得本发明颜料各组成达到以下比例:
25-40重量%载体材料,
0.1-3重量%SnO2,
20-40重量%TiO2(高折射率金属氧化物),
10-20重量%SiO2(低折射率金属氧化物),
10-35重量%CoAl2O4。
当二氧化钛用于第一层时,二氧化锡仅用于促进金红石发生变体。其直接沉淀在载体材料上。在US4867794中更详细地描述了该技术。
优选地用湿化学方法涂敷金属氧化物层,可使用为制备珍珠光泽颜料而开发的湿化学涂敷技术;例如,在以下文献中描述了这种技术:DE1467468、DE1959988、DE2009566、DE2214545、DE2215191、DE2244298、DE2313331、DE2522572、DE3137808、DE3137809、DE3151343、DE3151354、DE3151355、DE3211602、DE3235017、或其它专利文献和其它公开出版物。
对于涂层来说,将基体颗粒悬浮在水中,并在适合于水解的PH值下加入一种或多种可水解的金属盐,而且金属盐选择要使金属氧化物和/或金属氧化物水合物直接沉淀在颗粒上而在任何情况下又不会产生第二次沉淀。通常通过同时加入计量的碱使PH值保持恒定。
还有,也可在流化床反应器中使用气相涂敷方法进行涂敷。例如,可使用在EP0045851和EP0106235中提出的用于制备珍珠光泽颜料的方法。
作为高折射率的金属氧化物,可使用二氧化钛、二氧化锆或氧化锡,给出优选的实例是二氧化钛。作为低折射率的金属氧化物,可使用二氧化硅、或氧化铝,给出优选的实例是二氧化硅。
对于涂敷二氧化钛层而言,给出优选的方法是在US3553001中所述的方法。将钛盐水溶液缓慢地加入到已加热到大约50-100℃,特别是70-80℃的待涂敷材料的悬浮液中,通过同时加入计量的碱、如氨水或碱金属氢氧化物水溶液而使大约0.5-5,特别是1.5-2.5的PH值基本保持恒定。一旦TiO2沉淀层达到所需的厚度,即停止加入钛盐溶液和碱。该方法也称滴定工艺,由于它避免了过量的钛盐,所以是值得注意的。这可通过在单位时间内向水解反应仅提供数量为均匀涂层所必需的、且该数量在单位时间内被待涂敷颗粒的有效表面积所吸收的水合TiO2来实现。因此没有产生没有沉淀在待涂敷表面上的水合二氧化钛。
对于涂敷二氧化硅层而言,可使用以下方法:将硅酸钠溶液经计量加入到已加热到50-100℃,特别是70-80℃的待涂敷材料的悬浮液中。通过同时加入10%盐酸使4-10、优选为6.5-8.5的PH值保持恒定。加入硅酸盐溶液后接着再搅拌30分钟。
从US4084983中知道氧化铝水合物沉淀在碎片状载体材料上的有关内容。将材料悬浮在水中,将该悬浮液谨慎地加热到较高的温度,例如40-95℃。随后将水溶性铝盐如氯化铝、硝酸铝、硫酸钾铝或硫酸铝的酸性水溶液或铝酸盐如铝酸钠或铝酸钾的碱性水溶液加入到悬浮液中。在盐溶液中的铝离子浓度为0.1-5摩尔/升。同时,加入碱或酸以使PH值保持在3-10、优选在4-9之间。特别是,合适的碱包括碱金属氢氧化物和氢氧化铵,优选为含水NaOH或氨气。在加入酸的情况下,给出优选的实例是HCl、H2SO4或HNO3。
控制碱或酸的加入以使悬浮液的PH值在沉淀期间尽可能保持恒定。
在EP0342533中更详细地描述了氧化钴水合物沉淀的有关内容。其在4-9的PH值下进行。由于氧化钴水合物和氧化铝水合物的沉淀条件实际上是相同的,两种氧化物水合物可发生共沉淀。
如果氧化钴用于着色层,用上述方法同样可沉淀氧化钴水合物。
如果含钴玻璃用于着色层,则发生如下过程:
氧化钴水合物和氧化硅水合物在上述条件下作为混合沉淀相共沉淀在载体材料上形成第一层或第三层。在该情况下,在产物煅烧期间形成玻璃结构。
通式为MxWO3的钨青铜可同样用于着色层。接着用氢或另一种合适的还原剂还原沉淀在载体材料上的碱金属钨酸盐以便形成通式为M0.3WO3的化合物。这些钨酸盐颜色是蓝-紫色的。
另外,可使最终的颜料进行后涂敷或后处理过程,这样就进一步增加了颜料的光稳定性、气候稳定性和化学稳定性,或便于颜料的处理,特别是便于将其引入到不同的介质中。例如,合适的后涂敷和后处理方法是在DE-C2215191、DE-A3151354、DE-A3235017或DE-A3334598中描述的那些方法。
以下实施例用于说明本发明,但不是限制本发明。实施例1
将100克云母(10-60μm)悬浮在2升去离子水中,并将悬浮液加热到75℃,同时搅拌。用稀HCl使PH值为1.8,并以2毫升/分钟的速度加入在50毫升的去离子水中有3.2克SnCl4·5H2O和10毫升37%HCl的溶液。在滴加期间用32%NaOH使PH值保持恒定。搅拌30分钟后,同样以2毫升/分钟的速度计量450毫升TiCl4溶液(400克/升)。通过同时加入32%NaOH使PH值保持稳定。随后用NaOH将PH值调整到7.0并搅拌混合物30分钟。现在以2毫升/分钟的速度计量水玻璃溶液(135克水玻璃、相对于SiO2为27%、用135克水稀释),通过滴加10%HCl使PH值保持恒定。在滴加完毕后,在75℃下搅拌10分钟。随后,抽真空过滤悬浮液并用去离子水冲洗固体产物以除去盐,而且在110℃下干燥。随后,在800℃下煅烧30分钟,将产物过筛并再一次悬浮在2升去离子水中。用NaOH将PH值调整到7.5,并且在加入在1200毫升去离子水中有132克Co(NO3)2·6H2O和218克AlCl3·6H2O的溶液期间使PH值保持恒定,以2毫升/分钟的速度滴加。随后搅拌该悬浮液30分钟并抽真空过滤,用去离子水冲洗固体产物从而除去盐,并在110℃下干燥。随后在1000℃下煅烧干燥产物30分钟,并且在冷却后过筛。获得290克带有蓝色主色的金色干涉颜料。
根据X-射线结构分析,本发明颜料由云母、金红石变体型的TiO2和CoAl2O4(尖晶石)组成。
该颜料的光活性在常规商业TiO2颜料的范围内。
水浸泡试验(1层***、常规涂层材料)表明短期耐候性非常好。
灰度值(DIN54001;ISO标准105部分A02):
16h/66℃=5-4;而20H/80℃=4-5。实施例2
将100克SiO2碎片状粉末(按WO93/08237制备)悬浮在2升去离子水中,并将悬浮液加热到75℃。以2毫升/分钟的速度添加由在370毫升水中的12克SnCl4·5H2O和40毫升37%HCl组成的且PH值为1.8的溶液。在滴加期间,用32%NaOH溶液使PH值保持恒定。在SnCl4溶液滴加完毕后,搅拌10分钟,并随后以2毫升/分钟的速度添加620毫升TiCl4溶液(410克TiCl4/1升水)。在滴加操作期间,通过加入32%NaOH溶液使PH值保持恒定。30分钟后,用NaOH将PH值调整到7.0,并以2毫升/分钟的速度计量水玻璃溶液(用190克水稀释190克水玻璃),通过同时加入10%HCl使PH值保持恒定。滴加完毕后,在75℃下连续搅拌15分钟。过滤颜料,冲洗以除去盐,在60-180℃下干燥,并最后在800℃下煅烧60分钟。随后过筛,之后再将产物悬浮在1250毫升的去离子水中。当使PH值为7.5后,以2毫升/分钟的速度加入在900毫升水中有100克Co(NO3)2和164克AlCl3·6H2O的溶液,用NaOH使PH值保持恒定。随后搅拌混合物30分钟、过滤、冲洗,并冲洗固体产物以除去盐,在60-180℃下干燥固体产物和在1000℃下煅烧固体产物。
获得带有蓝色主色的金色干涉颜料。
Claims (16)
1.带有蓝色主色的多层干涉颜料,该颜料由碎片状载体材料和涂层组成,而涂层由以下结构组成;
(i)第一层,为高折射率的无色、透明金属氧化物层,
(ii)第二层,为低折射率的无色、透明金属氧化物层,
(iii)第三层,为铝酸钴、含钴玻璃或氧化钴的外层。
2.带有蓝色主色的多层干涉颜料,该颜料由碎片状载体材料和涂层组成,而涂层由以下结构组成;
(i)第一层,为铝酸钴、含钴玻璃或氧化钴层,
(ii)第二层,为低折射率的无色、透明金属氧化物层,
(iii)第三层,为高折射率的无色、透明金属氧化物外层。
3.权利要求1或2的干涉颜料,其特征在于:碎片状载体材料包括天然的或合成的云母、其它层状硅酸盐、玻璃碎片、氧化铝碎片状粉末或二氧化硅碎片状粉末。
4.权利要求1-3任何之一的干涉颜料,其特征在于:高折射率的无色、透明金属氧化物是氧化钛、氧化锆或氧化锡。
5.权利要求1-4任何之一的干涉颜料,其特征在于:低折射率的无色、透明金属氧化物是二氧化硅或氧化铝。
6.权利要求1的颜料的制备方法,其特征在于:
-将碎片状载体材料悬浮在水中,并将悬浮液加热到50-100℃,在适合于水解的PH下加入水溶性金属化合物,以便使高折射率的金属氧化物的水合物沉淀在悬浮的颗粒上面,确定各金属氧化物水合物沉淀所需的PH值,并通过同时加入酸或碱使PH保持恒定,
-随后用碱将PH值调整到4-10,并加入水溶性金属化合物,以便使低折射率的金属氧化物水合物沉淀在悬浮的颗粒上面,通过同时加入酸或碱使PH保持恒定,
-随后冲洗所获得的产物,在60-180℃下干燥和在500-1100℃下煅烧,
-随后将产物悬浮在水中,并在3-10的PH值下通过加入相应的水溶性金属化合物并使之水解从而用氧化钴和氧化铝的水合物涂敷产物,通过同时加入碱使PH值保持恒定,
-随后冲洗产物,在60-180℃下干燥和在500-1100℃下煅烧。
7.权利要求2的颜料的制备方法,其特征在于:
-将碎片状载体材料悬浮在水中,并将悬浮液加热到50-100℃,在3-10的PH值下通过加入相应的水溶性金属化合物并使之水解从而用氧化钴和氧化铝的水合物涂敷载体材料,通过同时加入碱使PH值保持恒定,
-随后用碱将PH值调整到4-10,并加入水溶性金属化合物,以便使低折射率的金属氧化物水合物沉淀在悬浮的颗粒上面,通过同时加入酸或碱使PH保持恒定,
-随后在适合水解的PH值下加入水溶性金属化合物,以便使高折射率的金属氧化物的水合物沉淀在悬浮的颗粒上面,确定各金属氧化物水合物沉淀所需的PH值,并通过同时加入酸或碱使PH值保持恒定,
-随后冲洗产物,在60-180℃下干燥和在500-1100℃下煅烧。
8.权利要求6或7的方法,其特征在于:碎片状载体材料包括天然的或合成的云母、其它层状硅酸盐、玻璃碎片、氧化铝碎片状粉末或二氧化硅碎片状粉末。
9.权利要求6-8任何之一的方法,其特征在于:高折射率的无色、透明金属氧化物是二氧化钛、二氧化锆或氧化锡。
10.权利要求6-9任何之一的方法,其特征在于:低折射率的无色、透明金属氧化物是二氧化硅或氧化铝。
11.权利要求6-9任何之一的方法,其特征在于:在将待涂敷的材料进行中间干燥后,接着在流化床反应器中用VCD涂敷金属氧化物。
12.权利要求1或2的颜料的应用,其用于油漆、印刷油墨、塑料、化妆品和陶瓷釉及玻璃釉。
13.权利要求12的应用,其特征在于:颜料与常规商业颜料一起作为混合物而应用。
14.权利要求1或2的颜料的应用,其用于塑料的激光标志。
15.用权利要求1或2的颜料着色的油漆,印刷油墨、塑料、化妆品、陶瓷和玻璃。
16.包括权利要求1或2的颜料的可激光标志的塑料。
Applications Claiming Priority (2)
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DE1998103550 DE19803550A1 (de) | 1998-01-30 | 1998-01-30 | Interferenzpigmente mit blauer Körperfarbe |
DE19803550.0 | 1998-01-30 |
Publications (2)
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CN1229110A true CN1229110A (zh) | 1999-09-22 |
CN1160423C CN1160423C (zh) | 2004-08-04 |
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CNB991014006A Expired - Fee Related CN1160423C (zh) | 1998-01-30 | 1999-01-28 | 带有蓝色主色的干涉颜料 |
Country Status (7)
Country | Link |
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US (1) | US6238471B1 (zh) |
EP (1) | EP0933403B1 (zh) |
JP (1) | JPH11279433A (zh) |
KR (1) | KR19990068195A (zh) |
CN (1) | CN1160423C (zh) |
DE (2) | DE19803550A1 (zh) |
TW (1) | TW438867B (zh) |
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- 1999-01-16 EP EP19990100755 patent/EP0933403B1/de not_active Expired - Lifetime
- 1999-01-19 JP JP1035599A patent/JPH11279433A/ja active Pending
- 1999-01-26 TW TW88101133A patent/TW438867B/zh not_active IP Right Cessation
- 1999-01-28 CN CNB991014006A patent/CN1160423C/zh not_active Expired - Fee Related
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- 1999-02-01 US US09/241,283 patent/US6238471B1/en not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
DE59907579D1 (de) | 2003-12-11 |
TW438867B (en) | 2001-06-07 |
MX9901112A (es) | 2000-03-31 |
KR19990068195A (ko) | 1999-08-25 |
EP0933403A3 (de) | 2000-01-05 |
EP0933403A2 (de) | 1999-08-04 |
US6238471B1 (en) | 2001-05-29 |
CN1160423C (zh) | 2004-08-04 |
DE19803550A1 (de) | 1999-08-05 |
EP0933403B1 (de) | 2003-11-05 |
JPH11279433A (ja) | 1999-10-12 |
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