JP2023544152A - 単体銀及び単体ルテニウムを有する粒子状担体材料を製造するための方法 - Google Patents
単体銀及び単体ルテニウムを有する粒子状担体材料を製造するための方法 Download PDFInfo
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- JP2023544152A JP2023544152A JP2023519895A JP2023519895A JP2023544152A JP 2023544152 A JP2023544152 A JP 2023544152A JP 2023519895 A JP2023519895 A JP 2023519895A JP 2023519895 A JP2023519895 A JP 2023519895A JP 2023544152 A JP2023544152 A JP 2023544152A
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- Prior art keywords
- ruthenium
- silver
- aqueous solution
- elemental
- water
- 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.)
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 81
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 78
- 239000004332 silver Substances 0.000 title claims abstract description 78
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 94
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 76
- 239000012876 carrier material Substances 0.000 claims description 47
- 239000011236 particulate material Substances 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 27
- 239000000047 product Substances 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 13
- 239000004033 plastic Substances 0.000 claims description 12
- 229920003023 plastic Polymers 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 150000003304 ruthenium compounds Chemical class 0.000 claims description 8
- 239000004793 Polystyrene Substances 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical class [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- -1 polysiloxane Polymers 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000002537 cosmetic Substances 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- BPEVHDGLPIIAGH-UHFFFAOYSA-N ruthenium(3+) Chemical class [Ru+3] BPEVHDGLPIIAGH-UHFFFAOYSA-N 0.000 claims description 3
- 229940024463 silicone emollient and protective product Drugs 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 229920003002 synthetic resin Polymers 0.000 claims description 3
- 239000000057 synthetic resin Substances 0.000 claims description 3
- 239000004753 textile Substances 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 229920002522 Wood fibre Polymers 0.000 claims description 2
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 2
- 229920002301 cellulose acetate Polymers 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000000017 hydrogel Substances 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 150000004767 nitrides Chemical class 0.000 claims description 2
- 239000000123 paper Substances 0.000 claims description 2
- 239000011087 paperboard Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000002985 plastic film Chemical group 0.000 claims description 2
- 229920006255 plastic film Chemical group 0.000 claims description 2
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 239000004626 polylactic acid Substances 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- YAYGSLOSTXKUBW-UHFFFAOYSA-N ruthenium(2+) Chemical class [Ru+2] YAYGSLOSTXKUBW-UHFFFAOYSA-N 0.000 claims description 2
- RADGOBKLTHEUQO-UHFFFAOYSA-N ruthenium(4+) Chemical class [Ru+4] RADGOBKLTHEUQO-UHFFFAOYSA-N 0.000 claims description 2
- 150000004760 silicates Chemical class 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 239000002025 wood fiber Substances 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims 1
- 239000004721 Polyphenylene oxide Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000010586 diagram Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 239000002245 particle Substances 0.000 description 21
- 239000000543 intermediate Substances 0.000 description 19
- 238000003756 stirring Methods 0.000 description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910001961 silver nitrate Inorganic materials 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 150000004676 glycans Chemical class 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- YLPJWCDYYXQCIP-UHFFFAOYSA-N nitroso nitrate;ruthenium Chemical compound [Ru].[O-][N+](=O)ON=O YLPJWCDYYXQCIP-UHFFFAOYSA-N 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 229920001282 polysaccharide Polymers 0.000 description 4
- 239000005017 polysaccharide Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 3
- 239000011859 microparticle Substances 0.000 description 3
- 229910052762 osmium Inorganic materials 0.000 description 3
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- NSNVGCNCRLAWOJ-UHFFFAOYSA-N [N+](=O)([O-])[O-].N(=O)[Ru+2].[N+](=O)([O-])[O-] Chemical compound [N+](=O)([O-])[O-].N(=O)[Ru+2].[N+](=O)([O-])[O-] NSNVGCNCRLAWOJ-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 description 1
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000011496 digital image analysis Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011022 operating instruction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- OJLCQGGSMYKWEK-UHFFFAOYSA-K ruthenium(3+);triacetate Chemical compound [Ru+3].CC([O-])=O.CC([O-])=O.CC([O-])=O OJLCQGGSMYKWEK-UHFFFAOYSA-K 0.000 description 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 1
- 239000012266 salt solution Substances 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
- UVGLBOPDEUYYCS-UHFFFAOYSA-N silicon zirconium Chemical class [Si].[Zr] UVGLBOPDEUYYCS-UHFFFAOYSA-N 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
- C23C18/1641—Organic substrates, e.g. resin, plastic
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1658—Process features with two steps starting with metal deposition followed by addition of reducing agent
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Abstract
Description
a)水不溶性粒子状担体材料と、(i)溶解した銀前駆体を含む水溶液A(簡潔にするために、以下の説明及び特許請求の範囲では単に「水溶液A」とも称する)及び溶解したルテニウム前駆体を含む水溶液B(簡潔にするために、以下の説明及び特許請求の範囲では単に「水溶液B」とも称する)、又は(ii)溶解した銀前駆体及び溶解したルテニウム前駆体の両方を含む水溶液(簡潔にするために、以下の説明及び特許請求の範囲では単に「水溶液C」とも称する)とを提供する工程、
b)当該水不溶性粒子状担体材料を、(i)水溶液A及び水溶液Bと、又は好ましくは(ii)水溶液Cと接触させて、中間体、好ましくは自由流動性含浸粒子状材料の形態の中間体を形成する工程、
c)当該中間体を、>7~14、好ましくは>11~14の範囲のpHを有してヒドラジンを含む水溶液と接触させて、単体銀及び単体ルテニウムを含む塊を形成する工程、
d)任意で、工程c)の完了後に得られた塊を洗浄する工程、並びに
e)工程c)又はd)の完了後に得られた塊から水及び他のあり得る揮発性成分を除去する工程、を含む。
工程b)で使用される粒子状担体材料のタイプ及び量、
工程b)で使用される水溶液Cの体積、
水溶液C中の銀:ルテニウムの重量比、
水溶液C中の銀+ルテニウムの重量分率、並びに
工程e)の完了後に得られたプロセス生成物の残留水分が挙げられる。
132.45gの硝酸銀水溶液(銀含有量36.24wt%、445mmolのAg)及び2.60gのニトロシル硝酸ルテニウム水溶液(ルテニウム含有量19.0wt%、4.9mmolのRu)を364.5gの脱塩水に加え、このようにして得られた前駆体水溶液を211.2gのセルロース粉末(J.Rettenmaier and Soehne GmbH&Co KG製Vitacel(登録商標)L-600)と均一に混合して、橙色の自由流動性含浸粒子状材料を得た。100mLのこの材料に対して、0.5rpmのPS Prozesstechnik GmbH(Neuhausstrasse 36、CH-4057 Basel)製のRevolution Powder Analyzerによって、35mmの内部深さ及び100mmの内径を有する円筒を使用し、20℃で回転法粉末解析を行ない、フレームレートを10画像/秒として、300回の雪崩を記録した。このようにして決定された雪崩角は75度であり、2つの雪崩の間の時間間隔は3.6秒であった。自由流動性含浸粒子状材料に、pHが14の705mLのヒドラジン水溶液[3.68g(115mmol)のヒドラジンと71.82gの32wt%水酸化ナトリウム溶液(575mmolのNaOH)、残りは水]を、室温で、撹拌しながら30mL/分の計量添加速度で添加した。時間の経過と共に、撹拌がますます容易になる黒色の均質なパルプが形成された。計量添加の完了後、窒素の放出がもはや観察され得なくなるまで、撹拌を30分間続けた。続いて、材料を濾し取り、合計1000mLの水で洗浄し、105℃/300mbarの乾燥キャビネット内で15wt%の残留含水量まで乾燥させた。ICP-OESによって、最終生成物(0wt%の残留水分を基準として)の銀含有量が18.3wt%、及びルテニウム含有量が0.19wt%と測定された。
97.96gの硝酸銀水溶液(銀含有量36.24wt%、329mmolのAg)及び3.68gのニトロシル硝酸ルテニウム水溶液(ルテニウム含有量19.0wt%、6.9mmolのRu)を554.9gの脱塩水に加え、このようにして得られた前駆体水溶液を299.2gのセルロース粉末(J.Rettenmaier and Soehne GmbH&Co KG製Vitacel(登録商標)L-600)と均一に混合して、橙色の自由流動性含浸粒子状材料を得た。100mLのこの材料に対して、0.5rpmのPS Prozesstechnik GmbH(Neuhausstrasse 36、CH-4057 Basel)製のRevolution Powder Analyzerによって、35mmの内部深さ及び100mmの内径を有する円筒を使用し、20℃で回転法粉末解析を行ない、フレームレートを10画像/秒として、300回の雪崩を記録した。このようにして決定された雪崩角は68度であり、2つの雪崩の間の時間間隔は3.0秒であった。自由流動性含浸粒子状材料に、pHが13.8の999.9mLのヒドラジン水溶液[2.80g(88mmol)のヒドラジンと54.66gの32wt%水酸化ナトリウム溶液(437mmolのNaOH)、残りは水]を、室温で、撹拌しながら30mL/分の計量添加速度で添加した。時間の経過と共に、撹拌がますます容易になる黒色の均質なパルプが形成された。計量添加の完了後、窒素の放出がもはや観察され得なくなるまで、撹拌を30分間続けた。続いて、材料を濾し取り、合計1000mLの水で洗浄し、105℃/300mbarの乾燥キャビネット内で15wt%の残留含水量まで乾燥させた。ICP-OESによって、最終生成物(0wt%の残留水分を基準として)の銀含有量が10.88wt%、及びルテニウム含有量が0.21wt%と測定された。
75.6g(445mmol)の硝酸銀固体及び13.94gのニトロシル硝酸ルテニウム溶液(ルテニウム含有量19.0wt%、26.2mmolのRu)を416.8gの脱塩水に溶解し、このようにして得られた前駆体水溶液を211.2gのセルロース粉末(J.Rettenmaier and Soehne GmbH&Co KG製Vitacel(登録商標)L-600)と均一に混合して、橙色の自由流動性含浸粒子状材料を得た。100mLのこの材料に対して、0.5rpmのPS Prozesstechnik GmbH(Neuhausstrasse 36、CH-4057 Basel)製のRevolution Powder Analyzerによって、35mmの内部深さ及び100mmの内径を有する円筒を使用し、20℃で回転法粉末解析を行ない、フレームレートを10画像/秒として、300回の雪崩を記録した。このようにして決定された雪崩角は73度であり、2つの雪崩の間の時間間隔は3.5秒であった。自由流動性含浸粒子状材料に、pHが13.9の705mLのヒドラジン水溶液[4.19g(131mmol)のヒドラジンと81.81gの32wt%水酸化ナトリウム溶液(654.51mmolのNaOH)、残りは水]を、室温で、撹拌しながら30mL/分の計量添加速度で添加した。時間の経過と共に、撹拌がますます容易になる黒色の均質なパルプが形成された。計量添加の完了後、窒素の放出がもはや観察され得なくなるまで、撹拌を30分間続けた。続いて、材料を濾し取り、合計1000mLの水で洗浄し、105℃/300mbarの乾燥キャビネット内で15wt%の残留含水量まで乾燥させた。ICP-OESによって、最終生成物(0wt%の残留水分を基準として)の銀含有量が18.9wt%、及びルテニウム含有量が1.0wt%と測定された。
Claims (18)
- 単体銀及び単体ルテニウムを有する粒子状担体材料を製造するための方法であって、以下の連続工程、すなわち、
a)水不溶性粒子状担体材料と、(i)溶解した銀前駆体を含む水溶液A及び溶解したルテニウム前駆体を含む水溶液B、又は(ii)溶解した銀前駆体及び溶解したルテニウム前駆体の両方を含む水溶液Cとを提供する工程、
b)前記水不溶性粒子状担体材料を、(i)水溶液A及び水溶液Bと、又は好ましくは(ii)水溶液Cと接触させて、中間体、好ましくは自由流動性含浸粒子状材料の形態の中間体を形成する工程、
c)前記中間体を、>7~14の範囲のpHを有してヒドラジンを含む水溶液と接触させて、単体銀及び単体ルテニウムを含む塊を形成する工程、
d)任意で、工程c)の完了後に得られた前記塊を洗浄する工程、並びに
e)工程c)又はd)の完了後に得られた前記塊から水及び他のあり得る揮発性成分を除去する工程、を含む、方法。 - 前記中間体が自由流動性含浸粒子状材料である、請求項1に記載の方法。
- 前記自由流動性含浸粒子状材料が、(i)水溶液A及び水溶液B、又は好ましくは(ii)水溶液Cで含浸された粒又はフレークの形態を有する、請求項2に記載の方法。
- 前記自由流動性含浸粒子状材料が、20℃で、PS Prozesstechnik GmbH製のRevolution Powder Analyzerを0.5rpmで使用し、35mmの内部深さ及び100mmの内径を有する円筒を使用して、100mLの前記自由流動性含浸粒子状材料での回転法粉末分析によって決定される、40~80度の範囲の雪崩角を有する、請求項2又は3に記載の方法。
- 前記自由流動性含浸粒子状材料が、2つの雪崩の間の時間間隔が2~5秒の範囲であることを更に特徴とする、請求項4に記載の方法。
- 前記水不溶性粒子状担体材料が、水で膨潤可能であるか、又はヒドロゲルを形成することができる、請求項1~5のいずれか一項に記載の方法。
- 前記水不溶性粒子状担体材料の材料が、ガラス、窒化物、高融点酸化物、ケイ酸塩、プラスチック、変性又は未変性の天然由来ポリマー、炭素基材及び木材からなる群から選択される、請求項1~5のいずれか一項に記載の方法。
- 前記水不溶性粒子状担体材料がセルロース粉末である、請求項1~5のいずれか一項に記載の方法。
- 前記銀前駆体及びルテニウム前駆体が、1種以上の銀(I)化合物、並びに、ルテニウム(II)化合物、ルテニウム(III)化合物及びルテニウム(IV)化合物からなる群から選択される1種以上のルテニウム化合物である、請求項1~8のいずれか一項に記載の方法。
- 工程b)で使用される水溶液AとBとの組み合わせにおける、又は水溶液Cにおける銀:ルテニウムの重量比が、銀1~2000重量部:ルテニウム1重量部の範囲である、請求項1~9のいずれか一項に記載の方法。
- 前記水溶液C中の銀+ルテニウムの重量分率が、0.5~20wt%の範囲である、請求項1~10のいずれか一項に記載の方法。
- 前記ヒドラジン水溶液のヒドラジン濃度が、0.1~5wt%の範囲である、請求項1~11のいずれか一項に記載の方法。
- 前記中間体に含まれる前記銀及びルテニウム前駆体を完全に還元するために化学量論的に必要な量以上で、前記ヒドラジン水溶液を前記中間体と接触させる、請求項1~12のいずれか一項に記載の方法。
- 請求項1~13のいずれか一項に記載の方法に従って製造された、単体銀及び単体ルテニウムを有する粒子状担体材料。
- 銀:ルテニウムの重量比が1~2000重量部の銀:1重量部のルテニウムの範囲で、銀+ルテニウムの重量分率が0.1~50wt%の範囲である、請求項14に記載の単体銀及び単体ルテニウムを有する粒子状担体材料。
- 請求項14若しくは15に記載の、又は請求項1~13のいずれか一項に記載の方法によって製造される単体銀及び単体ルテニウムを有する粒子状担体材料の使用であって、金属表面、コーティング剤、プラスター、成形コンパウンド、プラスチックフィルム、プラスチック部品又はプラスチック繊維の形態のプラスチック、合成樹脂製品、イオン交換樹脂、シリコーン製品、セルロース系製品、発泡体、織物、化粧品及び衛生用品の抗菌仕上げのための添加剤としての使用。
- 前記セルロース系製品が、紙製品、板紙、木材繊維製品及び酢酸セルロースからなる群から選択される、請求項16に記載の使用。
- 前記プラスチックが、ABSプラスチック、PVC、ポリ乳酸、PU、ポリ(メタ)アクリレート、PC、ポリシロキサン、フェノールホルムアルデヒド樹脂、メラミンホルムアルデヒド樹脂、ポリエステル、ポリアミド、ポリエーテル、ポリオレフィン、ポリスチレン、それらのハイブリッドポリマー、及びそれらの混合物からなる群から選択される、請求項16に記載の使用。
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