JP2017049231A - 水素変色ナノ粒子、この製造方法及びこれを含む水素センサ - Google Patents
水素変色ナノ粒子、この製造方法及びこれを含む水素センサ Download PDFInfo
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- JP2017049231A JP2017049231A JP2016142559A JP2016142559A JP2017049231A JP 2017049231 A JP2017049231 A JP 2017049231A JP 2016142559 A JP2016142559 A JP 2016142559A JP 2016142559 A JP2016142559 A JP 2016142559A JP 2017049231 A JP2017049231 A JP 2017049231A
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- hydrogen
- core
- hydrated
- nanoparticles
- transition metal
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Links
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 71
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title claims abstract 9
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 76
- 229910052751 metal Inorganic materials 0.000 claims abstract description 53
- 239000002184 metal Substances 0.000 claims abstract description 53
- 239000003054 catalyst Substances 0.000 claims abstract description 48
- 239000011258 core-shell material Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 4
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 20
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- 238000002845 discoloration Methods 0.000 claims description 11
- 239000012685 metal catalyst precursor Substances 0.000 claims description 11
- 229910052763 palladium Inorganic materials 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical group Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 7
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 7
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 5
- 239000011118 polyvinyl acetate Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 4
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910003445 palladium oxide Inorganic materials 0.000 claims description 3
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 3
- KGRJUMGAEQQVFK-UHFFFAOYSA-L platinum(2+);dibromide Chemical compound Br[Pt]Br KGRJUMGAEQQVFK-UHFFFAOYSA-L 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- WYRXRHOISWEUST-UHFFFAOYSA-K ruthenium(3+);tribromide Chemical compound [Br-].[Br-].[Br-].[Ru+3] WYRXRHOISWEUST-UHFFFAOYSA-K 0.000 claims description 3
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims description 3
- MJRFDVWKTFJAPF-UHFFFAOYSA-K trichloroiridium;hydrate Chemical compound O.Cl[Ir](Cl)Cl MJRFDVWKTFJAPF-UHFFFAOYSA-K 0.000 claims description 3
- 229920008347 Cellulose acetate propionate Polymers 0.000 claims description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 2
- XWURZHGKODQZMK-UHFFFAOYSA-N O.[Ru]=O Chemical compound O.[Ru]=O XWURZHGKODQZMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 2
- 229910002367 SrTiO Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- ZGVVPOQZNPUROP-UHFFFAOYSA-N acetyl acetate;iridium Chemical compound [Ir].CC(=O)OC(C)=O ZGVVPOQZNPUROP-UHFFFAOYSA-N 0.000 claims description 2
- 229920002301 cellulose acetate Polymers 0.000 claims description 2
- 229920006217 cellulose acetate butyrate Polymers 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000002923 metal particle Substances 0.000 claims description 2
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 claims description 2
- 229910003446 platinum oxide Inorganic materials 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
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- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
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- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 238000001308 synthesis method Methods 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- AYRBBDWFLGUINX-UHFFFAOYSA-N acetyl acetate;ruthenium Chemical compound [Ru].CC(=O)OC(C)=O AYRBBDWFLGUINX-UHFFFAOYSA-N 0.000 claims 1
- 150000002736 metal compounds Chemical class 0.000 claims 1
- JOKPITBUODAHEN-UHFFFAOYSA-N sulfanylideneplatinum Chemical compound [Pt]=S JOKPITBUODAHEN-UHFFFAOYSA-N 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 13
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 2
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 56
- 150000002431 hydrogen Chemical class 0.000 description 34
- 230000008859 change Effects 0.000 description 15
- 238000001514 detection method Methods 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000004040 coloring Methods 0.000 description 6
- 239000000446 fuel Substances 0.000 description 6
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- 230000002829 reductive effect Effects 0.000 description 6
- 230000004044 response Effects 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
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- 150000002500 ions Chemical class 0.000 description 3
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- 229910052723 transition metal Inorganic materials 0.000 description 3
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- AZFHXIBNMPIGOD-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;iridium Chemical compound [Ir].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O AZFHXIBNMPIGOD-LNTINUHCSA-N 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 2
- NVVMHYYKCATJAN-UHFFFAOYSA-K 3-oxobutanoate;ruthenium(3+) Chemical compound [Ru+3].CC(=O)CC([O-])=O.CC(=O)CC([O-])=O.CC(=O)CC([O-])=O NVVMHYYKCATJAN-UHFFFAOYSA-K 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- RKNFJIIYAUSTJA-UHFFFAOYSA-N bis(sulfanylidene)platinum Chemical compound S=[Pt]=S RKNFJIIYAUSTJA-UHFFFAOYSA-N 0.000 description 2
- 238000000224 chemical solution deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- RFLFDJSIZCCYIP-UHFFFAOYSA-L palladium(2+);sulfate Chemical compound [Pd+2].[O-]S([O-])(=O)=O RFLFDJSIZCCYIP-UHFFFAOYSA-L 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
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- 238000004544 sputter deposition Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 101150003085 Pdcl gene Proteins 0.000 description 1
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical compound [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 description 1
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- 125000004429 atom Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000000469 dry deposition Methods 0.000 description 1
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- 229910001922 gold oxide Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- HLYTZTFNIRBLNA-LNTINUHCSA-K iridium(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ir+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O HLYTZTFNIRBLNA-LNTINUHCSA-K 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/005—H2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
Description
脱色:2W5+−OH+1/2O2→2W6+=O+H2O(catalyzed by Ptnp)
変色:W6+=O+1/2H2→W5+−OH(catalyzed by Ptnp)・・・(1)
水和(hydrate)または非水和の(non−hydrated)遷移金属酸化物からなるコア;及び前記コアの表面に部分的にコーティングされた金属触媒からなるシェル;を含むコア−シェル構造の水素変色ナノ粒子を提供する。
水和または非水和の遷移金属酸化物を製造する段階;
金属触媒前駆体及び高分子化合物を有機溶媒に溶解させて金属触媒溶液を製造する段階;
前記金属触媒溶液に前記水和または非水和の遷移金属酸化物を投入して混合溶液を製造する段階;
前記混合溶液にUVを照射してコア−シェル構造の水素変色ナノ粒子を製造する段階;及び
前記混合溶液を濾過してコア−シェル構造の水素変色ナノ粒子を収得する段階;を含むコア−シェル構造の水素変色ナノ粒子の製造方法を提供する。
水和または非水和の遷移金属酸化物を製造する段階;
金属触媒前駆体及び高分子化合物を有機溶媒に溶解させて金属触媒溶液を製造する段階;
前記金属触媒溶液に前記水和または非水和の遷移金属酸化物を投入して混合溶液を製造する段階;
前記混合溶液にUVを照射してコア−シェル構造の水素変色ナノ粒子を製造する段階;及び
前記混合溶液を濾過してコア−シェル構造の水素変色ナノ粒子を収得する段階;を含むコア−シェル構造の水素変色ナノ粒子の製造方法を提供する。
パラタングステン酸アンモニウム水溶液を準備する段階(a段階);
前記パラタングステン酸アンモニウム水溶液に塩酸を投入して撹拌し、タングステン酸水溶液を製造する段階(b及びc段階);
前記タングステン酸水溶液に過酸化水素を投入してパーオキソ−ポリタングステン酸水溶液を製造する段階(d段階);
前記パーオキソ−ポリタングステン酸水溶液をオートクレーブに投入して一次熱処理を行う段階(e段階);
反応終結後に前記オートクレーブを空冷して水和されたタングステン酸化物(WO3−0.33H2O)を析出させる段階(f段階);及び
前記タングステン酸化物を収得する段階(g段階)を含むことができる。
実験方法及び装備
a.排出口のある開放チャンバを使用し、窒素、酸素及び水蒸気混合物の雰囲気下で1%水素(in 99% air balanceガス(N2、H2O、O2))の変色反応を調査した。
b.全てのガス彩色実験は室温で行っており、サンプル上に2L/minの流量を維持した。
反応器にパラタングステン酸アンモニウムと水を混合して1wt%のパラタングステンアンモニウム水溶液を製造した後、前記水溶液を撹拌しながら塩酸(HCl)(1.5ml)を添加し、30分間追加撹拌してタングステン水溶液を製造した。
前記製造例1で収得された、水和されたタングステン酸化物をオートクレーブに再投入した後、500℃で2時間の間二次熱処理を行って非水和のタングステン酸化物を製造した。
反応器に金属触媒であるパラジウムクロリド、高分子化合物であるポリビニルピロリドン及び有機溶媒であるメタノールを1:1.5:2.5(wt%)比率で投入し、約2時間の間撹拌しながら超音波粉砕した。
前記製造例2の非水和のタングステン酸化物に代えて製造例1の水和されたタングステン酸化物を使用することを除いては、前記実施例1と同じ方法を用いてコア−シェル構造の水素変色ナノ粒子を製造した。
(実験例1.水素ガス着色試験)
前記実施例1及び2で製造された水素変色ナノ粒子を、濾過紙に収得された状態のままで、窒素、酸素及び水蒸気が混合された空気雰囲気下で1%水素(99%窒素含有)ガスを通過させながら水素ガスに対する変色反応を肉眼で検査した。
前記実施例1及び2で製造された水素変色ナノ粒子を溶媒と交ぜてインクとして製造した後、これを紙または多孔性ポリマー基板に転写して水素センサを製造した。
Claims (20)
- 遷移金属酸化物からなるコア;及び
前記コアの表面に部分的にコーティングされた金属触媒からなるシェル;
を含むことを特徴とするコア−シェル構造の水素変色ナノ粒子。 - 前記遷移金属酸化物は、水分子がドーピングされない非水和の遷移金属酸化物、または水分子がドーピングされた水和された遷移金属酸化物を含むことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記遷移金属酸化物は、SnO2、TiO2、ZnO、VO2、In2O3、NiO、MoO3、SrTiO3、Fe2O3、WO3及びCuOからなる群より選択される単一物または2種以上の金属酸化物を含むことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記遷移金属酸化物は、タングステン酸化物を含むことを特徴とする、請求項1または請求項3に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記遷移金属酸化物の平均粒径は、1から200nmであることを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記金属触媒は、Pd、Pt、Ru、Mg、Ni、Au、及びこれらからなる群より選択される単一物または2種以上の金属粒子を含むことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記金属触媒は、塩化パラジウム、硝酸パラジウムアンモニウム、臭化パラジウム、パラジウムオキシドハイドレート、パラジウムサルフェート、パラジウムナイトレート、パラジウムアセチルアセテート、塩化白金、臭化白金、白金酸化物、硫化白金、ルテニウムオキシドハイドレート、ルテニウムアセチルアセテート、ルテニウムブロミド、塩化イリジウム、イリジウムアセチルアセテート、及びイリジウムクロリドハイドレートからなる群より選択される単一物または2種以上の金属化合物を含むことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記金属触媒は、塩化パラジウムを含むことを特徴とする、請求項1または請求項7に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記金属触媒からなるシェルは、UV照射を用いた溶液合成方法を用いて形成されることを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記金属触媒からなるシェルの厚さは、0.1から50nmであることを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記シェルは、前記コアの表面に点形態で部分的にコーティングされたことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。
- 前記水素変色ナノ粒子は、
水和または非水和の遷移金属酸化物からなるコア80から90重量%;及び金属触媒からなるシェル10から20重量%を含むことを特徴とする、請求項1に記載のコア−シェル構造の水素変色ナノ粒子。 - 水和または非水和の遷移金属酸化物を製造する段階;
金属触媒前駆体及び高分子化合物を有機溶媒に溶解させて金属触媒溶液を製造する段階;
前記金属触媒溶液に前記水和または非水和の遷移金属酸化物を投入して混合溶液を製造する段階;
前記混合溶液にUVを照射してコア−シェル構造の水素変色ナノ粒子を製造する段階;及び
前記混合溶液を濾過してコア−シェル構造の水素変色ナノ粒子を収得する段階;
を含むことを特徴とするコア−シェル構造の水素変色ナノ粒子の製造方法。 - 前記高分子化合物は、ポリウレタン、ポリエーテルウレタン、セルロースアセテート、セルロースアセテートブチレート、セルロースアセテートプロピオネート、ポリメチルメタクリレート、ポリメチルアクリレート、ポリアクリル共重合体、ポリビニルアセテート、ポリビニルアセテート共重合体、ポリビニルアルコール、ポリスチレン、ポリスチレン共重合体、ポリエチレンオキシド、ポリプロピレンオキシド、ポリエチレンオキシド共重合体、ポリカーボネート、ポリビニルクロリド、ポリカプロラクトン、ポリビニルピロリドン、ポリビニルフルオライド、ポリビニリデンフルオライド共重合体及びポリアマイドからなる群より選択される単一物または2種以上の混合物を含むことを特徴とする、請求項13に記載のコア−シェル構造の水素変色ナノ粒子の製造方法。
- 前記有機溶媒は、アルコール系溶媒を含むことを特徴とする、請求項13に記載のコア−シェル構造の水素変色ナノ粒子の製造方法。
- 前記UV照射段階は、室温で、UV波長365nm、出力1000Wの条件下で2分から3分間行うことを特徴とする、請求項13に記載のコア−シェル構造の水素変色ナノ粒子の製造方法。
- 請求項1に記載のコア−シェル構造の水素変色ナノ粒子;及び
選択的にポリマー、エアロゲル、及び溶媒からなる群より選択される少なくとも一つの部材をさらに含むことを特徴とする水素センサ。 - パラタングステン酸アンモニウム水溶液を準備する段階;
前記パラタングステン酸アンモニウム水溶液に塩酸を投入して撹拌し、タングステン酸水溶液を製造する段階;
前記タングステン酸水溶液に過酸化水素を投入してパーオキソ−ポリタングステン酸水溶液を製造する段階;
前記パーオキソ−ポリタングステン酸水溶液をオートクレーブに投入して一次熱処理を行う段階;
反応終結後に前記オートクレーブを空冷して水和されたタングステン酸化物を析出させる段階;
前記タングステン酸化物を収得する段階;及び
選択的に前記得られたタングステン酸化物に二次熱処理を行う段階を含むことを特徴とする、水和または非水和のタングステン酸化物の製造方法。 - 前記一次熱処理段階は、内部圧力が35から50barを維持するオートクレーブ内で160℃温度条件下で行うことを特徴とする、請求項18に記載の水和または非水和のタングステン酸化物の製造方法。
- 前記二次熱処理段階は、オートクレーブにタングステン酸化物を再投入した後、500℃温度条件下で行うことを特徴とする、請求項18に記載の水和または非水和のタングステン酸化物の製造方法。
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