JP6740043B2 - 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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- JP6740043B2 JP6740043B2 JP2016142559A JP2016142559A JP6740043B2 JP 6740043 B2 JP6740043 B2 JP 6740043B2 JP 2016142559 A JP2016142559 A JP 2016142559A JP 2016142559 A JP2016142559 A JP 2016142559A JP 6740043 B2 JP6740043 B2 JP 6740043B2
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- hydrogen
- hydrated
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- transition metal
- metal catalyst
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- 229910052739 hydrogen Inorganic materials 0.000 title claims description 83
- 239000001257 hydrogen Substances 0.000 title claims description 82
- 239000002105 nanoparticle Substances 0.000 title claims description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 35
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title 2
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 65
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 57
- 150000002431 hydrogen Chemical class 0.000 claims description 52
- 239000011258 core-shell material Substances 0.000 claims description 34
- 239000000126 substance Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 20
- 239000012685 metal catalyst precursor Substances 0.000 claims description 17
- 229920000642 polymer Polymers 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 14
- 238000002845 discoloration Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 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
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 5
- 239000011118 polyvinyl acetate Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
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- 229920001451 polypropylene glycol Polymers 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
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 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
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000003054 catalyst Substances 0.000 description 38
- 229910052751 metal Inorganic materials 0.000 description 38
- 239000002184 metal Substances 0.000 description 38
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 30
- 239000002245 particle Substances 0.000 description 26
- 239000000243 solution Substances 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 14
- 230000008859 change Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000011259 mixed solution Substances 0.000 description 13
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 13
- 229910001930 tungsten oxide Inorganic materials 0.000 description 13
- 230000035945 sensitivity Effects 0.000 description 12
- 238000001514 detection method Methods 0.000 description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 229910052763 palladium Inorganic materials 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 238000004040 coloring Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000446 fuel Substances 0.000 description 6
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- 238000010438 heat treatment Methods 0.000 description 6
- 230000004044 response Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 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 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 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
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 2
- XWURZHGKODQZMK-UHFFFAOYSA-N O.[Ru]=O Chemical compound O.[Ru]=O XWURZHGKODQZMK-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- RKNFJIIYAUSTJA-UHFFFAOYSA-N bis(sulfanylidene)platinum Chemical compound S=[Pt]=S RKNFJIIYAUSTJA-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 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 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 2
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910003445 palladium oxide Inorganic materials 0.000 description 2
- INIOZDBICVTGEO-UHFFFAOYSA-L palladium(ii) bromide Chemical compound Br[Pd]Br INIOZDBICVTGEO-UHFFFAOYSA-L 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 2
- 229910003446 platinum oxide Inorganic materials 0.000 description 2
- KGRJUMGAEQQVFK-UHFFFAOYSA-L platinum(2+);dibromide Chemical compound Br[Pt]Br KGRJUMGAEQQVFK-UHFFFAOYSA-L 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WYRXRHOISWEUST-UHFFFAOYSA-K ruthenium(3+);tribromide Chemical compound [Br-].[Br-].[Br-].[Ru+3] WYRXRHOISWEUST-UHFFFAOYSA-K 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 2
- MJRFDVWKTFJAPF-UHFFFAOYSA-K trichloroiridium;hydrate Chemical compound O.Cl[Ir](Cl)Cl MJRFDVWKTFJAPF-UHFFFAOYSA-K 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000469 dry deposition Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
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- 238000004880 explosion Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- RFLFDJSIZCCYIP-UHFFFAOYSA-L palladium(2+);sulfate Chemical compound [Pd+2].[O-]S([O-])(=O)=O RFLFDJSIZCCYIP-UHFFFAOYSA-L 0.000 description 1
- JKDRQYIYVJVOPF-FDGPNNRMSA-L palladium(ii) acetylacetonate Chemical compound [Pd+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O JKDRQYIYVJVOPF-FDGPNNRMSA-L 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
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- 239000002798 polar solvent Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000002441 reversible effect Effects 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
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- 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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- 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
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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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 (4)
- 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混合させて金属触媒前駆体分散液を製造する段階;
前記金属触媒前駆体分散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物を製造する段階;
前記混合物に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
前記混合物を濾過してコア−シェル構造の水素変色ナノ粒子を収得する段階;を含み、
前記遷移金属酸化物がWO3 からなり、
前記金属触媒前駆体がPdCl 2 からなり、
前記金属触媒前駆体分散液中での前記金属触媒前駆体:前記高分子化合物:前記有機溶媒の混合比(wt%)が、1:1から2:2から3であり、
前記混合物中での前記金属触媒前駆体:前記水和または非水和の遷移金属酸化物の混合比(wt%)が、8:10から12である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1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1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1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。
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KR102242201B1 (ko) * | 2019-07-10 | 2021-04-19 | 아주대학교 산학협력단 | 수소 센서 및 이의 제조방법 |
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EP3138630A1 (en) | 2017-03-08 |
US20190339239A1 (en) | 2019-11-07 |
KR101745128B1 (ko) | 2017-06-08 |
EP3138630B1 (en) | 2024-03-13 |
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JP2017049231A (ja) | 2017-03-09 |
US10921302B2 (en) | 2021-02-16 |
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