JP2016165675A - コア/シェル構造の触媒粒子が担持された触媒の製造方法 - Google Patents
コア/シェル構造の触媒粒子が担持された触媒の製造方法 Download PDFInfo
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- JP2016165675A JP2016165675A JP2015046360A JP2015046360A JP2016165675A JP 2016165675 A JP2016165675 A JP 2016165675A JP 2015046360 A JP2015046360 A JP 2015046360A JP 2015046360 A JP2015046360 A JP 2015046360A JP 2016165675 A JP2016165675 A JP 2016165675A
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- Prior art keywords
- platinum
- catalyst
- core
- copper
- core particles
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- 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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- 239000003054 catalyst Substances 0.000 title claims abstract description 82
- 239000002245 particle Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title abstract description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 147
- 239000007771 core particle Substances 0.000 claims abstract description 78
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 74
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010949 copper Substances 0.000 claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 32
- 150000003058 platinum compounds Chemical class 0.000 claims abstract description 24
- 238000006467 substitution reaction Methods 0.000 claims abstract description 21
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 31
- 229910052763 palladium Inorganic materials 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000151 deposition Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 39
- 230000000694 effects Effects 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 230000009467 reduction Effects 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000000446 fuel Substances 0.000 description 8
- 229910001252 Pd alloy Inorganic materials 0.000 description 7
- 238000005868 electrolysis reaction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 229910000990 Ni alloy Inorganic materials 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000001976 improved effect Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000005749 Copper compound Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001880 copper compounds Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000005518 polymer electrolyte Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 230000008093 supporting effect Effects 0.000 description 2
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- NGMTUCFCIUGWAG-UHFFFAOYSA-L [Cu+2].[O-]Cl=O.[O-]Cl=O Chemical compound [Cu+2].[O-]Cl=O.[O-]Cl=O NGMTUCFCIUGWAG-UHFFFAOYSA-L 0.000 description 1
- JHOUJCAXWAKHJT-UHFFFAOYSA-N [N+](=O)([O-])[O-].[N+](=O)([O-])[Pt+][N+](=O)[O-] Chemical compound [N+](=O)([O-])[O-].[N+](=O)([O-])[Pt+][N+](=O)[O-] JHOUJCAXWAKHJT-UHFFFAOYSA-N 0.000 description 1
- UIPMCPPCWSWWBJ-UHFFFAOYSA-K [Pt+3].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-] Chemical compound [Pt+3].C(CC(O)(C(=O)[O-])CC(=O)[O-])(=O)[O-] UIPMCPPCWSWWBJ-UHFFFAOYSA-K 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- FOSZYDNAURUMOT-UHFFFAOYSA-J azane;platinum(4+);tetrachloride Chemical compound N.N.N.N.[Cl-].[Cl-].[Cl-].[Cl-].[Pt+4] FOSZYDNAURUMOT-UHFFFAOYSA-J 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- YRNNKGFMTBWUGL-UHFFFAOYSA-L copper(ii) perchlorate Chemical compound [Cu+2].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O YRNNKGFMTBWUGL-UHFFFAOYSA-L 0.000 description 1
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- -1 platinum ion Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004758 underpotential deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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- 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
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Abstract
【解決手段】白金からなるシェル層と、前記シェル層に覆われた白金以外の金属よりなるコア粒子とからなる、コア/シェル構造を有する触媒粒子が担体に担持された触媒の製造方法であって、前記コア粒子を担持した前記担体を、銅イオンを含む電解液中で電解し、コア粒子表面に銅を析出させる電解処理工程と、銅を析出させた前記コア粒子に、白金化合物溶液を接触させることにより、コア粒子表面の銅を白金で置換し、白金からなるシェル層を形成する置換反応工程を含み、前記置換反応工程の白金化合物溶液は、クエン酸を含む触媒の製造方法。この電解処理工程の電解液の溶存酸素量は1ppm以下とすることが特に好ましい。
【選択図】図1
Description
第1実施形態:ここでは、パラジウムをコア粒子としたコア/シェル構造を有する触媒粒子が担持された触媒を製造し、その活性を評価した。まず、触媒の担体となるカーボン粉末(商品名:ケッチェンブラックEC、比表面積:800g/m3)35gを塩化パラジウム溶液(Pd量15g(0.028mol))に浸透させ、炭酸ナトリウムで中性にした。これを蟻酸ナトリウムにより還元処理してコア粒子となるパラジウム粒子を担持したカーボン粉末を製造した。
電解条件
・電位:0.39V(vs. RHE)で電位固定。
・電位固定時間:3時間
Claims (5)
- 白金からなるシェル層と、前記シェル層に覆われた白金以外の金属よりなるコア粒子とからなる、コア/シェル構造を有する触媒粒子が担体に担持された触媒の製造方法であって、
前記コア粒子を担持した前記担体を、銅イオンを含む電解液中で電解し、コア粒子表面に銅を析出させる電解処理工程と、
銅を析出させた前記コア粒子に、白金化合物溶液を接触させることにより、コア粒子表面の銅を白金で置換し、白金からなるシェル層を形成する置換反応工程を含み、
前記置換反応工程の白金化合物溶液は、クエン酸を含むことを特徴とする触媒の製造方法。 - 白金化合物溶液中のクエン酸の含有量は、白金化合物のモル数を基準として40倍以下である請求項1記載の触媒の製造方法。
- 電解処理工程の電解液の溶存酸素量を1ppm以下とする請求項1又は請求項2に記載の触媒の製造方法。
- 電解処理工程は、コア粒子を担持した担体を作用極上に堆積させて電解処理を行うものである請求項1〜請求項3のいずれかに記載の触媒の製造方法。
- コア粒子を構成する金属は、パラジウム、イリジウム、ロジウム、金又はこれらの金属の合金である請求項1〜請求項4のいずれかに記載の触媒の製造方法。
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PCT/JP2016/056353 WO2016143618A1 (ja) | 2015-03-09 | 2016-03-02 | コア/シェル構造の触媒粒子が担持された触媒の製造方法 |
CN201680014687.1A CN107405604B (zh) | 2015-03-09 | 2016-03-02 | 担载核/壳结构的催化剂颗粒的催化剂的制造方法 |
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US15/548,193 US10497942B2 (en) | 2015-03-09 | 2016-03-02 | Method for manufacturing catalyst having supported catalyst particles of core/shell structure |
TW105106507A TWI597099B (zh) | 2015-03-09 | 2016-03-03 | 載持核心/殼構造之觸媒粒子之觸媒之製造方法 |
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