JP7105941B2 - 一酸化炭素を用いたコアシェル粒子の製造方法 - Google Patents
一酸化炭素を用いたコアシェル粒子の製造方法 Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims description 96
- 239000011258 core-shell material Substances 0.000 title claims description 54
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims description 46
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 64
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 238000010926 purge Methods 0.000 claims description 45
- 239000002243 precursor Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 28
- 229910052697 platinum Inorganic materials 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 229910052763 palladium Inorganic materials 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 8
- 239000012498 ultrapure water Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 229910020427 K2PtCl4 Inorganic materials 0.000 claims 1
- 229910002666 PdCl2 Inorganic materials 0.000 claims 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical group Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 description 52
- 239000002184 metal Substances 0.000 description 52
- 150000003624 transition metals Chemical class 0.000 description 42
- 239000000243 solution Substances 0.000 description 38
- 239000010410 layer Substances 0.000 description 29
- 229910052723 transition metal Inorganic materials 0.000 description 21
- 239000002356 single layer Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 8
- 239000000446 fuel Substances 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 229910052741 iridium Inorganic materials 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 229910052707 ruthenium Inorganic materials 0.000 description 6
- 239000010420 shell particle Substances 0.000 description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 229910052702 rhenium Inorganic materials 0.000 description 4
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000001075 voltammogram Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 101150003085 Pdcl gene Proteins 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- -1 drying for 24 hours Substances 0.000 description 3
- 230000014509 gene expression Effects 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
- 230000001965 increasing effect Effects 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 229920003937 Aquivion® Polymers 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000004758 underpotential deposition Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
(実施例1)
超純水1.5Lに、カーボン粒子(粒子サイズ20~100nm、比表面積100~400m2/g)を3.5g混合して分散した。ここで、前記分散は、バッチタイプの超音波分散器(rpm 4,60min、intensity max)、ホーンタイプの超音波分散器(rpm max、30min、amp 25%)、およびバッチタイプの超音波分散(rpm 4,30min、intensity max)の順に行った。
前記実施例1で製造されたPd@Pt/Cを反応物質とし、実施例1と同様の過程を繰返して、Ptが2層の原子層でコートされたPd@Pt_2ML/Cを製造した。
Pt/Cの商用触媒(Johnson Matthey社、HiSpec4000製品)
Cu-UPD法を用いて製造されたPd@Pt/cコアシェル粒子。
前記実施例1で製造されたパラジウムコア-白金シェルが形成された粒子を、(Pd@Pt/C_CO)を用いて、ハーフセル(half-cell)テストを行った。前記ハーフセルテストの結果は、下記表1の通りである。
前記実施例1で製造されたパラジウムコア-白金シェルが形成された粒子を、(Pd@Pt/C_CO)を用いて、シングルセルテストを行った。この際の条件は、以下の通りであり、シングルセルテストの結果は、下記表3に示している。
燃料極(Anode) : TKKTEC10E50E(50%Pt/C), 「Aquivion」(登録商標) D83(I/C=0.8), Pt loading(0.12 mgPt/cm2)
活性領域(Active area,25cm2)、陽性子交換膜(PEM,NRE-211(25μm)、相対湿度(relative humidify,RH)100%
(実施例3)
その後、フィルター、エタノール、および超純水を用いて洗浄した後、24時間の間、乾燥して、カーボン上に、3層シェル構造(2ML)のパラジウムコア-白金シェルが形成された粒子(Pd@Pt_3ML/C)を製造した。
前記実施例3で製造された各層構造のパラジウムコア-白金シェルが形成された粒子(Pd@Pt/C_CO)を用いて、ハーフセルテストを行った。前記ハーフセルテストの結果は、下記表5の通りである。
(実施例4)
前記実施例1と同様に行い、PdCl2溶液の代わりに、イリジウム(Ir)前駆体を用いて、17.7重量%のイリジウムコア-白金シェルが形成された粒子(Ir@Pt/C)を製造した。
前記実施例1と同様に行い、PdCl2溶液の代わりに、ルテニウム(Ru)前駆体を用いて、17.2重量%のルテニウムコア-白金シェルが形成された粒子(Ru@Pt/C)を製造した。
前記実施例4、5で製造されたコアシェルが形成された粒子を用いて、ハーフセルテストを行った。前記ハーフセルテストの結果は、下記表6の通りである。
Claims (5)
- カーボン粒子が分散した溶液に、パラジウム(Pd)前駆体を添加する第1のステップと、
前記第1のステップの溶液のpHを、10~12に調節する第2のステップと、
前記第2のステップの溶液に1次窒素パージし、一酸化炭素パージを行って、一酸化炭素が吸着されたPd/C粒子を含有する溶液を製造する第3のステップと、
前記第3のステップの溶液に2次窒素パージし、2価白金(Pt)前駆体を添加する第4のステップと、を含むことを特徴とする一酸化炭素を用いたコアシェル粒子の製造方法。 - 前記カーボン粒子が分散した溶液は、溶媒が超純水又は炭素数1~6のアルコールであり、
前記パラジウム(Pd)前駆体は、PdCl2であり、
前記白金前駆体は、K 2 PtCl 4 であることを特徴とする請求項1に記載の一酸化炭素を用いたコアシェル粒子の製造方法。 - 前記第2のステップにおけるpHは、NaOHを用いて調節することを特徴とする請求項1に記載の一酸化炭素を用いたコアシェル粒子の製造方法。
- 前記第2のステップにおけるpHは、11であることを特徴とする請求項1に記載の一酸化炭素を用いたコアシェル粒子の製造方法。
- 前記第4のステップにより製造されたパラジウムコアと、白金シェルが形成された粒子を含有する溶液に、1次窒素パージ、一酸化炭素パージ、及び2次窒素パージを順次行うステップと、
前記パージが行われた溶液に、シェル用白金(Pt)前駆体を添加するステップと、
からなる過程を繰返し行って、パラジウムコアと、多層の白金シェルが形成された粒子を含有する溶液を製造することを特徴とする請求項1に記載の一酸化炭素を用いたコアシェル粒子の製造方法。
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