KR102658181B1 - 금속 코팅층이 형성된 연료전지용 분리판 및 그 제조방법 - Google Patents
금속 코팅층이 형성된 연료전지용 분리판 및 그 제조방법 Download PDFInfo
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- 239000000446 fuel Substances 0.000 title claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 33
- 239000002184 metal Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000011247 coating layer Substances 0.000 title description 13
- 239000000463 material Substances 0.000 claims abstract description 75
- 239000011248 coating agent Substances 0.000 claims abstract description 68
- 238000000576 coating method Methods 0.000 claims abstract description 67
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 27
- 230000008569 process Effects 0.000 claims description 15
- 239000012298 atmosphere Substances 0.000 claims description 5
- 238000009713 electroplating Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000007772 electroless plating Methods 0.000 claims description 4
- 238000005240 physical vapour deposition Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 41
- 238000005260 corrosion Methods 0.000 description 23
- 230000007797 corrosion Effects 0.000 description 23
- 239000010931 gold Substances 0.000 description 14
- 239000003792 electrolyte Substances 0.000 description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 7
- 229910052737 gold Inorganic materials 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 229910052741 iridium Inorganic materials 0.000 description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 229910052707 ruthenium Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002103 nanocoating Substances 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002335 surface treatment layer Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- -1 vacuum Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0258—Collectors; Separators, e.g. bipolar separators; Interconnectors characterised by the configuration of channels, e.g. by the flow field of the reactant or coolant
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0206—Metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0206—Metals or alloys
- H01M8/0208—Alloys
- H01M8/021—Alloys based on iron
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0267—Collectors; Separators, e.g. bipolar separators; Interconnectors having heating or cooling means, e.g. heaters or coolant flow channels
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
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Abstract
Description
도 2는 본 발명의 일 실시예 및 비교예에 따른 백금 코팅 단계를 모식적으로 나타낸 그림이다.
도 3은 본 발명의 일 실시예 및 비교예에 따른 열처리 단계를 모식적으로 나타낸 그림이다.
도 4는 본 발명의 실시예 및 비교예의 접촉저항을 측정하기 위한 시편 및 측정 위치를 설명하기 위한 개략도이다.
구분 | 모재 | 코팅재 (M) |
전해액 (M) |
인가전류 (mA/cm2) |
온도 (℃) |
실시예 1 | SUS316L | 0.1 H2PtCl6 | 0.1 HClO4 | 10 | 60 |
실시예 2 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 60 | |
실시예 3 | 0.05 H2PtCl6 | 0.5 H2SO4 | 10 | 60 | |
실시예 4 | 0.02 K2PtCl6 | 0.1 HClO4 | 20 | 40 | |
실시예 5 | 0.02 K2PtCl6 | 0.5 H2SO4 | 30 | 40 | |
비교예 1 | 5×10-5 H2PtCl6 | 0.5 H2SO4 | 10 | 60 | |
비교예 2 | 0.1 H2PtCl6 | 0.1 HClO4 | 3 | 60 | |
비교예 3 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 50 | |
비교예 4 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 60 | |
실시예 6 | Ti grade 1 | 0.1 H2PtCl6 | 0.1 HClO4 | 10 | 60 |
실시예 7 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 60 | |
실시예 8 | 0.05 H2PtCl6 | 0.5 H2SO4 | 10 | 60 | |
실시예 9 | 0.02 K2PtCl6 | 0.1 HClO4 | 20 | 40 | |
실시예 10 | 0.02 K2PtCl6 | 0.5 H2SO4 | 30 | 40 | |
비교예 5 | 0.1 H2PtCl6 | 0.05 HClO4 | 20 | 60 | |
비교예 6 | 0.1 H2PtCl6 | 0.1 HClO4 | 3 | 60 | |
비교예 7 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 60 | |
비교예 8 | 0.1 H2PtCl6 | 0.1 HClO4 | 20 | 60 |
구분 | 열처리 온도 (℃) |
열처리 시간 (분) |
실시예 1 | 190 | 60 |
실시예 2 | 200 | 60 |
실시예 3 | 210 | 60 |
실시예 4 | 220 | 50 |
실시예 5 | 230 | 40 |
비교예 1 | 210 | 60 |
비교예 2 | 220 | 60 |
비교예 3 | 220 | 120 |
비교예 4 | 150 | 60 |
실시예 6 | 350 | 60 |
실시예 7 | 350 | 40 |
실시예 8 | 450 | 60 |
실시예 9 | 450 | 40 |
실시예 10 | 350 | 60 |
비교예 5 | 350 | 60 |
비교예 6 | 450 | 60 |
비교예 7 | 350 | 120 |
비교예 8 | 250 | 60 |
구분 | 내용 |
부식용액 | 0.1N H2SO4 + 2ppm HF |
용액온도 | 80℃에서 유지 |
작동전극 노출면적 |
1.0 cm2 |
기준전극 | 환산수은전극(MSE) SCE(@0.6V vs SCE) |
상대전극 | 탄소전극봉 |
스캔 속도 | 1 mV/s |
스캔 범위 | -0.25V vs. OCV ~ 1.0 V |
평가기준 | 10 μA/cm2 이하 |
구분 | 계면접촉저항 (mΩ·cm2) |
부식성능 (μA/cm2) |
실시예 1 | 8.3 | 2.5 |
실시예 2 | 9.7 | 1.8 |
실시예 3 | 9.9 | 1.5 |
실시예 4 | 8.9 | 1.9 |
실시예 5 | 9.8 | 1.3 |
비교예 1 | 20.1 | 3.3 |
비교예 2 | 28.2 | 1.2 |
비교예 3 | 42.9 | 0.8 |
비교예 4 | 7.8 | 13.1 |
실시예 6 | 11.2 | 2.2 |
실시예 7 | 9.3 | 2.4 |
실시예 8 | 12.6 | 0.8 |
실시예 9 | 11.7 | 1.2 |
실시예 10 | 10.6 | 2.5 |
비교예 5 | 18.6 | 4.5 |
비교예 6 | 33.2 | 3.1 |
비교예 7 | 38.5 | 0.7 |
비교예 8 | 9.8 | 11.1 |
Claims (8)
- 모재를 마련하는 단계;
상기 모재에 백금(Pt)을 포함하는 코팅재 및 전해액을 적용하여 불연속적인 코팅막을 형성하는 단계; 및 코팅막이 형성된 모재를 열처리 하는 단계;를 포함하며,
상기 모재는 SUS300계 또는 SUS400계이며,
상기 코팅막은, 코팅재를 H2PtCl6 또는 K2PtCl6으로 0.02 내지 0.1 M으로,
전해액으로서 HClO4 또는 H2SO4를 0.1 내지 0.5 M의 범위에서 포함하며,
상기 열처리는 190 내지 230℃에서 40 내지 60분의 범위에서 이루어지는 것;을 특징으로 하는 차량용 연료전지 금속분리판 제조방법.
- 모재를 마련하는 단계;
상기 모재에 백금(Pt)을 포함하는 코팅재 및 전해액을 적용하여 불연속적인 코팅막을 형성하는 단계; 및 코팅막이 형성된 모재를 열처리 하는 단계;를 포함하며,
상기 모재는 Ti grade 1이며,
상기 코팅막은, 코팅재를 H2PtCl6 또는 K2PtCl6으로 0.02 내지 0.1 M으로,
전해액으로서 HClO4 또는 H2SO4를 0.1 내지 0.5 M의 범위에서 포함하며,
상기 열처리는 350 내지 450℃에서 40 내지 60분의 범위에서 이루어지는 것;을 특징으로 하는 차량용 연료전지 금속분리판 제조방법. - 제1항에 있어서, 상기 코팅막 형성 단계는 전해도금, 무전해도금 또는 PVD 공정 중 어느 한 가지를 통해 이루어지는 차량용 연료전지 금속분리판 제조방법.
- 제2항에 있어서, 상기 코팅막 형성 단계는 전해도금, 무전해도금 또는 PVD 공정 중 어느 한 가지를 통해 이루어지는 차량용 연료전지 금속분리판 제조방법.
- 제1항에 있어서, 상기 열처리 단계는 진공상태, 대기 중 및 산소 분위기 중 어느 하나의 조건에서 수행되는 것을 특징으로 하는 차량용 연료전지용 금속분리판 제조방법.
- 제2항에 있어서, 상기 열처리 단계는 진공상태, 대기 중 및 산소 분위기 중 어느 하나의 조건에서 수행되는 것을 특징으로 하는 차량용 연료전지용 금속분리판 제조방법.
- 제1항 내지 제6항 중 어느 하나의 방법으로 제조된 차량용 연료전지 금속분리판.
- 삭제
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AU2022383696A AU2022383696A1 (en) | 2021-11-04 | 2022-11-03 | Separator, having metal coating layer thereon, for fuel cell and manufacturing method therefor |
PCT/KR2022/017131 WO2023080675A1 (ko) | 2021-11-04 | 2022-11-03 | 금속 코팅층이 형성된 연료전지용 분리판 및 그 제조방법 |
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EP22890406.6A EP4428958A1 (en) | 2021-11-04 | 2022-11-03 | Separator, having metal coating layer thereon, for fuel cell and manufacturing method therefor |
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