JP7375723B2 - セパレータ及びセパレータの製造方法 - Google Patents
セパレータ及びセパレータの製造方法 Download PDFInfo
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- JP7375723B2 JP7375723B2 JP2020174915A JP2020174915A JP7375723B2 JP 7375723 B2 JP7375723 B2 JP 7375723B2 JP 2020174915 A JP2020174915 A JP 2020174915A JP 2020174915 A JP2020174915 A JP 2020174915A JP 7375723 B2 JP7375723 B2 JP 7375723B2
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- Prior art keywords
- plane
- titanium
- base material
- metal base
- fuel cell
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title description 11
- 239000010936 titanium Substances 0.000 claims description 152
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 149
- 229910052719 titanium Inorganic materials 0.000 claims description 148
- 229910052751 metal Inorganic materials 0.000 claims description 120
- 239000002184 metal Substances 0.000 claims description 120
- 239000000463 material Substances 0.000 claims description 114
- 239000000446 fuel Substances 0.000 claims description 87
- 239000010935 stainless steel Substances 0.000 claims description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims description 10
- 239000010410 layer Substances 0.000 description 117
- 238000010828 elution Methods 0.000 description 61
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 44
- 238000002441 X-ray diffraction Methods 0.000 description 33
- 239000010408 film Substances 0.000 description 28
- 238000000034 method Methods 0.000 description 25
- 239000002245 particle Substances 0.000 description 25
- 238000004544 sputter deposition Methods 0.000 description 25
- 238000005260 corrosion Methods 0.000 description 24
- 230000007797 corrosion Effects 0.000 description 24
- 229910052799 carbon Inorganic materials 0.000 description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 238000001878 scanning electron micrograph Methods 0.000 description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000011651 chromium Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000000691 measurement method Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002737 fuel gas Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002233 thin-film X-ray diffraction Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
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- H01M8/021—Alloys based on iron
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Description
(1)金属基材上にチタンを含むチタン層が成膜されている燃料電池用セパレータであって、
セパレータ表面のX線回折分析におけるチタンに由来する(100)面、(002)面、及び(101)面のピーク強度をそれぞれ相対強度で除した値の合計に対する(100)面の割合が、16.9%以上である、
前記燃料電池用セパレータ。
(2)セパレータ表面のX線回折分析におけるチタンに由来する(100)面、(002)面、及び(101)面のピーク強度をそれぞれ相対強度で除した値の合計に対する(002)面の割合が、61.0%以下である、(1)に記載の燃料電池用セパレータ。
(3)金属基材がステンレスである、(1)又は(2)に記載の燃料電池用セパレータ。
(4)金属基材上にチタンを含むチタン層が成膜されている燃料電池用セパレータの製造方法であって、
チタン層が、スパッタリング法を用いて、以下:
(a)UBMコイル電流値が6.5A~10Aであるか、又は、
(b)金属基材へのバイアス電圧値が-700V超-150V以下である
条件下で金属基材上に成膜される、
前記方法。
(5)金属基材が凹凸形状を有する、(4)に記載の方法。
本明細書では、適宜図面を参照して本発明の特徴を説明する。図面では、明確化のために各部の寸法及び形状を誇張しており、実際の寸法及び形状を正確に描写してはいない。それ故、本発明の技術的範囲は、これら図面に表された各部の寸法及び形状に限定されるものではない。なお、本発明のセパレータ及びセパレータの製造方法は、下記実施形態に限定されるものではなく、本発明の要旨を逸脱しない範囲において、当業者がおこない得る変更、改良などを施した種々の形態にて実施することができる。
(100)面の割合(配向比率)(%)
={((100)面のピーク強度/(100)面の相対強度)/[((100)面のピーク強度/(100)面の相対強度)+((002)面のピーク強度/(002)面の相対強度)+((101)面のピーク強度/(101)面の相対強度)]}×100
(002)面の割合(配向比率)(%)
={((002)面のピーク強度/(002)面の相対強度)/[((100)面のピーク強度/(100)面の相対強度)+((002)面のピーク強度/(002)面の相対強度)+((101)面のピーク強度/(101)面の相対強度)]}×100
金属基材として燃料電池用セパレータの形状に予めプレスしたステンレス(SUS304)を使用した。SUS表面上の不動態をArエッチングで除去した後、チタン層を、スパッタリング法を使用してSUS上に成膜し、その後導電層としてのカーボン層を、AIP法を使用してチタン層上に成膜することで、燃料電池用セパレータを製造した。得られた燃料電池用セパレータについて、耐食性の評価としての金属溶出量試験を実施し、金属の溶出量が少ないセパレータ(OK品)と鉄(Fe)の溶出量が多いセパレータ(NG品)を選定した。その後、OK品及びNG品のそれぞれについて、チタン層の結晶構造をSEM及びXRDで評価した。
金属基材として燃料電池用セパレータの形状に予めプレスしたステンレス(SUS304)を使用した。SUS表面上の不動態をArエッチングで除去した後、チタン層を、スパッタリング法を使用してSUS上に成膜し、その後導電層としてのカーボン層を、AIP法を使用してチタン層上に成膜することで、燃料電池用セパレータを製造した。得られた燃料電池用セパレータについて、前記の金属溶出量試験を実施し、さらにチタン層の結晶構造をXRDで評価した。
(2)検出されたチタンのメイン回折ピークである(100)面、(002)面、及び(101)面の各ピークを、分析装置内でフィッティングし、各ピークの信号強度を算出した。
(3)各格子面によってピーク強度は異なり、相対強度が存在するため、各格子面のピーク強度を相対強度(理論回折強度)で除した。なお、各格子面の相対強度として各格子面の理論回折強度を使用するための事前測定として、高純度Siの粉末結晶のXRDを、当該測定において使用したXRD装置(SmartLab(株式会社リガク製)、X線:CuKα)を用いて測定し、Siの各格子面の実測されたピーク強度の比と理論回折強度の比がほぼ同一になることを確認した。
(4)(3)で得られた各格子面の(ピーク強度/相対強度)を、各格子面の(ピーク強度/相対強度)の合計で除することによって、各格子面の配向比率を算出した。
実施例2において得られた燃料電池用セパレータについて、XRD回折パターンの結果より、各燃料電池用セパレータのチタンに由来する(002)面の配向比率を、前記の通り算出した。一例としての1つのある燃料電池用セパレータのチタンに由来する(002)面の配向比率の算出方法は、前記表1を参照されたい。
金属基材として燃料電池用セパレータの形状に予めプレスした凹凸形状を有するステンレス(SUS304)を使用した。SUS表面上の不動態をArエッチングで除去した後、チタン層を、スパッタリング法を使用して、UBMコイル電流値を4.0Aとし、金属基材へのバイアス電圧を-75Vとした条件下でSUS上に成膜し、その後導電層としてのカーボン層を、AIP法を使用してチタン層上に成膜することで、燃料電池用セパレータを製造した。
金属基材として燃料電池用セパレータの形状に予めプレスした凹凸形状を有するステンレス(SUS304)を使用した。SUS表面上の不動態をArエッチングで除去した後、チタン層を、スパッタリング法を使用して、UBMコイル電流値を6.5Aとし、金属基材へのバイアス電圧を0V、-50V又は-250Vとした条件下でSUS上に成膜し、その後導電層としてのカーボン層を、AIP法を使用してチタン層上に成膜することで、燃料電池用セパレータを製造した。
金属基材として燃料電池用セパレータの形状に予めプレスした凹凸形状を有するステンレス(SUS304)を使用した。SUS表面上の不動態をArエッチングで除去した後、チタン層を、スパッタリング法を使用して、UBMコイル電流値及び金属基材へのバイアス電圧値を様々に変更した条件下でSUS上に成膜し、その後導電層としてのカーボン層を、AIP法を使用してチタン層上に成膜することで、燃料電池用セパレータを製造した。
Claims (3)
- 金属基材上にチタンを含むチタン層が成膜されている燃料電池用セパレータであって、
以下の式で表されるセパレータ表面のX線回折分析におけるチタンに由来する(100)面、(002)面、及び(101)面のピーク強度をそれぞれ相対強度で除した値の合計に対する(100)面の割合
{((100)面のピーク強度/(100)面の相対強度)/[((100)面のピーク強度/(100)面の相対強度)+((002)面のピーク強度/(002)面の相対強度)+((101)面のピーク強度/(101)面の相対強度)]}×100
が、16.9%以上である、
前記燃料電池用セパレータ。 - 以下の式で表されるセパレータ表面のX線回折分析におけるチタンに由来する(100)面、(002)面、及び(101)面のピーク強度をそれぞれ相対強度で除した値の合計に対する(002)面の割合
{((002)面のピーク強度/(002)面の相対強度)/[((100)面のピーク強度/(100)面の相対強度)+((002)面のピーク強度/(002)面の相対強度)+((101)面のピーク強度/(101)面の相対強度)]}×100
が、61.0%以下である、請求項1に記載の燃料電池用セパレータ。 - 金属基材がステンレスである、請求項1又は2に記載の燃料電池用セパレータ。
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