CA2633147A1 - Stepped gradient fuel electrode and method for making the same - Google Patents

Stepped gradient fuel electrode and method for making the same Download PDF

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Publication number
CA2633147A1
CA2633147A1 CA002633147A CA2633147A CA2633147A1 CA 2633147 A1 CA2633147 A1 CA 2633147A1 CA 002633147 A CA002633147 A CA 002633147A CA 2633147 A CA2633147 A CA 2633147A CA 2633147 A1 CA2633147 A1 CA 2633147A1
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gradient
sub
layers
fuel cell
cell support
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CA002633147A
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French (fr)
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CA2633147C (en
Inventor
Keqin Huang
Harold D. Harter
Paul G. Turkal
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Siemens Energy Inc
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • H01M4/8621—Porous electrodes containing only metallic or ceramic material, e.g. made by sintering or sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • C23C28/3455—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/36—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including layers graded in composition or physical properties
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8636—Inert electrodes with catalytic activity, e.g. for fuel cells with a gradient in another property than porosity
    • H01M4/8642—Gradient in composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • H01M4/8885—Sintering or firing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9041—Metals or alloys
    • H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9066—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of metal-ceramic composites or mixtures, e.g. cermets
    • 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
    • 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
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • 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
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49108—Electric battery cell making

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Ceramic Engineering (AREA)
  • Plasma & Fusion (AREA)
  • Manufacturing & Machinery (AREA)
  • Thermal Sciences (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Inert Electrodes (AREA)
  • Fuel Cell (AREA)

Abstract

The present invention provides a method of depositing a stepped-gradient fuel electrode onto a fuel cell support 2 and the resulting fuel cell, that comprises placing a solid oxide fuel cell support that has at least an air electrode layer 4 and an electrolyte layer 6 into an atmospheric plasma sparying chamber and measuring spray parameters of an atmospheric plasma spray to obtain reactive oxides, conductive metal and graphite phases. Then spraying the spray parameters onto the solid oxide fuel cell support to produce multiple sub-layers 8 on the solid oxide fuel cell support, and adjusting usage of the atmospheric plasma spray. The adjusting of the hydrogen usage comprises using high hydrogen levels for the initial spraying of the sub-layers producing a first gradient region, and as lower hydrogen level for subsequent spraying of the sub-layers, producing a second gradient region.

Claims (19)

1. A method for depositing a stepped-gradient fuel electrode onto a fuel cell support, comprising:
placing a solid oxide fuel cell support that has an air electrode layer and an electrolyte layer into a atmospheric plasma spraying chamber;
measuring spray parameters of an atmospheric plasma spray to obtain reactive oxides, conductive metal and graphite phases;
spraying said spray parameters onto said solid oxide fuel cell support to produce a plurality of sub-layers on said solid oxide fuel cell support; and adjusting a hydrogen gas usage of said atmospheric plasma spray;
wherein the adjusting of said hydrogen gas usage comprises using high hydrogen levels for the initial spraying of said sub-layers producing a first gradient region, and a lower hydrogen gas level for subsequent spraying of said sub-layers, producing a second gradient region;
wherein said first gradient region has a reactive oxides content of 25-50%
by weight;
wherein said second gradient region has a reactive oxides content of 10-25%
by weight.
2. The method of claim 1, wherein said reactive oxides are YSZ/ScSZ.
3. The method of claim 1, wherein said conductive metal is nickel.
4. The method of claim 1, wherein a gun power of said atmospheric plasma spray is 10-20 kWe.
5. The method of claim 1, wherein said first gradient region comprises 1-4 sub-layers.
6. The method of claim 1, wherein said first gradient region has a porosity of not greater than 20%.
7. The method of claim 1, wherein said second gradient region has a porosity of at least 30%.
8. The method of claim 1, wherein said fuel electrode comprises more than two gradient regions.
9 9. The method of claim 1, wherein said spraying is done by indexing said solid oxide fuel cell support.
10. A method for spraying a fuel electrode layer onto a solid oxide fuel cell support, comprising:
using an atmospheric plasma sprayer to spay a plurality of sub-layers onto said fuel cell support, wherein said plurality of sub-layers comprise a reactive YSZ/ScSZ phase, a nickel conductive metal and graphite for porosity, and wherein said sub-layers form said fuel electrode layer;
making multiple adjustments to a hydrogen flow to said plasma sprayer during the spraying of said sub-layers;
wherein each adjustment of said hydrogen flow uses a proportionally greater hydrogen amount than each subsequent adjustment of said hydrogen gas flow, whereby sub-layers produced with proportionally greater hydrogen gas flow have proportionally greater reactive oxides content.
11. The method of claim 10, further comprising indexing said fuel cell support during the method.
12. The method of claim 10, wherein said plurality of sub-layers are 8-14 sub-layers, 7-11 µm in thickness each.
13. The method of claim 10, wherein 2-5 multiple adjustments are made, whereby 2-5 gradient regions are produced.
14. A stepped-gradient fuel electrode deposited on a support tube comprising:
a plurality of sub-layers;
a plurality of gradient regions, wherein each of said comprises at least one of said sub-layers;
wherein said sub-layers comprise a homogenous mixture of reactive oxides and conductive metal, and wherein said sub-layers have a porosity;
wherein initial gradient regions comprise greater reactive oxides concentration than succeeding gradient regions.
15. The stepped-gradient fuel electrode of claim 14, wherein the initial gradient regions comprise 25-50% by weight reactive oxides.
16. The stepped-gradient fuel electrode of claim 14, wherein the succeeding gradient regions comprise 10-25% by weight reactive oxides.
17. The stepped-gradient fuel electrode of claim 14, wherein said reactive oxides are YSZ/ScSZ.
18. The stepped-gradient fuel electrode of claim 14, wherein said conductive metal is nickel.
19. The stepped-gradient fuel electrode of claim 14, wherein the initial gradient regions comprise a lesser porosity than succeeding regions.
CA2633147A 2005-12-08 2006-09-20 Stepped gradient fuel electrode and method for making the same Expired - Fee Related CA2633147C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US11/298,321 2005-12-08
US11/298,321 US7637967B2 (en) 2005-12-08 2005-12-08 Stepped gradient fuel electrode and method for making the same
PCT/US2006/036427 WO2007067242A1 (en) 2005-12-08 2006-09-20 Stepped gradient fuel electrode and method for making the same

Publications (2)

Publication Number Publication Date
CA2633147A1 true CA2633147A1 (en) 2007-06-14
CA2633147C CA2633147C (en) 2011-12-13

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US (1) US7637967B2 (en)
EP (1) EP1964195B1 (en)
JP (1) JP5420250B2 (en)
KR (1) KR101497432B1 (en)
CA (1) CA2633147C (en)
WO (1) WO2007067242A1 (en)

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Also Published As

Publication number Publication date
CA2633147C (en) 2011-12-13
WO2007067242A1 (en) 2007-06-14
KR101497432B1 (en) 2015-03-02
EP1964195A1 (en) 2008-09-03
KR20080074224A (en) 2008-08-12
JP5420250B2 (en) 2014-02-19
JP2009518810A (en) 2009-05-07
US20070134543A1 (en) 2007-06-14
EP1964195B1 (en) 2011-08-10
US7637967B2 (en) 2009-12-29

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