WO2007015692A1 - Electrodeposition of biaxially textured layers on a substrate - Google Patents
Electrodeposition of biaxially textured layers on a substrate Download PDFInfo
- Publication number
- WO2007015692A1 WO2007015692A1 PCT/US2005/027263 US2005027263W WO2007015692A1 WO 2007015692 A1 WO2007015692 A1 WO 2007015692A1 US 2005027263 W US2005027263 W US 2005027263W WO 2007015692 A1 WO2007015692 A1 WO 2007015692A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- biaxially textured
- ceo
- layer
- substrate
- electrodeposited
- Prior art date
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 109
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 229910052768 actinide Inorganic materials 0.000 claims abstract description 10
- 150000001255 actinides Chemical class 0.000 claims abstract description 10
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 10
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 10
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 9
- 150000003624 transition metals Chemical class 0.000 claims abstract description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 99
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 88
- 239000000872 buffer Substances 0.000 claims description 31
- 239000002887 superconductor Substances 0.000 claims description 22
- 229910052741 iridium Inorganic materials 0.000 claims description 17
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 8
- 229910018663 Mn O Inorganic materials 0.000 claims description 6
- 229910003176 Mn-O Inorganic materials 0.000 claims description 6
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 134
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 40
- 239000007789 gas Substances 0.000 description 26
- 238000004549 pulsed laser deposition Methods 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000000151 deposition Methods 0.000 description 14
- 229910001868 water Inorganic materials 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 13
- 230000008021 deposition Effects 0.000 description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 238000004630 atomic force microscopy Methods 0.000 description 7
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical group [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 7
- 238000001636 atomic emission spectroscopy Methods 0.000 description 6
- 230000005291 magnetic effect Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910002480 Cu-O Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- MOOUSOJAOQPDEH-UHFFFAOYSA-K cerium(iii) bromide Chemical compound [Br-].[Br-].[Br-].[Ce+3] MOOUSOJAOQPDEH-UHFFFAOYSA-K 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- KEDNSMBVYXSBFC-UHFFFAOYSA-N 6-bromo-2-chloroquinoline-4-carbonyl chloride Chemical compound C1=C(Br)C=C2C(C(=O)Cl)=CC(Cl)=NC2=C1 KEDNSMBVYXSBFC-UHFFFAOYSA-N 0.000 description 4
- 150000000703 Cerium Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229940105965 yttrium bromide Drugs 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910015901 Bi-Sr-Ca-Cu-O Inorganic materials 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- GDMJROFSHZNDBN-UHFFFAOYSA-N [Br].[Sm] Chemical compound [Br].[Sm] GDMJROFSHZNDBN-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- XKUYOJZZLGFZTC-UHFFFAOYSA-K lanthanum(iii) bromide Chemical compound Br[La](Br)Br XKUYOJZZLGFZTC-UHFFFAOYSA-K 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- MOWMLACGTDMJRV-UHFFFAOYSA-N nickel tungsten Chemical compound [Ni].[W] MOWMLACGTDMJRV-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000005298 paramagnetic effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 150000000921 Gadolinium Chemical class 0.000 description 1
- 239000006173 Good's buffer Substances 0.000 description 1
- 150000001216 Samarium Chemical class 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- LCKCQECDYRMKII-UHFFFAOYSA-N [Br].[Gd] Chemical compound [Br].[Gd] LCKCQECDYRMKII-UHFFFAOYSA-N 0.000 description 1
- BRIAUPCYXMZZHP-UHFFFAOYSA-N [Br].[Y] Chemical compound [Br].[Y] BRIAUPCYXMZZHP-UHFFFAOYSA-N 0.000 description 1
- QTWZFOSNSSAAJU-UHFFFAOYSA-N [Zr].[Br] Chemical compound [Zr].[Br] QTWZFOSNSSAAJU-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- HTFVQFACYFEXPR-UHFFFAOYSA-K iridium(3+);tribromide Chemical compound Br[Ir](Br)Br HTFVQFACYFEXPR-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
- LSWWNKUULMMMIL-UHFFFAOYSA-J zirconium(iv) bromide Chemical compound Br[Zr](Br)(Br)Br LSWWNKUULMMMIL-UHFFFAOYSA-J 0.000 description 1
Classifications
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- 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
-
- 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
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
-
- 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
- C25D5/60—Electroplating characterised by the structure or texture of the layers
-
- 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
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
- C25D5/611—Smooth layers
-
- 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
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/615—Microstructure of the layers, e.g. mixed structure
- C25D5/617—Crystalline layers
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
- C25D7/123—Semiconductors first coated with a seed layer or a conductive layer
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02363—Special surface textures of the semiconductor body itself, e.g. textured active layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/036—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/036—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes
- H01L31/0392—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate
- H01L31/03926—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their crystalline structure or particular orientation of the crystalline planes including thin films deposited on metallic or insulating substrates ; characterised by specific substrate materials or substrate features or by the presence of intermediate layers, e.g. barrier layers, on the substrate comprising a flexible substrate
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/80—Constructional details
- H10N60/85—Superconducting active materials
- H10N60/855—Ceramic superconductors
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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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12639—Adjacent, identical composition, components
- Y10T428/12646—Group VIII or IB metal-base
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
- Y10T428/12861—Group VIII or IB metal-base component
- Y10T428/12875—Platinum group metal-base component
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
- Y10T428/12861—Group VIII or IB metal-base component
- Y10T428/12944—Ni-base component
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
Definitions
- the described subject matter relates to biaxially textured substrates, and more specifically, to electrodeposition of biaxially textured layers on a substrate.
- Superconducting materials are characterized by their very desirable ability to conduct electricity without resistance. These superconducting materials can be deposited onto a variety of substrates for use in a variety of applications, including, e.g., conductive wires, tapes, and electronic devices. To be commercially viable, superconducting materials used in these applications must have a high critical current density (J c ) (i.e., the maximum current density a superconductor can carry at a given temperature and magnetic field) because high electrical current is required to power any significant load. It has been shown that superconducting materials formed with biaxially textured crystalline structures have superior critical current densities.
- J c critical current density
- texturing refers to a cluster structure comprising a number of crystal particles that have the same crystal orientation (e.g., longitudinal axial direction) in a polycrystalline or other material.
- Biaxial texturing describes material in which a significant number of the crystal particles in the cluster structures are oriented generally uniformly in all of the three axes. When viewed under a microscope, biaxially textured superconductor materials appear to have numerous, elongated, crystalline structures oriented in a common longitudinal direction.
- biaxially textured crystalline substrates are critical to obtaining superior critical current densities (J c ) for YBa 2 Cu 3 O 7-S (YBCO) superconductors.
- One way to accomplish biaxial texturing in a superconducting material is to grow epitaxial YBCO onto biaxially textured substrates.
- Rolling-assisted biaxially textured substrate technology has also proven to be very promising for fabricating YBCO-coated conductors that can support large currents in high magnetic fields at 77 K.
- buffer layers are the key component in YBCO superconductors based on rolling-assisted biaxially textured substrates, such as, Ni and nickel alloys.
- buffer layers provide a chemically inert, continuous and smooth base for the growth of the YBCO layer, while transferring the biaxial texture from the substrate to the high- temperature superconductor (HTS) layer. Buffer layers also act as barriers to prevent the diffusion of metal to the HTS layer and oxidation of the metal substrate, because YBCO is processed at about 800 0 C in an oxygen atmosphere of 100 ppm or more.
- Ni-W substrates are sulfurized to form a protective sulfide surface layer.
- Commercial-quality buffer-layer architectures deposited on sulfurized Ni-W are typically CeO 2 /YSZ/Y 2 O 3 /Ni-W and CeO 2 /YSZ/CeO 2 /Ni-W.
- the buffer layers are typically deposited by direct current (DC) magnetron sputtering and pulsed-laser deposition (PLD), which operate at relatively slow deposition rates.
- DC direct current
- PLD pulsed-laser deposition
- An exemplary method of producing at least one biaxially textured layer on a substrate may comprise electrodepositing on the substrate a precursor material selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof.
- the method may be implemented to produce, e.g., a biaxially textured article.
- the method may also be implemented to produce, e.g., a superconductor having a biaxially textured layer.
- Another exemplary method of producing a superconducting material having at least one biaxially textured layer may comprise: selecting a precursor material from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof; and electrodepositing the selected precursor material on a biaxially textured substrate.
- An exemplary biaxially textured material may comprise a biaxially textured base material, and at least one biaxially textured layer selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof.
- the at least one biaxially textured layer is formed by electrodeposition on the biaxially textured base material.
- the substrate may be nickel-based, such as, e.g., Ni metal or Ni-W.
- the precursor material may be selected from the group consisting of CeO 2 , doped CeO 2 , La 2 O 3 , Ir, Ni-Ir, Ni, YSZ, Y 2 O 3 , and La- Mn-O.
- Figure 1 shows an exemplary biaxially textured article as it may be produced according to the methods described herein.
- Figure 2a is a representative XRD scan for annealed CeO 2 and CeO 2 : Sm prepared on a Ni-W substrate.
- Figure 2b is a representative omega scan on the (200) reflection for the annealed CeO 2 and CeO 2 : Sm prepared on a Ni-W substrate.
- Figures 3a and 3b are representative pole-figure scans for the annealed CeO 2 and CeO 2 : Sm prepared on a Ni-W substrate.
- Figures 4a and 4b are representative phi scans of (a) the annealed CeO 2 and CeO 2 : Sm and (b) the Ni-W substrate.
- Figures 5a and 5b are AFM images of the CeO 2 and CeO 2 : Sm layer.
- Figures 6a-d are scanning electron micrograph images of the CeO 2 :Sm layer.
- Figure 7a shows an Atomic Emission Spectrometry (AES) analysis of a superconductor having the structure: YBCOZCeO 2 A 7 SZZED-CeO 2 ZNi-W.
- Figure 7b shows an AES analysis of a YBCO superconductor directly on an ED-CeO 2 ZNi-W substrate to qualify the simple buffer layer architecture.
- AES Atomic Emission Spectrometry
- Figure 8 is a representative XRD diagram of a CYCZIr buffer layer electrodeposited on a Ni-W substrate.
- Figures 9a and 9b are representative pole-figure scans for (a) the CeO 2 and (b) the YSZ of respective layers prepared on a Ni-W substrate.
- Figures 10a and 10b are representative phi scans of (a) the CeO 2 and (b) the YSZ layers prepared on a Ni-W substrate.
- Figure 11a and lib are atomic force microscopy (AFM) micrographs of (a)
- Figures 12a-d are XRD omega and Phi scans of (a and b) a Ni-W substrate, and (c and d) electrodeposited Ni on a Ni-W substrate.
- Figure 13a and 13b are representative (a) XRD omega scan of YBCO superconductor on ED-Ni/Ni-W, and (b) XRD Phi scan of YBCO superconductor on ED-NiZNi-W.
- Figure 14 is a plot of the critical current density versus field of a PLD YBCOZCYCZED-NiZNi-W structure. Detailed Description
- biaxial texturing is accomplished by depositing one or more precursor materials onto a substrate, which itself has a biaxial texture. During the deposition, the growing crystalline particles conform to the same biaxially textured, crystalline orientation of the substrate. By growing a superconductor layer on a biaxially textured substrate, the biaxial texturing of the substrate is maintained in the resulting superconductor article.
- Biaxially textured layers may be prepared on a substrate inexpensively by an electrodeposition method. Electrodeposition is a low-cost, non-vacuum, high-rate deposition process that deposits uniform layer (or "layers") on large non-planar substrates. Exemplary embodiments discussed herein include biaxially textured layers of rare earths, transition metals, actinides, lanthanides, and oxides thereof.
- the precursor material may be selected from the group consisting of CeO 2 , doped CeO 2 , La 2 O 3 , Ir, Ni-Ir, Ni, YSZ, Y 2 O 3 , and La-Mn-O.
- Figure 1 shows an exemplary biaxially textured article 150 as it may be produced according to the methods described herein.
- Exemplary biaxially textured article 150 is shown having an outer layer 110 grown epitaxially over a buffer layer 120 on a substrate 130. It is noted, however, that the biaxially textured article 150 need not include two layers 110 and 120. For example, only one layer may be applied, or more than two layers may be applied.
- biaxial texturing refers to both partial and complete biaxial texturing, e.g., as indicated by X-ray diffraction scans.
- Each layer 110 and 120 may be textured relative to the substrate 130 such that the layers 110 and 120 have the same biaxial crystalline orientation as the substrate 130. That is, the biaxial texturing of the substrate 130 (indicated by arrows 135) induces corresponding biaxial texturing in the buffer layer 120 (indicated by arrows 125), which in turn induces corresponding biaxial texturing in the in outer layer 110, (indicated by arrows 115).
- the substrate 130 may be either a flexible or rigid metal or other material that can be fabricated into a variety of shapes, sizes and thicknesses.
- the substrate 130 may have any desired thickness, e.g., between about 0.005 and 0.5 millimeters (mm).
- Suitable metals include, but are not limited to, nickel, copper, titanium, palladium, and/or combinations or alloys thereof (e.g., nickel-tungsten (Ni-W) and nickel-chromium alloys).
- the substrate 130 may be biaxially textured, e.g., by a well-known process referred to as rolling-assisted biaxially textured substrates (RABiTS). While a biaxially textured substrate 130 is not required, use of a biaxially textured substrate 130 may enhance the ability to achieve biaxial texturing in the layers 110 and 120.
- RABiTS rolling-assisted biaxially textured substrates
- the layers 110 and 120 may be deposited onto the substrate 130 by electrodeposition in a chemical bath. Electrodeposition is generally performed at between about 0.05 and 25 mA/cm 2 , for between about 1 and 45 minutes, as discussed in more detail below in the Examples. Thicker layers may be produced by increasing the deposition time and/or a multilayer deposition process. In a multilayer deposition process, electrodeposited layer 120 has biaxial texturing, which provides an optimal surface for electrodeposition of the next layer 110.
- biaxial texturing may be enhanced by annealing in a suitable gas or mixture of gasses, such as, e.g., argon (Ar) and a forming gas.
- a suitable gas or mixture of gasses such as, e.g., argon (Ar) and a forming gas.
- the annealing process may be performed at between about 750 and 1200°C for between about 12 and 48 hours. Of course, any suitable annealing process maybe implemented.
- CeO 2 and doped CeO 2 layers may be electrodeposited on a biaxially textured nickel-based substrate, e.g., to form a buffer layer as follows.
- a CeO 2 layer (undoped) may be prepared in a bath containing cerium salt dissolved in deionized water.
- doped CeO 2 layers may be prepared, e.g., using samarium (Sm), gadolinium (Gd), and zirconium (Zr) or other elements, especially rare earths, transition, lanthanides and actinides.
- a Sm-doped CeO 2 layer may be prepared in a bath containing cerium salt and samarium salt dissolved in deionized water.
- a Gd-doped CeO 2 layer may be prepared in a bath containing cerium salt and gadolinium salt dissolved in deionized water.
- a Zr-doped CeO 2 layer may be prepared from a bath containing cerium salt and zirconium salt dissolved in deionized water.
- the layers may be electrodeposited in a vertical cell in which the electrodes (both working and counter electrodes) are suspended vertically from the top of the cell. Electrodeposition of the layers on a substrate may be performed at room temperature (about 22 to 25 °C) with constant stirring.
- the substrate may be a nickel-based substrate, such as, Ni-W (3% by weight or 3 wt%).
- the substrate may be a flat, 10 centimeter (cm) x 0.5 cm, Ni-W substrate, improved by an electropolishing technique.
- the electropolishing technique may include providing the substrate in a 5 vol% hydrazine hydrate solution at +0.6 V, where the Pt counter and Pt pseudo-reference electrode are shorted together.
- the electrodeposition precursors may be prepared at a commercially favorable constant current mode of about —2 volts (V), where the platinum (Pt) counter and Pt pseudo-reference electrodes are shorted together.
- the duration of electrodeposition may be less than 50 minutes, e.g., in the range of 3 to 20 minutes.
- a Princeton Applied Research potentiostat/galvanostat (Model 273A) with an IBM PC AT computer interface may be used to prepare the electrodeposition layers.
- XRD X-ray diffraction
- Out- of-plane alignment may be determined from an omega scan on the (200) CeO 2 reflection.
- In-plane alignment may be estimated from a pole figure and phi scans on the CeO 2 (111) reflection.
- the Gaussian distribution may be fitted to the phi- and omega-scan data to estimate full width at half maximum (FWHM).
- Layer morphology may be observed by scanning electron micrographs (SEM).
- Electrodeposited layer roughness may also be estimated from Atomic Force Microscopy (AFM) scans.
- AFM Atomic Force Microscopy
- Figure 2a is a representative XRD scan for annealed CeO 2 and CeO 2 :Sm prepared on a Ni-W substrate. It is observed that only the c-axis-oriented (200) CeO 2 reflection can be identified, but the intensity of Sm-doped layers is much higher due to better crystallinity and greater thickness.
- Figure 2b is a representative omega scan on the (200) reflection for the annealed CeO 2 and CeO 2 :Sm prepared on a Ni-W substrate. It is observed that the dispersion along the c-axis of the undoped CeO 2 and Sm-doped CeO 2 grains are as low as 3.8° and 3.5°, respectively.
- FIGS 3a and 3b are representative pole-figure scans for the annealed CeO 2 and CeO 2 : Sm prepared on a Ni-W substrate. The pole-figure scans show that CeO 2 and CeO 2 --Sm are biaxially textured.
- Figures 4a and 4b are representative phi scans of (a) the annealed CeO 2 and CeO 2 :Sm, and (b) the Ni-W substrate. It is observed in Figure 4a that an average in-plane mosaic spread from the phi scan of the CeO 2 layer is about 6.1°. The average in-plane mosaic spread from the phi scan of the CeO 2 :Sm layer is about 6.4°. It is observed in Figure 4b that an average in-plane mosaic spread from the phi-scan of the base Ni-W substrate is 7.6°.
- the improved values of omega and phi may be attributed to the relatively small grain size of the electrodeposited CeO 2 and CeO 2 : Sm precursor layers, which also show better grain alignment after annealing.
- FIGS 5a and 5b are AFM images of the CeO 2 and CeO 2 : Sm layer. It is observed that the average layer roughness is about 3 run.
- Figures 6a-d are SEM images of the CeO 2 : Sm layer. It is observed that both layers are free from any cracks.
- PLD pulsed laser deposition
- PLD is a well known technique, wherein a laser is focused on a target including the buffer material to be deposited. The incident laser generates a plume of buffer material from the target surface. The substrate is heated and positioned in the path of this plume to deposit the buffer material in the plume on the substrate.
- An exemplary YBCO superconductor may be produced, e.g., by PLD of a YSZ layer, PLD of a CeO 2 layer, and PLD of a YBCO layer over the electrodeposited CeO 2 layer to illustrate Ni inter-diffusion from the Ni-W substrate.
- Figure 7a shows an Atomic Emission Spectrometry (AES) analysis of a superconductor having the structure: YBCO/CeO/TSZ/ED-CeO ⁇ i- W. It is observed that Ni inter-diffusion is completely stopped at the first electrodeposited CeO 2 layer.
- Figure 7b shows an AES analysis of a YBCO superconductor directly on an ED- CeO 2 /Ni-W substrate to qualify the simple buffer layer architecture. It is observed that Ni inter-diffusion is stopped, but Ni penetrates deep inside the CeO 2 layer.
- AES Atomic Emission Spectrometry
- Iridium has excellent oxidation and corrosion resistance.
- iridium layers may be electrodeposited on a biaxially textured nickel-based substrate to form a buffer layer as follows.
- the iridium layer may be electrodeposited using a bath containing only Ir salt at 65 0 C.
- a vertical cell may be implemented in which the electrodes (both working and counter) are suspended vertically from the top of the cell.
- the electrodeposition precursors may be prepared at about -1.2 V for 2 to 45 minutes on a Ni-W (3 wt%) substrate, where the Pt counter and Pt pseudo-reference electrodes are shorted together.
- PLD pulsed laser deposition
- CeO 2 AfSZZCeO 2 structure and a simplified PLD YSZ/CeO 2 structure may be deposited on top of the Ir-coated Ni-W substrates.
- the electrodeposited Ir/metal substrates are first heated to 800 0 C in 500 mTorr of the forming gas, and then a CeO 2 seed layer is deposited in 180 mTorr of the forming gas. Subsequently, YSZ and CeO 2 layers are deposited sequentially in 0.1 mTorr of oxygen.
- the laser beam may be focused onto a 3 x 1 cm 2 spot on a target at a 45° angle, with a fluence of 2-3 J/cm 2 .
- the surface of YSZ (3 mole% Y 2 O 3 ) and CeO 2 targets may be cleaned in situ by exposure to 1000 laser shots prior to every deposition.
- the substrates may be mounted on the substrate holder-cum-heater, and the chamber evacuated to a base pressure of about 10 "6 torr prior to deposition.
- the target-to-substrate distance is kept at about 8 cm, and layers of YSZ and CeO 2 are deposited sequentially.
- Figure 8 is a representative XRD diagram of a CYC/Ir buffer layer electrodeposited on a Ni-W substrate.
- the XRD diagram of CeO 2 /YSZ/CeO 2 /Ir/Ni-W shows the epitaxial (001) phase formation for each deposited layer. No NiO phase formation was observed on this type of buffer architecture, even though the layers were annealed at 800°C.
- Out-of-plane omega values of the biaxially textured buffer layers were 6.5° and 8.7° for YSZ(200) and CeO 2 (200), respectively.
- Figures 9a and 9b are representative pole-figure scans for (a) the CeO 2 and (b) the YSZ layers prepared on a Ni-W substrate. It is observed that the CeO 2 top layer and YSZ are cube-textured.
- Figures 10a and 10b are representative phi scans of (a) the CeO 2 and (b) the YSZ of respective layers prepared on a Ni-W substrate. It is observed that the in-plane texture values (phi scan) of YSZ and CeO 2 were 7.0° and 8.0°, respectively.
- the final buffer layer configuration may be CeO 2 ZYSZZIr on a Ni-W substrate. Results for these structures are comparable to the CYCZIr configuration, and indicate a cube texture.
- Figure 11a and lib are atomic force microscopy (AFM) micrographs of (a) CeO 2 ZYSZZCeO 2 ZIrZNi-W and (b) CeO 2 ZYSZZIrZNi-W.
- the AFM micrographs show smooth, continuous, crack-free buffer architectures for both CeO 2 ZYSZZCeO 2 ZIrZNi-W and CeO 2 ZYSZZIrZNi-W.
- the average roughness is about 3 nm for the CYZIrZNi-W, and about 9 nm for the CYCZIrZNi-W.
- Electrodeposition of Ni may be performed using a bath containing 66g NiSO 4 ⁇ xH 2 O, 9g NiCl 2 ⁇ 6 H 2 O, and 7.6g boric acid dissolved in 200 mL of deionized water. Again, the layers may be deposited in a vertical cell in which the electrodes (both working and counter) are suspended vertically from the top of the cell at 65 0 C and without stirring.
- the electrodeposition precursors may be prepared by applying 0.4 mAZcm 2 current density at 65 0 C for 60 minutes, where the Pt counter and Pt pseudo-reference electrode are shorted together.
- the Ni-W substrate may be improved by an electro-polishing technique. Electropolishing of the Ni-W substrate may be done in 5 vol% hydrazine hydrate solution at -50 ⁇ AZcm 2 (at a corresponding voltage of about +0.8 V) where the Pt counter and Pt pseudo-reference electrode are shorted together.
- a Princeton Applied Research potentiostat/galvanostat Model 273 A with an IBM PC AT computer interface may be used to prepare electrodeposition layers.
- the thickness of the electrodeposition Ni layers is about 2.0 ⁇ m.
- the as-electrodeposited Ni layers are biaxially textured crystalline layers.
- the buffer structures are completed on these types of seed ED-Ni layers by PLD
- the electrodeposited Ni/Ni-W (3%) layer may be annealed at 850°C in 1 torr forming gas.
- a CeO 2 seed layer may be deposited at 850 0 C in 180 mtorr forming gas.
- the subsequent YSZ and CeO2 cap layers may be deposited at 850 0 C in 0.1 mtorr oxygen.
- the qualities of the ED-Ni layer may be assessed by depositing a PLD YBCO layer.
- PLD deposition of 300-nm-thick YBCO may be performed using a RrF excimer laser system, operated at a fluence of 2-3 J/cm 2 , the substrate held at 78O 0 C under an oxygen partial pressure of 150 mtorr.
- 0.5- ⁇ m-thick silver (Ag) contacts may be deposited by DC magnetron sputtering, and the samples annealed in flowing oxygen at 500 0 C for 90 min.
- Transport critical current (J c ) measurements may be performed at liquid nitrogen ( ⁇ 77 K) in varying applied magnetic fields using a standard 4-probe technique and the l ⁇ V/cm criterion.
- Figures 12a-d are XRD Omega and Phi scans of (a and b) a Ni-W substrate, and (c and d) electrodeposited Ni on a Ni-W substrate.
- Full-width at half-maximum (FWHM) values of the ⁇ scan (out-of-plane) and ⁇ scan (in-plane) of the Ni-W substrate are (a) 6.0° and (b) 8.3°.
- Full-width at half-maximum (FWHM) values of the ⁇ scan (out-of- plane) and ⁇ scan (in-plane) of the electrodeposited Ni layer are (c) 7.1° and (d) 7.0°, which is comparable to the base Ni-W (3%) substrates and indicates good biaxial texturing.
- the relatively small grain size of the electrodeposited Ni layer is helpful for growing a higher-quality superconductor layer.
- Figure 13a and 13b are representative XRD omega and Phi scans of (a) YBCO superconductor on ED-Ni/Ni-W, and (b) YBCO superconductor on ED-Ni/Ni-W.
- the XRD theta/2 theta scans show very good YBCO phase formation with some impurity-Ni (111) phase.
- Figure 14 is a plot of the critical current density versus field of a PLD YBCO/CYC/ED-Ni/Ni-W structure. It is observed that the critical current density at varying magnetic fields for a YBCO layer grown on an ED-Ni-based buffer layer is about 1.8 MA/cm 2 at 75.2K in a 600 Gauss magnetic field.
- high temperature superconductors may be produced by electrodepositing high temperature superconducting materials on the buffer layer to produce, e.g., Y-Ba 2 Cu 3 Ox (YBCO), Bi-Sr-Ca- Cu-O (BSCCO), Tl-Ba-Ca-Cu-O (TBCCO), Pb-Ba-Sr-Ca-Cu-O (PBSCCO), Tl-Sr-Ba-Ca-Cu-O (TSBCCO), Tl-Pb-Sr-Ba-Ca-Cu-O (TPSBCCO), Hg-Ba-Ca-Cu-O (HBCCO).
- YBCO Y-Ba 2 Cu 3 Ox
- BSCCO Bi-Sr-Ca- Cu-O
- THCCO Pb-Ba-Sr-Ca-Cu-O
- PBSCCO Pb-Ba-Sr-Ca-Cu-O
- TBSBCCO Tl-Pb-Sr-Ba-Ca-
- the superconducting material may be deposited epitaxially, such that the superconducting material has the same crystalline orientation as the buffer layer.
- crystalline silicon may be grown on the substrate to produce solar cells. Still other applications are also contemplated and will become readily apparent to those having ordinary skill in the art after becoming familiar with the teachings herein.
- Electrodeposited CeO 7 In this example, biaxially textured CeO 2 was prepared on Ni and Ni-W substrates. Specifically, 0.5g of cerium bromide was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.26 mA/cm 2 current density at room temperature (about 22°C) for 10 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 980 0 C in a mixture of Ar gas (95%) and a 5% forming gas [H 2 (10%)/N 2 ]. Electrodeposited Samarium doped CeO?. In this example, biaxially textured
- CeO 2 : Sm was prepared on Ni and Ni-W substrates. Specifically, 0.5g cerium bromide and O.Olg Samarium bromine was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.26 mA/cm 2 current density at room temperature (about 22°C) for 15 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 980 0 C in a mixture of Ar gas (95%) and a 5% forming gas [H 2 (10%)/N 2 ]. Electrodeposited CeO?;Gd. In this example, biaxially textured CeO 2 :Gd was prepared on a Ni-W substrate.
- 0.5g cerium bromide and 0.02g gadolinium bromine was dissolved in 200 niL of water.
- the layer was electrodeposited by applying 0.3 niA/cm 2 current density at room temperature (about 22°C) for 10 minutes.
- the electrodeposited layer was annealed at 1020 0 C in a mixture of Ar gas provided at 60 pounds per square inch (psi) and a forming gas [H 2 (10%)/N 2 ] provided at 2.5 psi for 2 hours.
- Electrodeposited CeO?:Zr biaxially textured CeO 2 :Zr was prepared on a Ni-W substrate. Specifically, 0.5g cerium bromide and 0.18g zirconium bromine was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.4 niA/cm 2 current density at room temperature (about 22°C) for 5 minutes. The electrodeposited layer was annealed at 1020 0 C in a mixture of Ar gas provided at 60 psi and forming gas [H 2 (10%)/N 2 ] provided at 2.5 psi for 2 hours.
- Electrodeposited La ⁇ O ⁇ In this example, biaxially textured La 2 O 3 was prepared on a Ni-W substrate. Specifically, O.lg lanthanum bromide was dissolved in a mixture of 100 mL of water (20%) and isopropyl alcohol (80%). The layer was electrodeposited by applying 0.4 niA/cm 2 current density at room temperature (about 22°C) for 10 minutes. The electrodeposited layer was annealed at 1030 0 C in a mixture of Ar gas (95%) and 5% forming gas [H 2 (10%)/N 2 ]. Electrodeposited Iridium (Ir). In this example, biaxially textured iridium was prepared on a Ni-W substrate. Specifically, 0.5g iridium bromide was dissolved in 100 mL of water. The layer was electrodeposited by applying 1 mA/cm 2 current density at 65° C for 15 minutes.
- Electrodeposited Ni-Ir In this example, biaxially textured Ni-Ir was prepared on a Ni-W substrate. Specifically, 66g NiSO 4 , 9g NiCl 2 , 7.6g boric acid, and 0.5g IrBr 3 was dissolved in 250 mL of water. The layer was electrodeposited by applying 0.4 niA/cm 2 current density at 65 0 C for 15 minutes.
- biaxially textured Ni was prepared on a Ni-W substrate. Specifically, 66g NiSO 4 , 9g NiCl 2 , and 7.6g boric acid was dissolved in 250 mL of water. The layer was electrodeposited by applying 0.4 mA/cm 2 current density at 65°C for 60 minutes.
- biaxially textured YSZ was prepared on a Ni-W substrate. Specifically, 2.1g zirconium bromide and 0.05g yttrium bromine was dissolved in 100 mL of water. The layer was electrodeposited by applying 3 mA/cm 2 current density at room temperature (about
- Electrodeposited Y 7 O ⁇ In this example, biaxially textured Y 2 O 3 was prepared on a Ni-W substrate. Specifically, 0.5g yttrium bromide was dissolved in a mixture of 100 mL of water (30%) and isopropyl alcohol (70%). The layer was electrodeposited by applying 0.8 mA/cm 2 current density at room temperature (about 22° C) for 15 minutes. The electrodeposited layer was annealed at 980 0 C in a mixture of Ar gas (95%) and a 5% forming gas [H 2 (10%)/N 2 ].
- biaxially textured Y 2 O 3 was prepared on a Ni-W as follows: 0.5g yttrium bromide was dissolved in 200 mL of isopropyl alcohol (isopropanol). The layer was electrodeposited by applying 0.1 mA/cm 2 current density at room temperature (about 22°C) for 30 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 1100 0 C in a mixture of Ar gas provided at 20 psi and a forming gas [H 2 (10%)/N 2 ] provided at 2.5 psi.
- biaxially textured Y 2 O 3 was prepared on a Ni-W substrate as follows: 1.Og yttrium bromide was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.8 mA/cm 2 current density at room temperature (about 22°C) for 20 minutes. The solution is stirred during deposition. The electrodeposited layer was annealed at 1100 0 C in a mixture of Ar gas provided at 20 psi and a forming gas [H 2 (10%)/N 2 ] provided at 2.5 psi.
- Electrodeposited La-Mn-Q In this example, biaxially textured La-Mn-O was prepared on a Ni-W substrate. Specifically, 0.7g lanthanum bromide and 0.6g Manganese bromide were dissolved in 200 mL of water. The layer was electrodeposited by applying 0.8 mA/cm 2 current density at room temperature (about 22°C) for 15 minutes. The electrodeposited layer was annealed at 990 0 C in a mixture of Ar gas (95%) and a 5% forming gas [H 2 (10%)/N 2 ]. Electrodeposited CeO? on electrodeposited Y 2 O ⁇ ZNi-W. In this example, biaxially textured CeO 2 was prepared on a Y 2 O 3 /Ni-W substrate.
- yttrium bromide was dissolved in 200 mL of isopropanol.
- the Y 2 O 3 layer was electrodeposited by applying 0.1 mA/cm current density at room temperature (about 22°C) for 30 minutes on a Ni-W substrate. The solution was stirred during deposition to form the Y 2 O 3 /Ni-W substrate.
- CeO2 was electrodeposited on the Y 2 O 3 /Ni-W substrate. Specifically, 0.5g cerium bromide and 0.0 Ig samarium bromine was dissolved in 200 mL of water. The CeO 2 layer was electrodeposited by applying 0.26 mA/cm 2 current density. The electrodeposited layer was annealed at 990 0 C in a mixture of Ar gas (95%) and a 5% forming gas [H 2 (10%)/N 2 ].
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Abstract
Methods of producing one or more biaxially textured layer on a substrate, and articles produced by the methods, are disclosed. An exemplary method may comprise electrodepositing on the substrate a precursor material selected from the group consisting of rare earths, transition metals, actinide, lanthanides, and oxides thereof. An exemplary article (150) may comprise a biaxially textured base material (130), and at least one biaxially textured layer (110) selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof. The at least one biaxially textured layer (110) is formed by electrodeposition on the biaxially textured base material (130).
Description
ELECTRODEPOSITION OF BIAXIALLY TEXTURED LAYERS ON A SUBSTRATE
Contractual Origin
The United States Government has rights in this invention under Contract No. DE-AC36- 99GO 10337 between the United States Department of Energy and the National Renewable Energy Laboratory, a Division of the Midwest Research Institute.
Technical Field
The described subject matter relates to biaxially textured substrates, and more specifically, to electrodeposition of biaxially textured layers on a substrate.
Background
Superconducting materials are characterized by their very desirable ability to conduct electricity without resistance. These superconducting materials can be deposited onto a variety of substrates for use in a variety of applications, including, e.g., conductive wires, tapes, and electronic devices. To be commercially viable, superconducting materials used in these applications must have a high critical current density (Jc) (i.e., the maximum current density a superconductor can carry at a given temperature and magnetic field) because high electrical current is required to power any significant load. It has been shown that superconducting materials formed with biaxially textured crystalline structures have superior critical current densities. Generally, texturing refers to a cluster structure comprising a number of crystal particles that have the same crystal orientation (e.g., longitudinal axial direction) in a polycrystalline or other material. Biaxial texturing describes material in which a significant number of the crystal particles in the cluster structures are oriented generally uniformly in all of the three axes. When viewed under a microscope, biaxially textured superconductor materials appear to have numerous, elongated, crystalline structures oriented in a common longitudinal direction.
It is now well established that biaxially textured crystalline substrates are critical to obtaining superior critical current densities (Jc) for YBa2Cu3O7-S (YBCO) superconductors. One way to accomplish biaxial texturing in a superconducting material
is to grow epitaxial YBCO onto biaxially textured substrates. Rolling-assisted biaxially textured substrate technology has also proven to be very promising for fabricating YBCO-coated conductors that can support large currents in high magnetic fields at 77 K. In any case, buffer layers are the key component in YBCO superconductors based on rolling-assisted biaxially textured substrates, such as, Ni and nickel alloys. These buffer layers provide a chemically inert, continuous and smooth base for the growth of the YBCO layer, while transferring the biaxial texture from the substrate to the high- temperature superconductor (HTS) layer. Buffer layers also act as barriers to prevent the diffusion of metal to the HTS layer and oxidation of the metal substrate, because YBCO is processed at about 8000C in an oxygen atmosphere of 100 ppm or more.
Recently, more attention has been given to paramagnetic Ni-W substrates to improve mechanical properties and reduce magnetism. Growth of oxide buffer layers directly on textured paramagnetic Ni-W substrates under typical conditions is challenging because the localized formation of tungsten oxide can deteriorate the properties of oxide buffer layers and YBCO layers. Currently, Ni-W substrates are sulfurized to form a protective sulfide surface layer. Commercial-quality buffer-layer architectures deposited on sulfurized Ni-W are typically CeO2/YSZ/Y2O3/Ni-W and CeO2/YSZ/CeO2/Ni-W. At present, the buffer layers are typically deposited by direct current (DC) magnetron sputtering and pulsed-laser deposition (PLD), which operate at relatively slow deposition rates.
The foregoing examples of the related art and limitations related therewith are intended to be illustrative and not exclusive. Other limitations of the related art will become apparent to those of skill in the art upon a reading of the specification and a study of the drawings.
Summary
The following embodiments and aspects thereof are described and illustrated in conjunction with systems, tools and methods that are meant to be exemplary and illustrative, not limiting in scope. In various embodiments, one or more of the above- described problems have been reduced or eliminated, while other embodiments are directed to other improvements.
An exemplary method of producing at least one biaxially textured layer on a substrate may comprise electrodepositing on the substrate a precursor material selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof. The method may be implemented to produce, e.g., a biaxially textured article. The method may also be implemented to produce, e.g., a superconductor having a biaxially textured layer.
Another exemplary method of producing a superconducting material having at least one biaxially textured layer may comprise: selecting a precursor material from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof; and electrodepositing the selected precursor material on a biaxially textured substrate.
An exemplary biaxially textured material may comprise a biaxially textured base material, and at least one biaxially textured layer selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof. The at least one biaxially textured layer is formed by electrodeposition on the biaxially textured base material.
In exemplary embodiments, the substrate may be nickel-based, such as, e.g., Ni metal or Ni-W. Also in exemplary embodiments, the precursor material may be selected from the group consisting of CeO2, doped CeO2, La2O3, Ir, Ni-Ir, Ni, YSZ, Y2O3, and La- Mn-O.
In addition to the exemplary aspects and embodiments described above, further aspects and embodiments will become apparent by reference to the drawings and by study of the following descriptions.
Brief Description of the Drawings
Exemplary embodiments are illustrated in referenced figures of the drawings. It is intended that the embodiments and figures disclosed herein are to be considered illustrative rather than limiting.
Figure 1 shows an exemplary biaxially textured article as it may be produced according to the methods described herein.
Figure 2a is a representative XRD scan for annealed CeO2 and CeO2: Sm prepared on a Ni-W substrate. Figure 2b is a representative omega scan on the (200) reflection for the annealed CeO2 and CeO2: Sm prepared on a Ni-W substrate.
Figures 3a and 3b are representative pole-figure scans for the annealed CeO2 and CeO2: Sm prepared on a Ni-W substrate.
Figures 4a and 4b are representative phi scans of (a) the annealed CeO2 and CeO2: Sm and (b) the Ni-W substrate.
Figures 5a and 5b are AFM images of the CeO2 and CeO2: Sm layer.
Figures 6a-d are scanning electron micrograph images of the CeO2:Sm layer. Figure 7a shows an Atomic Emission Spectrometry (AES) analysis of a superconductor having the structure: YBCOZCeO2A7SZZED-CeO2ZNi-W. Figure 7b shows an AES analysis of a YBCO superconductor directly on an ED-CeO2ZNi-W substrate to qualify the simple buffer layer architecture.
Figure 8 is a representative XRD diagram of a CYCZIr buffer layer electrodeposited on a Ni-W substrate.
Figures 9a and 9b are representative pole-figure scans for (a) the CeO2 and (b) the YSZ of respective layers prepared on a Ni-W substrate.
Figures 10a and 10b are representative phi scans of (a) the CeO2 and (b) the YSZ layers prepared on a Ni-W substrate. Figure 11a and lib are atomic force microscopy (AFM) micrographs of (a)
CeO2ZYSZZCeO2ZIrZNi-W and (b) CeO2ZYSZZIrZNi-W.
Figures 12a-d are XRD omega and Phi scans of (a and b) a Ni-W substrate, and (c and d) electrodeposited Ni on a Ni-W substrate.
Figure 13a and 13b are representative (a) XRD omega scan of YBCO superconductor on ED-Ni/Ni-W, and (b) XRD Phi scan of YBCO superconductor on ED-NiZNi-W.
Figure 14 is a plot of the critical current density versus field of a PLD YBCOZCYCZED-NiZNi-W structure.
Detailed Description
Briefly, biaxial texturing is accomplished by depositing one or more precursor materials onto a substrate, which itself has a biaxial texture. During the deposition, the growing crystalline particles conform to the same biaxially textured, crystalline orientation of the substrate. By growing a superconductor layer on a biaxially textured substrate, the biaxial texturing of the substrate is maintained in the resulting superconductor article.
Biaxially textured layers may be prepared on a substrate inexpensively by an electrodeposition method. Electrodeposition is a low-cost, non-vacuum, high-rate deposition process that deposits uniform layer (or "layers") on large non-planar substrates. Exemplary embodiments discussed herein include biaxially textured layers of rare earths, transition metals, actinides, lanthanides, and oxides thereof. For example, the precursor material may be selected from the group consisting of CeO2, doped CeO2, La2O3, Ir, Ni-Ir, Ni, YSZ, Y2O3, and La-Mn-O. Figure 1 shows an exemplary biaxially textured article 150 as it may be produced according to the methods described herein. Exemplary biaxially textured article 150 is shown having an outer layer 110 grown epitaxially over a buffer layer 120 on a substrate 130. It is noted, however, that the biaxially textured article 150 need not include two layers 110 and 120. For example, only one layer may be applied, or more than two layers may be applied.
As used herein, the term "biaxial texturing" refers to both partial and complete biaxial texturing, e.g., as indicated by X-ray diffraction scans. Each layer 110 and 120 may be textured relative to the substrate 130 such that the layers 110 and 120 have the same biaxial crystalline orientation as the substrate 130. That is, the biaxial texturing of the substrate 130 (indicated by arrows 135) induces corresponding biaxial texturing in the buffer layer 120 (indicated by arrows 125), which in turn induces corresponding biaxial texturing in the in outer layer 110, (indicated by arrows 115).
The substrate 130 may be either a flexible or rigid metal or other material that can be fabricated into a variety of shapes, sizes and thicknesses. The substrate 130 may have any desired thickness, e.g., between about 0.005 and 0.5 millimeters (mm). Suitable metals include, but are not limited to, nickel, copper, titanium, palladium, and/or
combinations or alloys thereof (e.g., nickel-tungsten (Ni-W) and nickel-chromium alloys).
The substrate 130 may be biaxially textured, e.g., by a well-known process referred to as rolling-assisted biaxially textured substrates (RABiTS). While a biaxially textured substrate 130 is not required, use of a biaxially textured substrate 130 may enhance the ability to achieve biaxial texturing in the layers 110 and 120.
The layers 110 and 120 may be deposited onto the substrate 130 by electrodeposition in a chemical bath. Electrodeposition is generally performed at between about 0.05 and 25 mA/cm2, for between about 1 and 45 minutes, as discussed in more detail below in the Examples. Thicker layers may be produced by increasing the deposition time and/or a multilayer deposition process. In a multilayer deposition process, electrodeposited layer 120 has biaxial texturing, which provides an optimal surface for electrodeposition of the next layer 110.
After electrodeposition, biaxial texturing may be enhanced by annealing in a suitable gas or mixture of gasses, such as, e.g., argon (Ar) and a forming gas. The annealing process may be performed at between about 750 and 1200°C for between about 12 and 48 hours. Of course, any suitable annealing process maybe implemented.
Having generally described biaxial textured articles and methods of production, the articles and methods may be better understood with reference to the following exemplary embodiments.
Electrodeposition of CeO?. CeO2 and doped CeO2 layers may be electrodeposited on a biaxially textured nickel-based substrate, e.g., to form a buffer layer as follows. In an exemplary embodiment, a CeO2 layer (undoped) may be prepared in a bath containing cerium salt dissolved in deionized water. In other exemplary embodiments, doped CeO2 layers may be prepared, e.g., using samarium (Sm), gadolinium (Gd), and zirconium (Zr) or other elements, especially rare earths, transition, lanthanides and actinides. For purposes of illustration, a Sm-doped CeO2 layer may be prepared in a bath containing cerium salt and samarium salt dissolved in deionized water. A Gd-doped CeO2 layer may be prepared in a bath containing cerium salt and gadolinium salt dissolved in deionized water. A Zr-doped CeO2 layer may be prepared from a bath containing cerium salt and zirconium salt dissolved in deionized water.
During exemplary production, the layers may be electrodeposited in a vertical cell in which the electrodes (both working and counter electrodes) are suspended vertically from the top of the cell. Electrodeposition of the layers on a substrate may be performed at room temperature (about 22 to 25 °C) with constant stirring. The substrate may be a nickel-based substrate, such as, Ni-W (3% by weight or 3 wt%). In an exemplary embodiment, the substrate may be a flat, 10 centimeter (cm) x 0.5 cm, Ni-W substrate, improved by an electropolishing technique. The electropolishing technique may include providing the substrate in a 5 vol% hydrazine hydrate solution at +0.6 V, where the Pt counter and Pt pseudo-reference electrode are shorted together. The electrodeposition precursors may be prepared at a commercially favorable constant current mode of about —2 volts (V), where the platinum (Pt) counter and Pt pseudo-reference electrodes are shorted together. The duration of electrodeposition may be less than 50 minutes, e.g., in the range of 3 to 20 minutes. A Princeton Applied Research potentiostat/galvanostat (Model 273A) with an IBM PC AT computer interface may be used to prepare the electrodeposition layers.
In an exemplary embodiment, the electrodeposited layers may be characterized by X-ray diffraction (XRD), in Θ/2Θ geometry, using CuK01 radiation (λ=1.5406 nm). Out- of-plane alignment may be determined from an omega scan on the (200) CeO2 reflection. In-plane alignment may be estimated from a pole figure and phi scans on the CeO2 (111) reflection. The Gaussian distribution may be fitted to the phi- and omega-scan data to estimate full width at half maximum (FWHM). Layer morphology may be observed by scanning electron micrographs (SEM). Electrodeposited layer roughness may also be estimated from Atomic Force Microscopy (AFM) scans.
Figure 2a is a representative XRD scan for annealed CeO2 and CeO2:Sm prepared on a Ni-W substrate. It is observed that only the c-axis-oriented (200) CeO2 reflection can be identified, but the intensity of Sm-doped layers is much higher due to better crystallinity and greater thickness. Figure 2b is a representative omega scan on the (200) reflection for the annealed CeO2 and CeO2:Sm prepared on a Ni-W substrate. It is observed that the dispersion along the c-axis of the undoped CeO2 and Sm-doped CeO2 grains are as low as 3.8° and 3.5°, respectively. The omega-scan value of CeO2 is better
than the 7.4° reading for the base Ni-W substrate. Figures 3a and 3b are representative pole-figure scans for the annealed CeO2 and CeO2: Sm prepared on a Ni-W substrate. The pole-figure scans show that CeO2 and CeO2--Sm are biaxially textured.
Figures 4a and 4b are representative phi scans of (a) the annealed CeO2 and CeO2:Sm, and (b) the Ni-W substrate. It is observed in Figure 4a that an average in-plane mosaic spread from the phi scan of the CeO2 layer is about 6.1°. The average in-plane mosaic spread from the phi scan of the CeO2:Sm layer is about 6.4°. It is observed in Figure 4b that an average in-plane mosaic spread from the phi-scan of the base Ni-W substrate is 7.6°. The improved values of omega and phi may be attributed to the relatively small grain size of the electrodeposited CeO2 and CeO2: Sm precursor layers, which also show better grain alignment after annealing. Figures 5a and 5b are AFM images of the CeO2 and CeO2: Sm layer. It is observed that the average layer roughness is about 3 run. Figures 6a-d are SEM images of the CeO2: Sm layer. It is observed that both layers are free from any cracks. In an exemplary embodiment, pulsed laser deposition (PLD) may be implemented to deposit layers of buffer materials on the substrate. PLD is a well known technique, wherein a laser is focused on a target including the buffer material to be deposited. The incident laser generates a plume of buffer material from the target surface. The substrate is heated and positioned in the path of this plume to deposit the buffer material in the plume on the substrate. An exemplary YBCO superconductor may be produced, e.g., by PLD of a YSZ layer, PLD of a CeO2 layer, and PLD of a YBCO layer over the electrodeposited CeO2 layer to illustrate Ni inter-diffusion from the Ni-W substrate.
Figure 7a shows an Atomic Emission Spectrometry (AES) analysis of a superconductor having the structure: YBCO/CeO/TSZ/ED-CeO^i- W. It is observed that Ni inter-diffusion is completely stopped at the first electrodeposited CeO2 layer. Figure 7b shows an AES analysis of a YBCO superconductor directly on an ED- CeO2/Ni-W substrate to qualify the simple buffer layer architecture. It is observed that Ni inter-diffusion is stopped, but Ni penetrates deep inside the CeO2 layer.
EIectrodeposition of Iridium. Iridium (Ir) has excellent oxidation and corrosion resistance. In addition, the lattice mismatch of cubic Ir (a=3.84 A) is very close to that of
CeO2 [a=5.411 A, a/(square root of 2) = 3.826 A] and Ni (a=3.524 A), making iridium a good buffer layer for use in YBCO high-temperature superconductors.
In exemplary embodiments, iridium layers may be electrodeposited on a biaxially textured nickel-based substrate to form a buffer layer as follows. The iridium layer may be electrodeposited using a bath containing only Ir salt at 650C. Again, a vertical cell may be implemented in which the electrodes (both working and counter) are suspended vertically from the top of the cell. The electrodeposition precursors may be prepared at about -1.2 V for 2 to 45 minutes on a Ni-W (3 wt%) substrate, where the Pt counter and Pt pseudo-reference electrodes are shorted together. To qualify the electrodeposited Ir buffer layer, a pulsed laser deposition (PLD)
CeO2AfSZZCeO2 structure and a simplified PLD YSZ/CeO2 structure may be deposited on top of the Ir-coated Ni-W substrates. The electrodeposited Ir/metal substrates are first heated to 8000C in 500 mTorr of the forming gas, and then a CeO2 seed layer is deposited in 180 mTorr of the forming gas. Subsequently, YSZ and CeO2 layers are deposited sequentially in 0.1 mTorr of oxygen.
The PLD system may be a standard PLD chamber (Neocera) and an excimer KrF laser (Lambda Physik, Compex 201, λ=248 run) operated at 260 mJ and 10 Hz. The laser beam may be focused onto a 3 x 1 cm2 spot on a target at a 45° angle, with a fluence of 2-3 J/cm2. The surface of YSZ (3 mole% Y2O3) and CeO2 targets may be cleaned in situ by exposure to 1000 laser shots prior to every deposition. The substrates may be mounted on the substrate holder-cum-heater, and the chamber evacuated to a base pressure of about 10"6 torr prior to deposition. The target-to-substrate distance is kept at about 8 cm, and layers of YSZ and CeO2 are deposited sequentially. The electrodeposited layers may be characterized by X-ray diffraction (XRD), in Θ/2Θ geometry, using CuKαl radiation (λ=1.5406 nm).
Figure 8 is a representative XRD diagram of a CYC/Ir buffer layer electrodeposited on a Ni-W substrate. The XRD diagram of CeO2/YSZ/CeO2/Ir/Ni-W shows the epitaxial (001) phase formation for each deposited layer. No NiO phase formation was observed on this type of buffer architecture, even though the layers were
annealed at 800°C. Out-of-plane omega values of the biaxially textured buffer layers were 6.5° and 8.7° for YSZ(200) and CeO2(200), respectively.
Figures 9a and 9b are representative pole-figure scans for (a) the CeO2 and (b) the YSZ layers prepared on a Ni-W substrate. It is observed that the CeO2 top layer and YSZ are cube-textured. Figures 10a and 10b are representative phi scans of (a) the CeO2 and (b) the YSZ of respective layers prepared on a Ni-W substrate. It is observed that the in-plane texture values (phi scan) of YSZ and CeO2 were 7.0° and 8.0°, respectively. These values are comparable to the Ni-W substrate (Δω=7.0° and Δφ=7.5°), indicating the good epitaxial nature of the CeO2A7-SZZCeO2ZIrZNi-W configuration. It is noted that an initial CeO2 layer is not needed to produce electrodeposited Ir on a Ni-based substrate. In an exemplary embodiment, the final buffer layer configuration may be CeO2ZYSZZIr on a Ni-W substrate. Results for these structures are comparable to the CYCZIr configuration, and indicate a cube texture.
Figure 11a and lib are atomic force microscopy (AFM) micrographs of (a) CeO2ZYSZZCeO2ZIrZNi-W and (b) CeO2ZYSZZIrZNi-W. The AFM micrographs show smooth, continuous, crack-free buffer architectures for both CeO2ZYSZZCeO2ZIrZNi-W and CeO2ZYSZZIrZNi-W. The average roughness is about 3 nm for the CYZIrZNi-W, and about 9 nm for the CYCZIrZNi-W.
EIectrodeposition of Ni. Electrodeposition of Ni may be performed using a bath containing 66g NiSO4^xH2O, 9g NiCl2^6H2O, and 7.6g boric acid dissolved in 200 mL of deionized water. Again, the layers may be deposited in a vertical cell in which the electrodes (both working and counter) are suspended vertically from the top of the cell at 650C and without stirring.
The electrodeposition precursors may be prepared by applying 0.4 mAZcm2 current density at 650C for 60 minutes, where the Pt counter and Pt pseudo-reference electrode are shorted together. The Ni-W substrate may be improved by an electro-polishing technique. Electropolishing of the Ni-W substrate may be done in 5 vol% hydrazine hydrate solution at -50 μAZcm2 (at a corresponding voltage of about +0.8 V) where the Pt counter and Pt pseudo-reference electrode are shorted together.
A Princeton Applied Research potentiostat/galvanostat Model 273 A with an IBM PC AT computer interface may be used to prepare electrodeposition layers. The thickness of the electrodeposition Ni layers is about 2.0 μm. The as-electrodeposited Ni layers are biaxially textured crystalline layers. The buffer structures are completed on these types of seed ED-Ni layers by PLD
CeO2Af SZ/CeO2. Specifically, the electrodeposited Ni/Ni-W (3%) layer may be annealed at 850°C in 1 torr forming gas. A CeO2 seed layer may be deposited at 8500C in 180 mtorr forming gas. The subsequent YSZ and CeO2 cap layers may be deposited at 8500C in 0.1 mtorr oxygen. The qualities of the ED-Ni layer may be assessed by depositing a PLD YBCO layer. Again, PLD deposition of 300-nm-thick YBCO may be performed using a RrF excimer laser system, operated at a fluence of 2-3 J/cm2, the substrate held at 78O0C under an oxygen partial pressure of 150 mtorr. After YBCO deposition, 0.5-μm-thick silver (Ag) contacts may be deposited by DC magnetron sputtering, and the samples annealed in flowing oxygen at 5000C for 90 min. Transport critical current (Jc) measurements may be performed at liquid nitrogen (~77 K) in varying applied magnetic fields using a standard 4-probe technique and the lμV/cm criterion.
Figures 12a-d are XRD Omega and Phi scans of (a and b) a Ni-W substrate, and (c and d) electrodeposited Ni on a Ni-W substrate. Full-width at half-maximum (FWHM) values of the ω scan (out-of-plane) and φ scan (in-plane) of the Ni-W substrate are (a) 6.0° and (b) 8.3°. Full-width at half-maximum (FWHM) values of the ω scan (out-of- plane) and φ scan (in-plane) of the electrodeposited Ni layer are (c) 7.1° and (d) 7.0°, which is comparable to the base Ni-W (3%) substrates and indicates good biaxial texturing. The relatively small grain size of the electrodeposited Ni layer is helpful for growing a higher-quality superconductor layer.
Figure 13a and 13b are representative XRD omega and Phi scans of (a) YBCO superconductor on ED-Ni/Ni-W, and (b) YBCO superconductor on ED-Ni/Ni-W. The XRD theta/2 theta scans show very good YBCO phase formation with some impurity-Ni (111) phase. Figure 14 is a plot of the critical current density versus field of a PLD YBCO/CYC/ED-Ni/Ni-W structure. It is observed that the critical current density at
varying magnetic fields for a YBCO layer grown on an ED-Ni-based buffer layer is about 1.8 MA/cm2 at 75.2K in a 600 Gauss magnetic field.
It is readily appreciated that applications of the technology described herein may include, but are not limited to, superconductors, semiconductors, ferroelectrics, pyroelectrics, magnetic, optics, sensors, semiconductor layers, and photovoltaic. In an exemplary application, high temperature superconductors may be produced by electrodepositing high temperature superconducting materials on the buffer layer to produce, e.g., Y-Ba2Cu3Ox (YBCO), Bi-Sr-Ca- Cu-O (BSCCO), Tl-Ba-Ca-Cu-O (TBCCO), Pb-Ba-Sr-Ca-Cu-O (PBSCCO), Tl-Sr-Ba-Ca-Cu-O (TSBCCO), Tl-Pb-Sr-Ba-Ca-Cu-O (TPSBCCO), Hg-Ba-Ca-Cu-O (HBCCO). The superconducting material may be deposited epitaxially, such that the superconducting material has the same crystalline orientation as the buffer layer. In other exemplary applications, crystalline silicon may be grown on the substrate to produce solar cells. Still other applications are also contemplated and will become readily apparent to those having ordinary skill in the art after becoming familiar with the teachings herein.
Examples
The following examples are provided to further characterize the methods and articles described herein. These examples are illustrative and not intended to be limiting. Electrodeposited CeO7. In this example, biaxially textured CeO2 was prepared on Ni and Ni-W substrates. Specifically, 0.5g of cerium bromide was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.26 mA/cm2 current density at room temperature (about 22°C) for 10 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 9800C in a mixture of Ar gas (95%) and a 5% forming gas [H2 (10%)/N2]. Electrodeposited Samarium doped CeO?. In this example, biaxially textured
CeO2: Sm was prepared on Ni and Ni-W substrates. Specifically, 0.5g cerium bromide and O.Olg Samarium bromine was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.26 mA/cm2 current density at room temperature (about 22°C) for 15 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 9800C in a mixture of Ar gas (95%) and a 5% forming gas [H2 (10%)/N2].
Electrodeposited CeO?;Gd. In this example, biaxially textured CeO2:Gd was prepared on a Ni-W substrate. Specifically, 0.5g cerium bromide and 0.02g gadolinium bromine was dissolved in 200 niL of water. The layer was electrodeposited by applying 0.3 niA/cm2 current density at room temperature (about 22°C) for 10 minutes. The electrodeposited layer was annealed at 10200C in a mixture of Ar gas provided at 60 pounds per square inch (psi) and a forming gas [H2 (10%)/N2] provided at 2.5 psi for 2 hours.
Electrodeposited CeO?:Zr. In this example, biaxially textured CeO2:Zr was prepared on a Ni-W substrate. Specifically, 0.5g cerium bromide and 0.18g zirconium bromine was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.4 niA/cm2 current density at room temperature (about 22°C) for 5 minutes. The electrodeposited layer was annealed at 10200C in a mixture of Ar gas provided at 60 psi and forming gas [H2 (10%)/N2] provided at 2.5 psi for 2 hours.
Electrodeposited La^O^ In this example, biaxially textured La2O3 was prepared on a Ni-W substrate. Specifically, O.lg lanthanum bromide was dissolved in a mixture of 100 mL of water (20%) and isopropyl alcohol (80%). The layer was electrodeposited by applying 0.4 niA/cm2 current density at room temperature (about 22°C) for 10 minutes. The electrodeposited layer was annealed at 10300C in a mixture of Ar gas (95%) and 5% forming gas [H2 (10%)/N2]. Electrodeposited Iridium (Ir). In this example, biaxially textured iridium was prepared on a Ni-W substrate. Specifically, 0.5g iridium bromide was dissolved in 100 mL of water. The layer was electrodeposited by applying 1 mA/cm2 current density at 65° C for 15 minutes.
Electrodeposited Ni-Ir. In this example, biaxially textured Ni-Ir was prepared on a Ni-W substrate. Specifically, 66g NiSO4, 9g NiCl2, 7.6g boric acid, and 0.5g IrBr3 was dissolved in 250 mL of water. The layer was electrodeposited by applying 0.4 niA/cm2 current density at 650C for 15 minutes.
Electrodeposited Ni. In this example, biaxially textured Ni was prepared on a Ni-W substrate. Specifically, 66g NiSO4, 9g NiCl2, and 7.6g boric acid was dissolved
in 250 mL of water. The layer was electrodeposited by applying 0.4 mA/cm2 current density at 65°C for 60 minutes.
In this example, biaxially textured YSZ was prepared on a Ni-W substrate. Specifically, 2.1g zirconium bromide and 0.05g yttrium bromine was dissolved in 100 mL of water. The layer was electrodeposited by applying 3 mA/cm2 current density at room temperature (about
22°C) for 10 minutes.
Electrodeposited Y7O^. In this example, biaxially textured Y2O3 was prepared on a Ni-W substrate. Specifically, 0.5g yttrium bromide was dissolved in a mixture of 100 mL of water (30%) and isopropyl alcohol (70%). The layer was electrodeposited by applying 0.8 mA/cm2 current density at room temperature (about 22° C) for 15 minutes. The electrodeposited layer was annealed at 9800C in a mixture of Ar gas (95%) and a 5% forming gas [H2 (10%)/N2].
In another example, biaxially textured Y2O3 was prepared on a Ni-W as follows: 0.5g yttrium bromide was dissolved in 200 mL of isopropyl alcohol (isopropanol). The layer was electrodeposited by applying 0.1 mA/cm2 current density at room temperature (about 22°C) for 30 minutes. The solution was stirred during deposition. The electrodeposited layer was annealed at 11000C in a mixture of Ar gas provided at 20 psi and a forming gas [H2 (10%)/N2] provided at 2.5 psi. In yet another example, biaxially textured Y2O3 was prepared on a Ni-W substrate as follows: 1.Og yttrium bromide was dissolved in 200 mL of water. The layer was electrodeposited by applying 0.8 mA/cm2 current density at room temperature (about 22°C) for 20 minutes. The solution is stirred during deposition. The electrodeposited layer was annealed at 11000C in a mixture of Ar gas provided at 20 psi and a forming gas [H2 (10%)/N2] provided at 2.5 psi.
Electrodeposited La-Mn-Q. In this example, biaxially textured La-Mn-O was prepared on a Ni-W substrate. Specifically, 0.7g lanthanum bromide and 0.6g Manganese bromide were dissolved in 200 mL of water. The layer was electrodeposited by applying 0.8 mA/cm2 current density at room temperature (about 22°C) for 15 minutes. The electrodeposited layer was annealed at 9900C in a mixture of Ar gas (95%) and a 5% forming gas [H2 (10%)/N2].
Electrodeposited CeO? on electrodeposited Y2O^ZNi-W. In this example, biaxially textured CeO2 was prepared on a Y2O3/Ni-W substrate. First, 0.5g yttrium bromide was dissolved in 200 mL of isopropanol. The Y2O3 layer was electrodeposited by applying 0.1 mA/cm current density at room temperature (about 22°C) for 30 minutes on a Ni-W substrate. The solution was stirred during deposition to form the Y2O3/Ni-W substrate.
Then electrodeposited CeO2 was electrodeposited on the Y2O3/Ni-W substrate. Specifically, 0.5g cerium bromide and 0.0 Ig samarium bromine was dissolved in 200 mL of water. The CeO2 layer was electrodeposited by applying 0.26 mA/cm2 current density. The electrodeposited layer was annealed at 9900C in a mixture of Ar gas (95%) and a 5% forming gas [H2 (10%)/N2].
It is noted that the examples discussed above are provided for purposes of illustration and are not intended to be limiting. Still other embodiments and modifications are also contemplated. While a number of exemplary aspects and embodiments have been discussed above, those of skill in the art will recognize certain modifications, permutations, additions and sub combinations thereof. It is therefore intended that the following appended claims and claims hereafter introduced are interpreted to include all such modifications, permutations, additions and sub-combinations as are within their true spirit and scope.
Claims
1. A method of producing at least one biaxially textured layer on a substrate, comprising electrodepositing on the substrate a precursor material selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof.
2. The method of claim 1, wherein the precursor material is selected from the group consisting of CeO2, doped CeO2, La2O3, Ir, Ni-Ir, Ni, YSZ, Y2O3, and La-Mn-O.
3. The method of claim 1 , wherein the substrate is biaxially textured.
4. The method of claim 1 , wherein the substrate comprises Ni.
5. The method of claim 1 , wherein the substrate comprises Ni-W.
6. The method of claim 1 , wherein the precursor material is CeO2.
7. The method of claim 1, wherein the precursor material is a doped CeO2.
8. The method of claim 1, wherein the CeO2 is doped with Sm, Gd, or Zr.
9. The method of claim 1, further comprising electrodepositing CeO2 on electrodeposited Y2O3.
10. The method of claim 1, wherein electrodepositing is at a current density in the range of about 0.05 to 25 mA/cm2.
11. The method of claim 1, wherein electrodepositing is during stirring of a bath containing the precursor material.
12. The method of claim 1, wherein electrodepositing is in the range of about 200C to 1000C.
13. The method of claim 1, wherein electrodepositing is at about room temperature.
14. The method of claim 1, wherein electrodepositing is for about 1 to 30 minutes.
15. The method of claim 1, further including annealing the biaxially textured layer at about 700 to 12000C.
16. The method of claim 1, further including annealing the biaxially textured layer in a gas mixture.
17. The method of claim 1 , further including annealing the biaxially textured layer.
18. A superconductor having a biaxially textured layer produced according to the process of claim 1.
19. A biaxially textured article produced according to the process of claim 1.
20. The biaxially textured article of claim 19, wherein the at least one biaxially textured layer is a buffer layer.
21. The biaxially textured article of claim 19, wherein the at least one biaxially textured layer is deposited over a biaxially textured buffer layer.
22. A method of producing a superconducting material having at least one biaxially textured layer, comprising: selecting a precursor material from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof; and electrodepositing the selected precursor material on a biaxially textured substrate.
23. The method of claim 22, further comprising constantly stirring a bath with the precursor material during the step of electrodepositing.
24. The method of claim 22, further comprising thermally annealing the electrodeposited precursor material.
25. The method of claim 22, wherein the biaxially textured substrate is Ni-based.
26. The method of claim 22, wherein the precursor material is selected from the group consisting of CeO2, doped CeO2, La2O3, Ir, Ni-Ir, Ni, YSZ, Y2O3, and La-Mn-O.
27. A biaxially textured material, comprising: a biaxially textured base material; at least one biaxially textured layer selected from the group consisting of rare earths, transition metals, actinides, lanthanides, and oxides thereof, the at least one biaxially textured layer formed by electrodeposition on the biaxially textured base material.
28. The biaxially textured material of claim 27, wherein the at least one biaxially textured layer is a buffer layer.
29. The biaxially textured material of claim 27, wherein the at least one biaxially textured layer is electrodeposited over a buffer layer.
30. The biaxially textured material of claim 27, wherein the biaxially textured base material is Ni-based.
31. The biaxially textured material of claim 27, wherein the at least one biaxially textured layer is selected from the group consisting of CeO2, doped CeO2, La2O3, Ir, Ni-Ir, Ni, YSZ, Y2O3, and La-Mn-O.
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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PCT/US2005/027263 WO2007015692A1 (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on a substrate |
US11/817,452 US8586506B2 (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on a substrate |
JP2008524945A JP2009503269A (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on substrates |
EP05810135A EP1912785B1 (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on a substrate |
DE602005026462T DE602005026462D1 (en) | 2005-08-01 | 2005-08-01 | GALVANIC COATING OF BIAXIAL STRUCTURED LAYERS ON A SUBSTRATE |
US14/055,048 US20140100112A1 (en) | 2005-08-01 | 2013-10-16 | Electrodeposition of biaxially textured layers on a substrate |
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PCT/US2005/027263 WO2007015692A1 (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on a substrate |
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US11/817,452 A-371-Of-International US8586506B2 (en) | 2005-08-01 | 2005-08-01 | Electrodeposition of biaxially textured layers on a substrate |
US14/055,048 Division US20140100112A1 (en) | 2005-08-01 | 2013-10-16 | Electrodeposition of biaxially textured layers on a substrate |
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EP (1) | EP1912785B1 (en) |
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Cited By (4)
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JP2008303404A (en) * | 2007-06-05 | 2008-12-18 | Kyushu Electric Power Co Inc | Metal plated composite base material |
JP2010123516A (en) * | 2008-11-21 | 2010-06-03 | Fujikura Ltd | Method of manufacturing substrate for oxide superconductor, method of manufacturing oxide superconductor, and device for forming cap layer for oxide superconductor |
WO2011012818A1 (en) * | 2009-07-30 | 2011-02-03 | Snecma | Part comprising a substrate supporting a ceramic coating layer |
WO2011012819A1 (en) * | 2009-07-30 | 2011-02-03 | Snecma | Method for manufacturing a thermal barrier |
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US7906229B2 (en) * | 2007-03-08 | 2011-03-15 | Amit Goyal | Semiconductor-based, large-area, flexible, electronic devices |
US8993092B2 (en) | 2011-02-18 | 2015-03-31 | Ut-Battelle, Llc | Polycrystalline ferroelectric or multiferroic oxide articles on biaxially textured substrates and methods for making same |
ITVR20130200A1 (en) * | 2013-08-13 | 2015-02-14 | Sofcpower S P A | METHOD OF DEPOSITION OF A MATERIAL LAYER ON A METAL SUPPORT FOR FUEL CELLS OR CELLS FOR ELECTROLYSIS |
WO2015033808A1 (en) | 2013-09-04 | 2015-03-12 | 東洋鋼鈑株式会社 | Method for depositing oxide layer, and layered substrate for epitaxial growth and process for producing same |
CN108779568B (en) * | 2016-03-11 | 2021-06-01 | 应用材料公司 | Method for electrochemically forming yttria on semiconductor processing equipment |
KR102453489B1 (en) * | 2018-04-10 | 2022-10-11 | 한국전기연구원 | High-temperature superconducting wire with superconducting layer laminated and method for manufacturing the same |
KR102218695B1 (en) * | 2018-09-17 | 2021-02-19 | 동우 화인켐 주식회사 | Touch sensor and method of manufacturing the same |
US11306407B2 (en) * | 2018-12-21 | 2022-04-19 | The Board Of Trustees Of The University Of Alabama | Methods for electrodeposition |
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- 2005-08-01 EP EP05810135A patent/EP1912785B1/en not_active Expired - Fee Related
- 2005-08-01 WO PCT/US2005/027263 patent/WO2007015692A1/en active Application Filing
- 2005-08-01 JP JP2008524945A patent/JP2009503269A/en active Pending
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JP2008303404A (en) * | 2007-06-05 | 2008-12-18 | Kyushu Electric Power Co Inc | Metal plated composite base material |
JP2010123516A (en) * | 2008-11-21 | 2010-06-03 | Fujikura Ltd | Method of manufacturing substrate for oxide superconductor, method of manufacturing oxide superconductor, and device for forming cap layer for oxide superconductor |
WO2011012818A1 (en) * | 2009-07-30 | 2011-02-03 | Snecma | Part comprising a substrate supporting a ceramic coating layer |
WO2011012819A1 (en) * | 2009-07-30 | 2011-02-03 | Snecma | Method for manufacturing a thermal barrier |
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US9260791B2 (en) | 2009-07-30 | 2016-02-16 | Snecma | Method of fabricating a thermal barrier |
Also Published As
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US20140100112A1 (en) | 2014-04-10 |
US20100167084A1 (en) | 2010-07-01 |
EP1912785B1 (en) | 2011-02-16 |
US8586506B2 (en) | 2013-11-19 |
JP2009503269A (en) | 2009-01-29 |
EP1912785A1 (en) | 2008-04-23 |
DE602005026462D1 (en) | 2011-03-31 |
EP1912785A4 (en) | 2009-02-18 |
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