# US 2013/0153408 A1 · Method for producing cubic zirconia layers > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2013/0153408 A1 - Document ID: US20130153408A1 - Status: Published application - Kind: A1 - Application number: 13/497,283 - Filed: 2010-09-24 - Published: 2013-06-20 - Earliest claimed: 2009-09-25 - Assignees: Oerlikon Trading AG, Truebbach - Inventors: Jürgen Ramm; Beno Widrig - Web page: https://patentgrep.com/patent/US20130153408A1 ## CPC - C23C 14/24: Vacuum evaporation - C23C 14/0021: {Reactive sputtering or evaporation} - C23C 14/0676: {Oxynitrides} - C23C 14/083: {of refractory metals or yttrium} - C23C 14/325: {Electric arc evaporation} - C23C 14/0036: {Reactive sputtering} - C23C 14/0042: {Controlling partial pressure or flow rate of reactive or inert gases with feedback of measurements} - C23C 14/3485: {using pulsed power to the target} - Y02E 60/50: Fuel cells - Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product - C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION - Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS ## Abstract In order to produce zirconia-based layers on a deposition substrate, wherein reactive spark deposition using pulsed spark current and/or the application of a magnetic field that is perpendicular to the spark target are employed, a mixed target comprising elemental zircon and at least one stabilizer is used, or a zirconium target comprising elemental zirconium is used, wherein in addition to oxygen, nitrogen is used as the reactive gas. As an alternative, combined with the use of the mixed target, nitrogen can also be used as the reactive gas in addition to oxygen. ## Claims ### Claim 1 A method for producing a zirconia-based layer on a deposition substrate by using reactive spark evaporation using pulsed spark current and/or applying a magnetic field that is perpendicular to the spark target, characterized in that a mixed target comprising elemental zirconium and at least one stabilizer is used. ### Claim 2 (depends on 1) The method according to claim 1, characterized in that the layer is produced in a cubic and/or tetragonal crystal structure. ### Claim 3 (depends on 1) The method according to claim 1, characterized in that an oxygen partial pressure is chosen to be greater than 0.1 Pa. ### Claim 4 (depends on 1) The method according to claim 1, characterized in that the concentration ratio of zirconia and stabilizer of the layer is essentially given by the concentration ratio of elemental zirconium and stabilizer of the mixed target. ### Claim 5 (depends on 2) The method according to claim 2, characterized in that by selecting the concentration of the stabilizers in the mixed target, the cubic and/or tetragonal crystal structure is achieved. ### Claim 6 (depends on 3) The method according to claim 3, characterized in that an oxygen partial pressure, which is at least essentially a free setting parameter in terms of achieving a cubic and/or tetragonal crystal structure, is used for determining a layer morphology. ### Claim 7 (depends on 1) The method according to claim 1, characterized in that a reactive gas, in addition to oxygen, includes nitrogen. ### Claim 8 A method for producing a zirconia-based layer on a deposition substrate, wherein reactive spark deposition using pulsed spark current and/or the application of a magnetic field that is perpendicular to the spark target are employed, characterized in that a zirconium target comprising elemental zirconium is used and wherein in addition to oxygen, nitrogen is used as a reactive gas. ### Claim 9 (depends on 8) The method according to claim 8, characterized in that the layer is produced in a cubic and/or tetragonal crystal structure. ### Claim 10 (depends on 8) The method according to claim 8, characterized in that by setting pressure ratios during the spark evaporation process a layer is generated containing zircon, oxygen and nitrogen, with cubic and/or tetragonal crystal structure. ### Claim 11 (depends on 8) The method according to claim 8, characterized in that the oxygen proportion is set through a gas flow control device whilst the proportion of nitrogen is chosen according to a total pressure control device. ### Claim 12 (depends on 8) The method according to claim 8, characterized in that the zirconia-based layer is deposited as a pure ZrO2 layer in a cubic crystal structure on a cubic crystallized layer containing zircon, nitrogen and oxygen. ### Claim 13 (depends on 1, 8) The method according to claim 1 or 8 for the production of a layer as a layer in a layer stack. ### Claim 14 (depends on 1, 8) The method according to claim 1 or 8, characterized in that the layer is produced as multi-layer coating by varying the oxygen/nitrogen content. ### Claim 15 (depends on 1, 8) The method according to claim 1 or 8, characterized in that the deposition of the layer occurs at a substrate temperature between 200° C. and 700° C. ### Claim 16 (depends on 1, 8) Method The method according to claim 1 or 8, characterized in that the forming of the cubic or tetragonal phase occurs while not in the thermal state of equilibrium. ### Claim 17 (depends on 1, 8) The method according to claim 1 or 8, characterized in that oxides of other metals than zirconium are integrated into the layer material. ### Claim 18 (depends on 1, 8) The method according to claim 1 or 8, wherein the deposition substrate has a metallic surface, characterized in that a supporting layer is deposited onto the metallic surface, and the zirconia-based layer is deposited on the supporting layer. ### Claim 19 (depends on 1, 8) The method according to claim 1 or 8, characterized in that no working gas is used. ### Claim 20 (depends on 12) Use of the method according to claim 12 for the production of a layer that can revert to the monoclinic phase. ### Claim 21 (depends on 1, 8) Use of the method according to claim 1 or 8 for the production of a solid electrolyte layer in a fuel cell. ### Claim 22 (depends on 1, 6, 8) The method according to claim 1, 6 or 8, wherein at least one of the following characteristics applies: the stabilizer is freely chosen; layer composition, phase composition and layer morphology are set at least essentially independently from one another by means of the adjustment of parameters of a vaporization process; the layer morphology can be adjusted from glass-like to columnar; the solid electrolyte layer is produced without stabilizer; the layer is produced with a gradient of the layer material composition in the direction of its thickness dimension, wherein the morphology and phase can be chosen freely. ### Claim 23 (depends on 1, 8) Use of the method according to claim 1 or 8 for a production of the layer as growth substrate for an YSZ. ### Claim 24 (depends on 1, 8) Use of the method according to claim 1 or 8 for increasing the ion transport along grain boundaries. ### Claim 25 An anode for a spark evaporation source comprising: an anode body with an anode surface, a heating coil along the anode surface, insulated electrically from the anode body, connections, insulated electrically from the anode body, for the heating coil. ### Claim 26 (depends on 25) The anode according to claim 25, characterized in that the anode body is formed of sheet material. ### Claim 27 (depends on 25) A method for operating a spark evaporation installation with an anode according to claims 25, characterized in that the anode surface is subjected to a temperature change caused by means of activation/deactivation of the heating coil in order to at least partially clean it from an interference coating, such that the anode surface is distorted and the interference coating spalls. ### Claim 28 (depends on 27) The method according to claim 27, characterized in that with the heating coil, a substrate to be coated by spark evaporation is also heated.