WO2006029587A1 - Verfahren zur herstellung dünner, dichter keramikschichten - Google Patents

Verfahren zur herstellung dünner, dichter keramikschichten Download PDF

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Publication number
WO2006029587A1
WO2006029587A1 PCT/DE2005/001380 DE2005001380W WO2006029587A1 WO 2006029587 A1 WO2006029587 A1 WO 2006029587A1 DE 2005001380 W DE2005001380 W DE 2005001380W WO 2006029587 A1 WO2006029587 A1 WO 2006029587A1
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
ceramic
layer
kelvin
less
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DE2005/001380
Other languages
German (de)
English (en)
French (fr)
Inventor
Robert Vassen
Dag Hathiramani
Detlev STÖVER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Priority to US11/662,787 priority Critical patent/US20070259126A1/en
Priority to EP05773241A priority patent/EP1789600B1/de
Priority to ES05773241T priority patent/ES2387891T3/es
Priority to JP2007530578A priority patent/JP4738414B2/ja
Publication of WO2006029587A1 publication Critical patent/WO2006029587A1/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/123—Spraying molten metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
    • H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to a method for the production of ceramic layers, in particular of ceramic layers with egg ner thickness below 100 microns, which are configured gas-tight.
  • spraying techniques in particular atmospheric plasma spraying, have proven to be very suitable.
  • a plasma is a hot gas in which, due to the high temperature, the neutral particles dissociate and ionize.
  • charged particles such as electrons and ions are also in a plasma.
  • an arc is interposed in the so-called plasma burner by high-frequency ignition
  • the process parameters to be set are, in particular, the flow rate and the composition for the plasma gas and the powder carrier gas, current, voltage, powder quantity and particle velocity and temperature, as well as substrate temperature and also spray intervals and relative velocity between plasma torch and substrate.
  • Atmospherically plasma-sprayed ceramic layers usually have a multitude of pore-like structures that can be divided into two different types: cracks, as well as coarse, usually globular pores.
  • segmentation cracks and microcracks In the case of the cracks, in turn, one can distinguish so-called segmentation cracks and microcracks.
  • the former run parallel to the coating direction through several spray lamellae, and sometimes even through the entire layer.
  • the width of the crack opening is typically well above one micrometer.
  • the microcracks are located between the lamellae (interlamellar) or in the lamellae (intralamellar) and have significantly lower crack opening widths typically below one micron.
  • the microcracks are networked mitein ⁇ other and have a gas permeability of the layer result. Likewise, the gas permeability is promoted by the globular pores and segmentation cracks, especially those running through the entire layer.
  • the object of the invention is to provide a method for the production of thin and simultaneously gas-tight ceramic layers on a substrate which, in particular without additional thermal aftertreatment, have a leakage rate of less than 10 -1 mbar L / (cm 2 s).
  • the object of the invention is achieved by an atmospheric plasma spraying method in which a number of special parameters are set during the execution of the method.
  • the combination of these parameters has the effect that a thin ceramic layer, in particular one with a layer thickness of less than 100 ⁇ m, is deposited on a substrate which is advantageously gas-tight and has a leak rate below 10 -1 mbar L / (cm 2 s) ,
  • the abovementioned process parameters can be realized in part by the geometry of the plasma torch for substrate surface.
  • the setting of the parameters in accordance with items 4 and 5 can generally be advantageously realized by using not too large spray distances, that is typically below 150 mm.
  • the choice of spray additive in the form of fine, but still flowable particles with d 50 values makes it easier below 50 ⁇ m, advantageously even below 30 ⁇ m, the setting of a high density in the layer to be deposited.
  • the robot speed and the powder delivery rate are chosen so that a correspondingly dense layer with a layer thickness of less than 100 ⁇ m is produced with a single transition.
  • Favorable robot speeds lie between 50 and 500 mm / s.
  • Suitable materials for the abovementioned process are, in particular, ceramic materials which have a melting point, such as, for example, zirconium oxide, also with stabilizer additives, perovskites, pyrochlors, aluminates, alumina, spinels, boron carbides, titanium carbides and the like. a. exposed.
  • the method according to the invention can be easily applied to the production of various layers, in particular for dense electrolyte layers for the high-temperature fuel cell, membranes for gas separation technologies and for oxidation or corrosion protection layers
  • Porous, provided with an anode substrates are preheated to temperatures of about 500 0 C with the plasma torch.
  • plasma torch can z.
  • the TRIPLEX II - or the F4 - Burners from Sulzer Metco are used. Performance and process gas flows are selected to be high enough to produce high process gas velocities and temperatures.
  • the powder used is a molten, broken, fully yttrium-stabilized zirconium oxide (YSZ) with an ad 50 value of 20 ⁇ m.
  • the particle velocities are on impact with the substrate at over 300 m / s, the temperatures above 3000 0 C.
  • the spray distance is 90 mm.
  • the Substrattempe ⁇ temperatures during the coating reached about 800 0 C.
  • the robot speed and the powder feed rate are selected so that with a transition a thick, about 90 microns di ⁇ blocks YSZ layer.
  • the robot speed set for this is 150 mm / s.
  • the YSZ layer thus prepared has a regularly Leck ⁇ rate of less than 10 "2 mbar L / (cm 2 s) on.
  • the FIGURE shows the layer structure of the aforementioned embodiment with a porous substrate, an intermediate layer arranged thereon and a dense YSZ electrolyte layer arranged thereon, which was applied by the APS process according to the invention.
  • Composites are provided with a mullite layer, which still has cracks.
  • This layer is coated with another, gas-tight layer of La 2 Hf 2 O 7 according to the invention set forth here in order to prevent attack of corrosive or oxidizing gas atmospheres both on the substrate and on the mullite layer.
  • a ceramic interlayer may be included which suppresses reactions between mullite and La 2 Hf 2 O 7 .
  • spray-dried powder with a d 50 value of about 30 ⁇ m is used.
  • the burner In the preheating of the substrate with the burner (TRIPLEX II, F4, or more powerful burners variants) is preheated to 400 0 C.
  • the particle velocity is about 210 m / s at temperatures around 2900 0 C.
  • the achieved layer thickness is about 35 microns.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Laminated Bodies (AREA)
PCT/DE2005/001380 2004-09-13 2005-08-04 Verfahren zur herstellung dünner, dichter keramikschichten Ceased WO2006029587A1 (de)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US11/662,787 US20070259126A1 (en) 2004-09-13 2005-08-04 Method for the Production of Thin Dense Ceramic Layers
EP05773241A EP1789600B1 (de) 2004-09-13 2005-08-04 Verfahren zur herstellung dünner, dichter keramikschichten
ES05773241T ES2387891T3 (es) 2004-09-13 2005-08-04 Procedimiento para la fabricación de capas cerámicas finas y compactas
JP2007530578A JP4738414B2 (ja) 2004-09-13 2005-08-04 薄く高密度のセラミック層の製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004044597.4 2004-09-13
DE102004044597A DE102004044597B3 (de) 2004-09-13 2004-09-13 Verfahren zur Herstellung dünner, dichter Keramikschichten

Publications (1)

Publication Number Publication Date
WO2006029587A1 true WO2006029587A1 (de) 2006-03-23

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Family Applications (1)

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PCT/DE2005/001380 Ceased WO2006029587A1 (de) 2004-09-13 2005-08-04 Verfahren zur herstellung dünner, dichter keramikschichten

Country Status (6)

Country Link
US (1) US20070259126A1 (enExample)
EP (1) EP1789600B1 (enExample)
JP (1) JP4738414B2 (enExample)
DE (1) DE102004044597B3 (enExample)
ES (1) ES2387891T3 (enExample)
WO (1) WO2006029587A1 (enExample)

Cited By (2)

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Publication number Priority date Publication date Assignee Title
WO2016198730A1 (en) * 2015-06-12 2016-12-15 Elcogen Oy Protection arrangement for structure plates of solid oxide cells and method of forming said protection arrangement
DE102020126082A1 (de) 2020-10-06 2022-04-07 Forschungszentrum Jülich GmbH Verfahren zur Herstellung einer Beschichtung sowie Beschichtung

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DE102008007870A1 (de) * 2008-02-06 2009-08-13 Forschungszentrum Jülich GmbH Wärmedämmschichtsystem sowie Verfahren zu seiner Herstellung
US9725797B2 (en) 2008-04-30 2017-08-08 United Technologies Corporation Process for forming an improved durability thick ceramic coating
DE102008026101B4 (de) * 2008-05-30 2010-02-18 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Thermisch gespritzte Al2O3-Schichten mit einem hohen Korundgehalt ohne eigenschaftsmindernde Zusätze und Verfahren zu ihrer Herstellung
US20110048017A1 (en) * 2009-08-27 2011-03-03 General Electric Company Method of depositing protective coatings on turbine combustion components
DE102013017888A1 (de) 2013-10-28 2015-04-30 Robert Brockmann Verfahren zur Verheilung der Passivschicht eines Bauteils von Aluminium zur Wiedererlangung der Gasdichtheit
US10196728B2 (en) * 2014-05-16 2019-02-05 Applied Materials, Inc. Plasma spray coating design using phase and stress control
JP6590686B2 (ja) * 2014-12-24 2019-10-16 トーカロ株式会社 絶縁軸受、並びに軸受のコーティング方法
KR102026578B1 (ko) * 2015-09-14 2019-09-27 엘코겐 오와이 고체 산화물 전지들의 구조 플레이트들을 위한 보호 장치 및 상기 보호 장치를 형성하는 방법
US11404710B2 (en) 2018-12-17 2022-08-02 Cummins Enterprise Llc Assembled portion of a solid oxide fuel cell and methods for inspecting the same

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016198730A1 (en) * 2015-06-12 2016-12-15 Elcogen Oy Protection arrangement for structure plates of solid oxide cells and method of forming said protection arrangement
US10770735B2 (en) 2015-06-12 2020-09-08 Elcogen Oy Protection arrangement and method of solid oxide cells
DE102020126082A1 (de) 2020-10-06 2022-04-07 Forschungszentrum Jülich GmbH Verfahren zur Herstellung einer Beschichtung sowie Beschichtung
WO2022073697A1 (de) 2020-10-06 2022-04-14 Forschungszentrum Jülich GmbH Verfahren zur herstellung einer beschichtung sowie beschichtung

Also Published As

Publication number Publication date
DE102004044597B3 (de) 2006-02-02
US20070259126A1 (en) 2007-11-08
EP1789600A1 (de) 2007-05-30
EP1789600B1 (de) 2012-05-30
ES2387891T3 (es) 2012-10-03
JP4738414B2 (ja) 2011-08-03
JP2008512566A (ja) 2008-04-24

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