WO2004109821A2 - Reactive deposition for electrochemical cell production - Google Patents

Reactive deposition for electrochemical cell production Download PDF

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Publication number
WO2004109821A2
WO2004109821A2 PCT/US2004/017793 US2004017793W WO2004109821A2 WO 2004109821 A2 WO2004109821 A2 WO 2004109821A2 US 2004017793 W US2004017793 W US 2004017793W WO 2004109821 A2 WO2004109821 A2 WO 2004109821A2
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WO
WIPO (PCT)
Prior art keywords
deposition
particles
flow
coating
reactant
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/US2004/017793
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English (en)
French (fr)
Other versions
WO2004109821A3 (en
Inventor
Craig R. Horne
William E. Mcgovern
Robert B. Lynch
Ronald J. Mosso
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Nanogram Corp
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Nanogram Corp
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Publication date
Application filed by Nanogram Corp filed Critical Nanogram Corp
Priority to JP2006515207A priority Critical patent/JP2006527463A/ja
Priority to EP04754404A priority patent/EP1644552A4/en
Publication of WO2004109821A2 publication Critical patent/WO2004109821A2/en
Publication of WO2004109821A3 publication Critical patent/WO2004109821A3/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/405—Oxides of refractory metals or yttrium
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/48—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation
    • C23C16/483—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating by irradiation, e.g. photolysis, radiolysis, particle radiation using coherent light, UV to IR, e.g. lasers
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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    • C23C18/06—Coating on selected surface areas, e.g. using masks
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    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
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    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
    • C23C18/143—Radiation by light, e.g. photolysis or pyrolysis
    • 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
    • C23C24/00—Coating starting from inorganic powder
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    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/13—Single electrolytic cells with circulation of an electrolyte
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/8605—Porous electrodes
    • H01M4/8621—Porous electrodes containing only metallic or ceramic material, e.g. made by sintering or sputtering
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • H01M4/8885—Sintering or firing
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    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9041—Metals or alloys
    • H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9066—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of metal-ceramic composites or mixtures, e.g. cermets
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/02—Details
    • H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
    • H01M8/0273—Sealing or supporting means around electrodes, matrices or membranes with sealing or supporting means in the form of a frame
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    • 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
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    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
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Definitions

  • Fig. 8 is a schematic diagram of a light reactive deposition apparatus in which a particle coating is applied to a subsfrate within the particle production chamber.
  • Fig. 9 is a perspective of a reactant nozzle delivering reactants to a reaction zone positioned near a subsfrate.
  • amorphous particles can be consolidated to form a glass material, and crystalline particles can be consolidated to form a crystalline material.
  • appropriate heating and quenching rates can be used to consolidate an amorphous material into a crystalline layer, either single crystalline or polycrystalline, (generally slow quenching rates) and a crystalline powder into a glass layer (generally a rapid quench).
  • the electrodes have a non-planar stracture.
  • a corrugated electrode stracture is described further below.
  • the electrodes can be formed on a rod with an inner electrode and an outer concentric electrolyte.
  • the further outer electrode can be similarly concentric or it can have another shape with the rod embedded within the outer electrode.
  • a ceramic elecfrolyte layer and/or an electrode layer can be deposited onto a rod using a rod shaped substrate and rotating the rod within the reactive flow.
  • Other specific processing approaches for particular fuel cell applications are described further below.
  • the plurality of aerosols can be introduced into a common gas flow for delivery into the reaction chamber through a common nozzle.
  • a plurality of reactant inlets can be used for the separate delivery of aerosol and/or vapor reactants into the reaction chamber such that the reactants mix within the reaction chamber prior to entry into the reaction zone.
  • vapor/gas reactants generally can be supplied at higher purity than is readily available at low cost for aerosol delivered compositions.
  • the powder coatings are formed by light reactive deposition, hi light reactive deposition, a highly uniform flow of product particles is formed that are directed toward a substrate to be coated.
  • the resulting particle coating can be formed into desired components of an electrochemical cell.
  • the rate of production and/or deposition of the particles can be varied substantially, depending on a number of factors (e.g., the starting materials being utilized, the desired reaction product, the reaction conditions, the deposition efficiency, and the like, and combinations thereof).
  • the rate of particle production can vary in the range(s) from about 1 grams per hour of reaction product to about 100 kilograms per hour of desired reaction product.
  • Tubular sections 110, 112 extend from the main chamber 104.
  • Tubular sections 110, 112 hold windows 114, 116, respectively, to define a hght beam path 118 through the reaction chamber 100.
  • Tubular sections 110, 112 can comprise inert gas inlets 120, 122 for the introduction of inert gas into tubular sections 110, 112.
  • Outlet 106 can lead to a conduit directed to a coating chamber.
  • the reaction zone is located within the reaction chamber.
  • a change in dimension does not necessarily demarcate a transition from the reaction chamber to a conduit to the coating chamber for appropriate embodiments.
  • the conduit can but does not necessarily involve a change in direction of the flow.
  • a subsfrate can intercept the product flow to coat the substrate within the reactant chamber.
  • a separate shielding gas system 360 can be used to dehvery inert shielding gas to a moving nozzle assembly in reaction chamber 304, although inert gas source 324 can be used to supply inert gas to an external section of the moving nozzle.
  • the shielding gas from the external sections of the nozzle serve as a guide for the reactant precursor stream into the light reaction zone.
  • exhaust system 308 comprises a conduit 560, as shown schematically in Fig. 13.
  • Conduit 560 comprises channels 566, 568, 570, 572 that connect respectively with vents 400, 402, 404, 406.
  • Exhaust system 308 further comprises a particle filter 574, two in-line Sodasorb® (W.R. Grace) chlorine traps 576, 578 and a pump 580.
  • Conduit 560 connects with particle filter 574, and Sodasorb® traps 576, 578 are placed between particle filter 574 and pump 580 to prevent chlorine from damaging the pump.
  • the line from second chlorine trap 578 can go directly to the pump.
  • a suitable pump is a dry rotary pump from Edwards, such as model QDP80.
  • a rod shaped subsfrate 600 is mounted within reaction chamber 252.
  • Substrate 600 is supported by axel 602, which is connected to drive 604.
  • Drive includes, for example, a suitable motor to turn axel 602.
  • a direct drive or a drive with a suitable transmission can be used.
  • a range of suitable motors is known in the art and are commercially available.
  • Drive 604 can rotate subsfrate 600 to provide desired coating onto the outside of subsfrate 600.
  • the composition of product particles deposited on the substrate can be changed during the deposition process to deposit particles with a particular composition at selected locations on the substrate to vary the resulting composition of the material along the x-y plane. For example, if the product particle compositions are changed while sweeping the substrate through the product particle stream, stripes or grids can be formed on the subsfrate surface with different particle compositions in different stripes or grid locations.
  • the product composition can be varied by adjusting the reactants that react to form the product particle or by varying the reaction conditions.
  • the reaction conditions can also affect the resulting product particle properties. For example, the reaction chamber pressure, flow rates, radiation intensity, radiation energy/wavelength, concenfration of inert diluent gas in the reaction stream, temperature of the reactant flow can affect the composition and other properties of the product particles.
  • a release layer is deposited that has a significantly different coefficient of thermal expansion such that heating or cooling fractures the release layer providing for the release of the stracture.
  • the platen is coated with a highly crosslinked polymer such that the deposited structure will easily release form the material.
  • the initial particle size of the deposited material is significantly larger than subsequent particles such that the larger particles do not stick well to the surface, and mechanical force releases the stracture form the substrate.
  • Adaptation of laser pyrolysis for the performance of light reactive deposition can be used to produce coatings of comparable compositions as the particles with selected compositions that can be produced by laser pyrolysis, which span a broad range of compositions.
  • the compositions can comprise one or more metal/metalloid elements forming a crystalline or amorphous material with an optional dopant or additive composition, hi addition, dopant(s)/additive(s) can be used to alter the chemical and/or physical properties of the particles.
  • the powders comprise fine or ultrafine particles with particle sizes in the submicron/nanometer range. The particles may or may not partly fuse or sinter during the deposition while forming a powder coating.
  • compositions are described with respect to particular stoichiometries/ compositions, stoichiometries generally are only approximate quantities.
  • materials can have contaminants, defects and the like.
  • some amorphous materials can comprise essentially blends such that the relative amounts of different components are continuously adjustable over ranges in which the materials are miscible.
  • phase separated amorphous materials can be formed with differing compositions at different domains due to immiscibility of the materials at the average composition.
  • the materials can comprise a plurality of oxidation states.
  • Metal borates can be similarly formed using one or more metal precursors and a boron precursor.
  • TiB 2 has potential utility in battery applications.
  • Suitable titanium precursors include, for example, titanium tetrachloride (TiC ), titanium isopropoxide (Ti[OCH(CH 3 ) 2 ] 4 ), and the like, and combinations of any two or more thereof
  • Suitable boron precursors comprise, for example, boron trichloride (BC1 3 ), diborane (B 2 H 6 ), BH 3 , and the like, and combinations of any two or more thereof.
  • dielectric oxides suitable for incorporation into ceramic chip capacitors with appropriate dopant(s)/additive(s) comprise, for example, SrTiO 3 , CaTiO 3 , SrZrO 3 , CaZrO 3 , Nd 2 O 3 -2TiO 3 , La 2 O 3 -2TiO 2 , and the like, and any two or more thereof.
  • no primary particles have an average diameter in the range(s) of greater than about 10 times the average diameter, in some embodiments in the range(s) of greater than about 5 times the average diameter, in further embodiments in the range(s) of greater than about 4 times the average diameter, in additional embodiments in the range(s) of greater than about 3 times the average diameter, and in other embodiment in the range(s) greater than about 2 times the average diameter.
  • a person of ordinary skill in the art will recognize that other ranges of distribution cut-offs within these explicit ranges are contemplated and are within the present disclosure.
  • the particle size distribution effectively does not have a tail indicative of a small number of particles with significantly larger sizes relative to the average size.
  • the distance from the substrate to the reaction zone and the temperature of the subsfrate can be adjusted to control the character of the deposit on the subsfrate surface.
  • the particles on the surface form a powder coating.
  • the powder coating can be in the form of independent primary particles randomly stacked on the surface.
  • the coating of primary particles may only be held together by electromagnetic forces between adjacent and nearby particles. In some embodiments, it may be desirable to form a powder coating with some degree of hard fusing between primary particles.
  • the polymer is imbibed into porous matrix deposited by light reactive deposition.
  • the porous mafrix generally is electrically insulating and does not block or inhibit ionic flow through the elecfrolyte.
  • the porous matrix can be formed from a proton conducting ceramic or a hydroscopic solid material.
  • the electrodes can be laminated to the elecfrolyte before, during or after introduction of the polymer, or the electrodes can be deposited in association with the electrolyte matrix by light reactive deposition.
  • the electrodes would comprise a suitable catalyst material and, if necessary, a suitable electrical conductor.
  • composition and/or particle morphology can be varied across a layer.
  • concentration/activity of the reactant drops. Therefore, it may be desirable to have a higher concenfration of catalyst, which can be the electrocatalyst and/or a reformation catalyst, away from the reactant inlet to compensate for the decrease in reactant concentration.
  • This gradient can also be established at an angle to the symmetry axes of the face of the elecfrode by placing the subsfrate at a co ⁇ esponding angle in the coating apparatus. In this way, the cu ⁇ ent/elecfrochemical reaction can be more uniform across the cell for improved cell performance.
  • This example demonstrates the synthesis of aluminum doped lithium manganese oxides and LiAlO2 by laser pyrolysis with an aerosol.
  • Laser pyrolysis was carried out using a reaction chamber essentially as described above with respect to Figs. 1, 3 and 4.

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US7521097B2 (en) 2009-04-21

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