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1. (EP2314734) Method of producing porous metal oxide films using template assisted electrostatic spray deposition
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Claims

1. A method of producing a porous metal oxide film on a substrate comprising

(a) forming a precursor solution comprising a solvent, at least one metal precursor and at least one pore forming organic template

(b) depositing the precursor solution formed in (a) onto a substrate using electrostatic spray deposition process and

(c) thermally treating the product obtained in (b) in an atmosphere having an oxygen content from 0 to 50 vol.-% and by following a temperature profile comprising one or more heating ramps, one or more temperature plateaus and one or more cooling ramps.


  2. The method according to claim 1, characterized in that the substrate is pretreated by applying a passivation layer onto its surface prior to depositing the precursor solution.
  3. The method according to claims 1 or 2, characterized in that the deposition of the precursor solution and part of the thermal treatment of the film are performed concurrently.
  4. The method according to the preceding claims, characterized in that at least one metal precursor comprises metal halogenides, metal nitrates, metal sulphates, metal acetates, metal citrates, metal alkoxides or a mixture thereof, preferably metal alkoxides.
  5. The method according to the preceding claims, characterized in that at least one pore forming organic template is an ionic or non-ionic surfactant, an amphiphilic block copolymer, a solid organic particle having a mean diameter in the range of 50 nm to 5 µm, preferably in the range of 50 nm to 500 nm, or a mixture thereof.
  6. The method according to claim 5, characterized in that the ionic or non-ionic surfactant, the amphiphilic block copolymer or the mixture thereof is used in a concentration being above the critical micelle concentration, the concentration preferably being in the range of 0.01 to 5 g/l, more preferred in the range of 0.1 to 2 g/l and most preferred in the range of 0.1 to 1 g/l.
  7. The method according to claim 5, characterized in that the solid organic particles are used in the range of 0.1 to 50 g/l preferably in the range of 0.1 to 30g/l and more preferred in the range of 1 to 10 g/l.
  8. The method according to any one of the preceding claims, characterized in that the amphiphilic block polymer is a di-block, tri-block or multi-block copolymer capable of forming micelles in aqueous and non-aqueous solvents, preferably polyethylene oxide-blockpolypropylene oxide-block-polyethylene oxide, polypropylene oxide-block-polyethylene oxide-block-polypropylene oxide, polyethylene oxide-block-polyisobutylene-blockpolyethylene oxide, polyethylene-block-polyethylene oxide, polyisobutylene-block-polyethylene oxide or a mixture thereof, more preferred polyethylene oxide-block-polypropylene oxide-block-polyethylene oxide.
  9. The method according to any one of the preceding claims, characterized in that the solid organic particles are polystyrene, polymethyl methacrylate, styrene-acrylate copolymer, styrene-butadiene-copolymer, nitrile-butadiene-copolymer, pyridine-styrene-butadiene-copolymer or mixtures thereof, preferably polymethyl metacrylate.
  10. The method according to any one of claims 5 to 9, characterized in that the pore forming organic template is a mixture of an amphiphilic block copolymer and solid organic particles in the range of 20:1 to 1:20, preferably in the range of 10:1 to 1:10 and more preferred in the range of 5:1 to 1:5.
  11. The method according to any one of the preceding claims, characterized in that the substrate material comprises steel, glass, graphite or other material withstanding the thermal treatment.
  12. The method according to any one of the preceding claims, characterized in that the solvent is a polar organic solvent, preferably a volatile polar organic solvent, a mixture of two or more volatile polar organic solvents or a mixture thereof with water.
  13. A porous film obtainable by the production method according to any one of claims 1 to 12.
  14. The porous film according to claim 13, characterized in that the porosity is greater than 60%, preferably greater than 70% and more preferred greater than 80%.
  15. Use of the porous film according to claims 13 or 14 as material for catalysis, power storage, sensing and compound separation.