Process for anodically coating aluminum and/or titanium with ceramic oxides
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C25D-011/02
C25D-011/04
C25D-009/06
C25D-009/00
출원번호
UP-0972594
(2004-10-25)
등록번호
US-7578921
(2009-09-08)
발명자
/ 주소
Dolan, Shawn E.
출원인 / 주소
Henkel KGaA
대리인 / 주소
Cameron, Mary K.
인용정보
피인용 횟수 :
11인용 특허 :
65
초록▼
An article of manufacture and a process for making the article by generating corrosion-, heat-and abrasion-resistant ceramic coatings comprising titanium and/or zirconium dioxide using direct and alternating current on anodes comprising aluminum and/or titanium. Optionally, the article is coated wi
An article of manufacture and a process for making the article by generating corrosion-, heat-and abrasion-resistant ceramic coatings comprising titanium and/or zirconium dioxide using direct and alternating current on anodes comprising aluminum and/or titanium. Optionally, the article is coated with additional layers, such as paint, after deposition of the ceramic coating.
대표청구항▼
What is claimed is: 1. A method of forming a protective coating on a surface of an aluminum, aluminum alloy, titanium or titanium alloy article, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt, and one or more additional compon
What is claimed is: 1. A method of forming a protective coating on a surface of an aluminum, aluminum alloy, titanium or titanium alloy article, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt, and one or more additional components selected from the group consisting of: a) water-soluble complex fluorides, b) water-soluble complex oxyfluorides, c) water-dispersible complex fluorides, and d) water-dispersible complex oxyfluorides of elements selected from the group consisting of Ti, Zr, Hf, Sn, Al, Ge and B and mixtures thereof; B) providing a cathode in contact with said anodizing solution; C) placing an aluminum, aluminum alloy, titanium or titanium alloy article as an anode in said anodizing solution; and D) passing a pulsed direct current between the anode and cathode through said anodizing solution for a time effective to form a protective coating on at least one surface of the article. 2. The method of claim 1 wherein the article comprises predominantly titanium. 3. The method of claim 1 wherein the article comprises predominantly aluminum and the protective coating is predominantly titanium dioxide. 4. The method of claim 1 wherein the protective coating comprises predominantly oxides of Ti, Zr, Hf, Sn, Ge and/or B. 5. The method of claim 1 wherein the protective coating is predominantly comprised of titanium dioxide. 6. The method of claim 1 wherein said current is pulsed direct current having an average voltage of not more than 200 volts. 7. The method of claim 1 wherein during step (D) said protective coating is formed at a rate of at least 1 micron thickness per minute. 8. The method of claim 1 wherein said current is pulsed direct current having a peak voltage of 300-600 volts. 9. The method of claim 1 wherein said anodizing solution comprises water, a phosphorus containing acid and water-soluble and/or water-dispersible complex fluorides of Ti and/or Zr. 10. The method of claim 1 wherein the anodizing solution has a pH of 1-6. 11. The method of claim 1 wherein the anodizing solution is prepared using a complex fluoride selected from the group consisting of H2TiF6, H2ZrF6, H2HfF6, H2GeF6, H2SnF6, H3AlF6, HBF4 and salts and mixtures thereof. 12. The method of claim 11 wherein the anodizing solution is additionally comprised of HF or a salt thereof. 13. The method of claim 1 wherein the anodizing solution is additionally comprised of a chelating agent. 14. The method of claim 1 wherein said phosphorus containing acid and/or salt is present in a concentration, measured as P, of 0.01 to 0.25 M. 15. The method of claim 1 wherein the article is an automobile wheel. 16. A method of forming a protective coating on a surface of a metallic article comprised predominantly of aluminum or titanium, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing oxy acid and/or salt, and a water-soluble complex fluoride and/or oxyfluoride of an element selected from the group consisting of Ti, Zr, and combinations thereof; B) providing a cathode in contact with said anodizing solution; C) placing a metallic article comprised predominantly of aluminum or titanium as an anode in said anodizing solution; and D) passing a non-pulsed direct current or an alternating current between the anode and the cathode at voltage from 200 to 600 volts for a time effective to form a protective coating comprising oxides of Ti and/or Zr on at least one surface of the metallic article. 17. The method of claim 16 wherein the anodizing solution is prepared using a complex fluoride comprising an anion comprising at least 4 fluorine atoms and at least one atom selected from the group consisting of Ti, Zr, and combinations thereof. 18. The method of claim 16 wherein the anodizing solution is prepared using a complex fluoride selected from the group consisting of H2TiF6, H2ZrF6, and salts and mixtures thereof. 19. The method of claim 16 wherein said complex fluoride is introduced into the anodizing solution at a concentration of at least 0.01M. 20. The method of claim 16 wherein the anodizing solution is additionally comprised of a chelating agent. 21. The method of claim 16 wherein the anodizing solution is comprised of at least one complex oxyfluoride prepared by combining at least one complex fluoride of at least one element selected from the group consisting of Ti and Zr and at least one compound which is an oxide, hydroxide, carbonate or alkoxide of at least one element selected from the group consisting of Ti, Zr, Hf, Sn, B, Al and Ge. 22. The method of claim 16 wherein the anodizing solution has a pH of from 2 to 6. 23. The method of claim 16 wherein the article is an automobile wheel. 24. A method of forming a protective coating on an article having at least one metallic surface comprised of titanium, titanium alloy, aluminum or aluminum alloy, said method oomprising: A) providing an anodizing solution, said anodizing solution having been prepared by dissolving a water-soluble complex fluoride and/or oxyfluoride of an element selected from the group consisting of Ti, Zr, Hf, Sn, Ge, B and combinations thereof, and an acid and/or salt that contains phosphorus in water; B) providing a cathode in contact with said anodizing solution; C) placing said metallic surface comprised of titanium, titanium alloy, aluminum or aluminum alloy as an anode in said anodizing solution; and D) passing a non-pulsed direct current or an alternating current between the anode and the cathode at voltage from 200 to 600 volts for a time effective to form a protective coating on said metallic surface of the article. 25. The method of claim 24 wherein pH of the anodizing solution is adjusted using ammonia, an amine, an alkali metal hydroxide or a mixture thereof. 26. The method of claim 24 wherein said phosphorus containing acid and/or salt is present in a concentration, measured as P, of 0.01 to 0.25 M. 27. The method of claim 24 wherein the anodizing solution is additionally comprised of a chelating agent. 28. The method of claim 24 wherein at least one compound which is an oxide, hydroxide, carbonate or alkoxide of at least one element selected from the group consisting of Ti, Zr, Si, Hf, Sn, B, Al and Ge is additionally used to prepare said anodizing solution. 29. The method of claim 28 wherein zirconium basic carbonate is used to prepare the anodizing solution. 30. The method of claim 24 wherein the protective coating comprises predominantly oxides of Ti, Zr, Hf, Sn, Ge and/or B. 31. The method of claim 24 wherein one or more of H2TiF6, salts of H2TiF6, H2ZrF6, and salts of H2ZrF6 is used to prepare the anodizing solution. 32. The method of claim 24 wherein the one or more water-soluble complex fluorides is a complex fluoride of titanium and the current is direct current. 33. The method of claim 16 wherein the article is an automobile wheel. 34. A method of forming a protective coating on an article having at least one surface comprising aluminum and/or titanium, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt, a water-soluble and/or water-dispersible complex fluoride of Ti and one or more additional components selected from the group consisting of: a) water-soluble and/or water-dispersible complex fluorides of elements selected from the group consisting of Zr, Hf, Sn, Al, Ge and B; b) water-soluble and/or water-dispersible zirconium oxysalts; c) water-soluble and/or water-dispersible vanadium oxysalts; d) water-soluble and/or water-dispersible titanium oxysalts; e) water-soluble and/or water-dispersible niobium salts; f) water-soluble and/or water-dispersible molybdenum salts; g) water-soluble and/or water-dispersible manganese salts; and h) water-soluble and/or water-dispersible tungsten salts; B) providing a cathode in contact with said anodizing solution; C) placing an article having at least one surface comprising aluminum and/or titanium as an anode in said anodizing solution; and D) passing a non-pulsed direct current or an alternating current between the anode and cathode through said anodizing solution at voltage from 200 to 600 volts for a time effective to form a protective coating on at least one surface of the article. 35. The method of claim 34 wherein the pH is 2-6 and the anodizing solution additionally comprises water-soluble and/or water-dispersible alkali metal fluorides and/or hydroxides. 36. The method of claim 34 wherein the anodizing solution comprises water-soluble and/or water-dispersible complex fluorides of Ti and/or Zr; and at least one compound which is an oxide, hydroxide, carbonate or alkoxide of at least one element selected from the group consisting of Ti, Zr, Hf, Sn, B, Al and Ge. 37. The method of claim 34 wherein the anodizing solution comprises water-soluble and/or water-dispersible complex fluorides of elements selected from the group consisting of Ti, Zr, Hf, Sn, Al, Ge and B; and at least one of said zirconium oxysalts, vanadium oxysalts, titanium oxysalts, niobium salts, molybdenum salts, manganese salts and/or tungsten salts. 38. The method of claim 37 wherein said protective coating comprises a ceramic film of zirconium oxide and/or titanium oxide further comprising niobium, molybdenum, manganese, and/or tungsten co-deposited therein. 39. The method of claim 34 wherein said one or more additional components comprises water-soluble and/or water-dispersible complex fluorides of elements selected from the group consisting of Zr, Hf, Sn, Al, Ge and B and the protective coating comprises predominantly oxides of Ti, Zr, Hf, Sn, Ge and/or B. 40. The method of claim 39 wherein said protective coating comprises a ceramic film of zirconium oxide and/or titanium oxide, said ceramic film further comprising niobium, molybdenum, manganese, and/or tungsten co-deposited therein. 41. The method of claim 34 wherein the article comprises predominantly aluminum, said one or more additional components comprises water-soluble and/or water-dispersible complex fluorides of Zr and the protective coating is predominantly titanium dioxide and zirconium oxide. 42. The method of claim 34 wherein the article is an automobile wheel. 43. A method of forming a protective coating on an article having at least one surface comprising aluminum and/or titanium, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt, one or more water-soluble and/or water-dispersible complex fluorides of elements selected from the group consisting of Ti, Zr, Hf, Sn, Al, Ge and B; and one or more additional components selected from the group consisting of: a) water-soluble and/or water-dispersible zirconium oxysalts; b) water-soluble and/or water-dispersible vanadium oxysalts; c) water-soluble and/or water-dispersible titanium oxysalts; d) water-soluble and/or water-dispersible niobium salts; e) water-soluble and/or water-dispersible molybdenum salts; f) water-soluble and/or water-dispersible manganese salts; and g) water-soluble and/or water-dispersible tungsten salts; B) providing a cathode in contact with said anodizing solution; C) placing an article having at least one surface comprising aluminum and/or titanium as an anode in said anodizing solution; and D) passing a pulsed direct current between the anode and cathode through said anodizing solution, said current having a peak voltage from 300 to 600 volts, for a time effective to form a protective coaling on at least one surface of the article. 44. A method of forming a protective coating on a surface of an aluminum or aluminum alloy article, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt, and one or more additional components selected from the group consisting of: a) water-soluble complex fluorides, b) water-soluble complex oxyfluorides, c) water-dispersible complex fluorides, and d) water-dispersible complex oxyfluorides of elements selected from the group consisting of Ti, Zr, Hf, Sn, Al, Ge and B and mixtures thereof; B) providing a cathode in contact with said anodizing solution; C) placing an aluminum or aluminum alloy article as an anode in said anodizing solution; and D) passing a current between the anode and cathode through said anodizing solution for a time effective to form a protective coating on at least one surface of the article wherein the article comprises predominantly aluminum and the protective coating is predominantly titanium dioxide. 45. A method of forming a protective coating on an article having at least one surface comprising aluminum and/or titanium, said method comprising: A) providing an anodizing solution comprised of water, a phosphorus containing acid and/or salt and one or more additional components selected from the group consisting of: a) water-soluble and/or water-dispersible zirconium oxysalts; b) water-soluble and/or water-dispersible vanadium oxysalts; c) water-soluble and/or water-dispersible titanium oxysalts; d) water-soluble and/or water-dispersible niobium salts; e) water-soluble and/or water-dispersible molybdenum salts; f) water-soluble and/or water-dispersible manganese salts; and g) water-soluble and/or water-dispersible tungsten salts; B) providing a cathode in contact with said anodizing solution; C) placing an article having at least one surface comprising aluminum and/or titanium as an anode in said anodizing solution; and D) passing a non-pulsed direct current or an alternating current between the anode and cathode through said anodizing solution at voltage from 200 to 600 volts for a time effective to form a protective coating on at least one surface of the article; wherein the anodizing solution comprises water-soluble and/or water-dispersible complex fluorides of elements selected from the group consisting of Ti, Zr, Hf, Sn, Al, Ge and B.
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