SELF-ORDERED NANOTUBES OF TITANIUM OXIDES AND TITANIUM ALLOY OXIDES FOR ENERGY STORAGE AND BATTERY APPLICATIONS

• US 20100320089A1
• Filed: 12/12/2007
• Published: 12/23/2010
• Est. Priority Date: 12/12/2006
• Status: Abandoned Application

• Current Assignee: Board of Regents Nevada System of Higher Education (State of Nevada)
• Original Assignee: Board of Regents Nevada System of Higher Education (State of Nevada)
• Inventors: Mahajan, Vishal K., Zhong, Kangnian, Raja, Krishnan S., Misra, Manoranjan
• Application Number:
  US12/518,053
• Publication Number:
  US 20100320089A1
• Time in Patent Office: Days
• US Class Current: 205/109
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01G 23/047 Titanium dioxide
• CPC Class Codes: C01G 45/00 Compounds of manganese
• CPC Class Codes: C01P 2002/34 perovskite-type (ABO3)
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/13 Nanotubes
• CPC Class Codes: C01P 2006/40 Electric properties
• CPC Class Codes: C25D 11/26 of refractory metals or alloys based thereon
• CPC Class Codes: C30B 7/005 Epitaxial layer growth
• CPC Class Codes: H01M 4/485 of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy H01M4/505, H01M4/525 take precedence
• CPC Class Codes: Y02E 60/10 Energy storage using batteries

Abstract

The present disclosure provides oxide nanotubes formed by anodizing and oxidatively-annealing a titanium or titanium allow substrate with or without ultrasonication. If desired, carbon nanotubes may be grown in the oxide nanotubes. The substrates show improved specific capacity and charge-discharge rates for use as an electrode in lithium-ion batteries.

Claims

1-20. -20. (canceled)

21. A method of manufacturing an anodized and oxidatively-annealed titanium oxide or for energy storage, comprising:

anodizing a titanium substrate under conditions sufficient to form an anodized titanium oxide having a plurality of self-ordered oxide nanotubes on the anodized surface; and

annealing the oxide nanotubes in a controlled oxidizing atmosphere to produce an anodized and oxidatively-annealed titanium oxide substrate having a surface area sufficient to incorporate ions for energy storage.

22. The method of claim 21, wherein the anodizing step comprises electrochemically anodizing the titanium material in an aqueous or non-aqueous electrolyte solution containing a fluoride salt.

23. The method of claim 22, wherein the non-aqueous solution is a polyhydric alcohol selected from the group consisting of glycerol, ethylene glycol, diethylene glycol, and mixtures thereof.

24. The method of claim 22, wherein the electrolyte solution further comprises a complexing agent.

25. The method of claim 21, wherein the anodizing step further comprises ultrasonicating the electrolyte solution during anodization.

26. The method of claim 21, further comprising the steps of:

electrodepositing a plurality of catalyst particles in the oxide nanotubes to provide nucleation sites for carbon nanotube growth, and growing carbon nanotubes at the nucleation sites by introducing a carbon source, hydrogen gas, and an inert gas onto the titanium oxide or titanium alloy oxide substrate under chemical vapor deposition process conditions.

27. A method of manufacturing an anodized titanium alloy oxide substrate, comprising:

anodizing a titanium alloy substrate under conditions sufficient to form anodized titanium alloy oxide having a plurality of self-ordered oxide nanotubes on the anodized surface; and

annealing the oxide nanotubes in a controlled gaseous atmosphere to produce an anodized titanium alloy oxide substrate.

28. The method of claim 27, wherein the anodizing step comprises electrochemically anodizing the titanium alloy material in an aqueous or non-aqueous electrolyte solution containing a fluoride salt.

29. The method of claim 28, wherein the non-aqueous solution is a polyhydric alcohol is selected from the group consisting of glycerol, ethylene glycol, diethylene glycol, and mixtures thereof.

30. The method of claim 27, wherein the electrolyte solution further comprises a complexing agent.

31. The method of claim 27, wherein the anodizing step further comprises ultrasonicating the electrolyte solution during anodization.