Electrode structure, substrate holder, and method for forming anodic oxidation layer
US-9315916-B2 · Apr 19, 2016 · US
US9903035B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9903035-B2 |
| Application number | US-201314649188-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 2, 2013 |
| Priority date | Dec 3, 2012 |
| Publication date | Feb 27, 2018 |
| Grant date | Feb 27, 2018 |
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The present disclosure provides devices, systems and methods with applicability in the coating of surfaces, in particular three-dimensional surfaces, via anodization reactions. For example, the disclosed devices, systems and methods find use in the formation of microstructured or nanostructured layers, e.g., metal oxide microstructured or nanostructured layers, via anodization on a variety of devices including, e.g., medical devices. Devices modified with one or more microstructured or nanostructured layers are also provided.
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What is claimed is: 1. A method of forming metal oxide nanotubes uniformly on a three dimensional surface of a structure, the method comprising: positioning a single structure in a coating device comprising: a first plate comprising a central anode receiving opening and at least three cathode receiving openings positioned radially around the central anode receiving opening; a second plate positioned in opposition to the first plate and comprising at least three cathode receiving openings; a plurality of supports separating the first and second plates, the at least three cathodes extending through the at least three cathode receiving openings of the first plate and into the at least three cathode receiving openings of the second plate; and the anode extending through the central anode receiving opening and contacting the structure and positioning the structure in the centrally positioned receiving region relative to at least three cathodes, wherein the structure comprises a metal and the metal is at least 0.1 weight percent of the structure and wherein the structure is positioned at an equal distance from each of the at least three cathodes, wherein the anode holds the structure in place and electrically connects the structure to a power source and wherein the at least three cathodes are separate individual cathodes; submerging the structure and the at least three cathodes in an electrolyte solution; and applying electrical energy between the anode and the at least three cathodes for a period of time sufficient to form metal oxide nanotubes on the three dimensional surface of the structure, wherein the method provides for uniform growth of the metal oxide nanotubes on the three dimensional surface of the structure. 2. The method of claim 1 , wherein the nanotube comprises an oxide of the metal. 3. The method of claim 1 , wherein the oxide of the metal is a metal oxide comprising an oxide of aluminum, niobium, tantalum, titanium, tungsten, zirconium or mixtures thereof. 4. The method of claim 1 , wherein the metal is at least 10 weight percent of the structure. 5. The method of claim 1 , wherein the period of time is sufficient to form at least one nanotube with a length of at least 10 nm on the three dimensional surface of the structure. 6. The method of claim 1 , wherein the diameter of the at least one nanotube is a diameter in the range of from 1 nm to 1,000 nm. 7. The method of claim 1 , wherein the diameter of the at least one nanotube is a diameter in the range of from 10 nm to 200 nm. 8. The method of claim 1 , wherein the step of applying electrical energy between the anode and the at least three cathodes comprises applying a substantially constant voltage for the period of time ranging from 5 minutes to 90 minutes. 9. The method of claim 8 , wherein the substantially constant voltage is a substantially constant voltage in the range of from about 10 Volt to 100 kilovolts. 10. The method of claim 1 , wherein the step of applying electrical energy between the anode and the at least three cathodes comprises applying a substantially constant current for the period of time. 11. The method of claim 10 , wherein the substantially constant current is a substantially constant current in the range of from about 1 femtoampere to about 100 kiloamperes. 12. The method of claim 1 , wherein the electrolyte solution comprises compounds of aluminum, niobium, tantalum, titanium, tungsten, zirconium or mixtures thereof. 13. The method of claim 1 , wherein the structure comprises a medical device or a portion thereof. 14. The method of claim 13 , wherein the medical device comprises a stent, sensor, arteriovenous shunt, pacemaker, or combinations thereof. 15. The method of claim 1 , wherein the method comprises maintaining the electrolyte solution at a substantially constant temperature. 16. The method of claim 15 , wherein the substantially constant temperature is above a freezing point of the electrolyte solution and below a boiling point of the electrolyte solution. 17. The method of claim 16 , wherein the substantially constant temperature is a substantially constant temperature in the range of from about 10° C. to about 50° C. 18. The method of claim 1 , wherein the period of time is a time in the range of from 5 seconds to 5 days. 19. The method of claim 18 , wherein the period of time is a time in the range of from 10 min to 60 min. 20. The method of claim 1 , wherein the structure is electropolished prior to the submerging in the electrolyte solution. 21. The method of claim 1 , wherein the one or more cathodes comprise aluminum, niobium, tantalum, titanium, tungsten, zirconium or alloys thereof. 22. The method of claim 1 , wherein the one or more cathodes comprise graphite. 23. The method of claim 1 , wherein the second plate includes a projection and wherein the structure is held in place by the anode and the projection. 24. The method of claim 1 , wherein the device comprises at least five cathodes and wherein the first plate comprises at least five cathode receiving openings positioned radially around the central anode receiving opening and the second plate comprises at least five cathode receiving openings and the structure is positioned at an equal distance from each of the at least five cathodes.
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