IP Library Granted Patent US 9,068,271
Granted Patent B2
US 9,068,271 · App. 13/581,184 · Granted Jun 30, 2015

Electrochemical nitridation of metal surfaces

Inventors: Heli Wang (Littleton, CO); John A. Turner (Littleton, CO)
Assignee: Alliance for Sustainable Energy, LLC
C25D11/00C23C8/48C23C8/50C25D11/02H01M8/021H01M8/0215H01M8/0228H01M2008/1095Y02E60/50
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Quick Facts
Patent No.
US 9,068,271
App. No.
13/581,184
Granted
Jun 30, 2015
Kind
B2
Abstract

Electrochemical nitridation of metals and the produced metals are disclosed. An exemplary method of electrochemical nitridation of metals comprises providing an electrochemical solution at low temperature. The method also comprises providing a three-electrode potentiostat system. The method also comprises stabilizing the three-electrode potentiostat system at open circuit potential. The method also comprises applying a cathodic potential to a metal.

Claims (22)

1. A method of electrochemical nitridation of a metal, the method comprising:

providing a potentiostat system comprising a potentiostat, a counter electrode, a reference electrode, and a working electrode comprising the metal;

immersing the working electrode, the counter electrode, and the reference electrode in a solution, wherein the solution consists of nitric acid and at least one nitrate; and

applying a cathodic potential, whereby the metal is nitrided with a nitride surface layer.

2. The method of claim 1 , wherein the metal comprises a self-passivating metal.

3. The method of claim 2 , wherein the self-passivating metal comprises at least one of Cr, Al, Fe, or Ti.

4. The method of claim 1 , further comprising stabilizing the potentiostat system at an open circuit potential, wherein the stabilizing occurs before applying the cathodic potential, and occurs for less than about 10 minutes.

5. The method of claim 4 , wherein the stabilizing is performed for about 5 minutes.

6. The method of claim 1 , wherein the cathodic potential ranges from about −0.7V to about −1V.

7. The method of claim 6 , wherein the applying the cathodic potential is performed for a period of time ranging from about 0.5 to about 8 hours.

8. The method of claim 1 , wherein the immersing in the solution is performed at a temperature ranging from about 0° C. to about 100° C.

9. The method of claim 1 , wherein the reference electrode comprises a saturated calomel electrode.

10. The method of claim 1 , wherein the nitric acid has a concentration of about 0.1 M and the at least one nitrate is at a concentration of about 0.5 M.

11. The method of claim 1 , wherein the at least one nitrate is at least one of NaNO 3 , NH 4 NO 3 , or Mg(NO 3 ) 2 .

12. The method of claim 1 , wherein the solution has a pH ranging from about 0 to about 3.

13. The method of claim 1 , wherein the applying the cathodic potential is performed for a period of time ranging from about 0.5 hours to about 8 hours.

14. The method of claim 1 , wherein the cathodic potential is applied until the nitride surface layer ranges in thickness from about 2 nm to about 5 nm.

15. A method of electrochemical nitridation of a metal, the method comprising:

providing a potentiostat system comprising a potentiostat, a working electrode comprising the metal, a platinum counter electrode, and a reference electrode comprising a saturated calomel electrode, wherein the metal comprises at least one of Cr, Al, Fe, or Ti;

immersing the working electrode, the counter electrode, and the reference electrode in a solution at a temperature ranging from about 0° C. to about 100° C., wherein the solution consists of nitric acid and at least one of NaNO 3 , NH 4 NO 3 , or Mg(NO3) 2 , and the solution is adjusted to a pH ranging from about zero to three;

stabilizing the potentiostat system at an open circuit potential for a first period of time ranging from about 30 seconds to about 10 minutes; and

applying a cathodic potential ranging from about −0.7V to about −1V for a second period of time ranging from about 0.5 hours to about 8 hours, whereby the metal is nitrided with a nitride surface layer ranging in thickness from about 2 nm to about 5 nm.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 8, 2015
From: WANG, HELI; TURNER, JOHN A.
To: ALLIANCE FOR SUSTAINABLE ENERGY, LLC
Reel/Frame 034665/0737 →
CONFIRMATORY LICENSE Recorded Oct 26, 2012
From: ALLIANCE FOR SUSTAINABLE ENERGY, LLC
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 029235/0355 →
Continuity (1)
Related Publication 20120325673A1 · Dec 27, 2012