Unsupported palladium alloy membranes and methods of making same

Patent metadata

Field	Value
Publication number	US-9044715-B2
Application number	US-19721808-A
Country	US
Kind code	B2
Filing date	Aug 22, 2008
Priority date	Aug 22, 2007
Publication date	Jun 2, 2015
Grant date	Jun 2, 2015

Abstract

The invention provides support-free palladium membranes and methods of making these membranes. Single-gas testing of the unsupported foils produced hydrogen permeabilities equivalent to thicker membranes produced by cold-rolling. Defect-free films as thin as 7.2 microns can be fabricated, with ideal H 2 /N 2 selectivities as high as 40,000. Homogeneous membrane compositions may also be produced using these methods.

First claim

What is claimed is:

1. A method of forming a free-standing hydrogen permeable palladium membrane comprising:
electroless plating of a surface of a support to form a palladium membrane on the support;
intentionally removing the palladium membrane from the support to produce the free-standing hydrogen permeable palladium membrane; and
plating the free-standing hydrogen permeable palladium membrane with a second metal.

2. The method of claim 1 , wherein the support is seeded with metallic palladium crystallites prior to the electroless plating.

3. The method of claim 2 , wherein the seeding comprises contacting the support with a solution of palladium acetate in an organic solvent.

4. The method of claim 2 , further comprising decomposing the palladium acetate prior to the electroless plating.

5. The method of claim 4 , wherein the decomposing comprise immersing the seeded support in a 3 wt % solution of hydrogen peroxide.

6. The method of claim 5 , wherein the immersing is conducted for about 30 minutes.

7. The method of claim 2 , further comprising reducing the support.

8. The method of claim 7 , wherein the reducing comprises contacting the support with hydrazine after the seeding.

9. The method of claim 8 , wherein the contacting is conducted for about 20 minutes at about 50° C.

10. The method of claim 1 , wherein the support is a stainless steel support.

11. The method of claim 10 , wherein the support is a mirror-finished stainless steel support.

12. The method of claim 1 , wherein the electroless plating comprises immersing the support in a palladium plating bath.

13. The method of claim 12 , wherein the palladium plating bath contains no ethylenediaminetetraacetic (EDTA).

14. The method of claim 1 , wherein the electroless plating comprises immersing the support in a palladium plating bath at about 50° C.; and, adding hydrazine to the plating bath.

15. The method of claim 14 , wherein the hydrazine is a 3M solution of hydrazine added to the plating solution in a 100:1 ratio of plating bath to hydrazine.

16. The method of claim 1 , wherein the removing comprises scoring the edge of the palladium film and lifting the film away from the support.

17. The method of claim 1 , further comprising electroless plating of a second metal onto the palladium membrane to form a layered metal membrane before the removing.

18. The method of claim 17 , wherein the second metal is selected from the group consisting of copper, silver and gold.

19. The method of claim 17 , further comprising annealing the layered metal membrane prior to the removing.

20. The method of claim 1 , wherein the second metal is selected from the group consisting of copper, silver and gold.

Assignees

• Way J Douglas
• Thoen Paul
• Gade Sabina K
• Colorado School Of Mines

Inventors

• Way J Douglas
• Thoen Paul
• Gade Sabina K

Classifications

• B01D2325/20

  Specific permeability or cut-off range · CPC title

• C23C18/1657

  Electroless forming, i.e. substrate removed or destroyed at the end of the process · CPC title

• C23C18/44

  using reducing agents · CPC title

• C23C18/1605

  by masking · CPC title

• C23C18/1692

  Heat-treatment · CPC title