IP Library Granted Patent US 9,290,845
Granted Patent B2
US 9,290,845 · App. 13/142,495 · Granted Mar 22, 2016

Stainless steel for polymer fuel cell separator and method for preparing same

Inventors: Jonghee Kim (Pohang-si, KR); Kihoon Jo (Pohang-si, KR); Younghwan Kim (Pohang-si, KR); Jeonghe Lee (Pohang-si, KR); Yunyong Lee (Pohang-si, KR); Jinsuk Kim (Pohang-si, KR); Jongheon Seok (Pohang-si, KR)
Assignee: POSCO
C23C22/34C22C38/001C22C38/004C22C38/005C22C38/02C22C38/04C22C38/06C22C38/42C22C38/44C22C38/46C22C38/48C22C38/50C23C8/02C23G1/081H01M8/021H01M2008/1095Y02E60/50
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Quick Facts
Patent No.
US 9,290,845
App. No.
13/142,495
Granted
Mar 22, 2016
Kind
B2
Abstract

There are provided a ferrite stainless steel for a polymer fuel cell separator having excellent corrosion resistance and interfacial contact resistance under an operating environment of a polymer fuel cell, and a preparation method of the stainless steel. A stainless steel includes C: 0.02 wt % or less, N: 0.02 wt % or less, Si: 0.4 wt % or less, Mn: 0.2 wt % or less, P: 0.04 wt % or less, S: 0.02 wt % or less, Cr: 25.0 to 32.0 wt %, Cu: 0 to 2.0 wt %, Ni: 0.8 wt % or less, Ti: 0.5 wt % or less, Nb: 0.5 wt % or less, waste Fe and inevitably contained elements. A preparation method of the stainless steel having a second passive film formed on a surface thereof includes forming a first passive film on the surface of the stainless steel by bright-annealing or annealing-pickling the stainless steel; removing the first passive film by pickling the stainless steel in a 10 to 20 wt % sulfuric acid solution at a temperature of 50 to 75° C. for a predetermined time; water-washing the stainless steel; and forming the second passive film by performing a passivation treatment on the stainless steel in the mixture of a 10 to 20 wt % nitric acid and a 1 to 10 wt % fluorine acid at a temperature of 40 to 60° C. for the predetermined time. Accordingly, it is possible to prepare a stainless steel having reduced elution resistance and excellent corrosion resistance and to produce a stainless steel for a polymer fuel cell separator, which has low interfacial contact resistance and excellent long-term performance even under a fuel cell operating condition of 60 to 150° C. and various surface roughness conditions.

Claims (32)

1. A preparation method of a stainless steel for a polymer fuel cell separator, comprising C: 0.02 wt % or less, N: 0.02 wt % or less, Si: 0.4 wt % or less, Mn: 0.2 wt % or less, P: 0.04 wt % or less, S: 0.02 wt % or less, Cr: 25.0 to 32.0 wt %, Cu: 0 to 2.0 wt %, Ni: 0.8 wt % or less, Ti: 0.5 wt % or less, Nb: 0.5 wt % or less, waste Fe and inevitably contained elements, in which a second passive film is formed on a surface of the stainless steel, the method comprising:

forming a first passive film on the surface of the stainless steel by bright-annealing or annealing-pickling the stainless steel;

removing the first passive film by pickling the stainless steel in a 10 to 20 wt % sulfuric acid solution at a temperature of 50 to 75° C. for a first processing time controlled based on a surface roughness Ra of the stainless steel, wherein the first processing time is increased as the surface roughness Ra is increased;

water-washing the stainless steel; and

forming the second passive film by performing a passivation treatment on the stainless steel in the mixture of a 10 to 20 wt % nitric acid and a 1 to 10 wt % fluorine acid at a temperature of 40 to 60° C. for a second processing time controlled based on the surface roughness Ra,

wherein, in the forming of the second passive film, the second processing time is controlled according to the following expression:

120+6.73(1/ Ra )≦second processing time(second)≦140+6.73(1/ Ra ).

2. The method of claim 1 , wherein the stainless steel is a ferrite stainless steel further comprising Mo: 5.0 wt % or less.

3. The method of claim 1 , wherein the stainless steel further comprises one or two or more elements selected from the group consisting of V: 0.1 to 1.5 wt %, W: 0.1 to 2.0 wt %, La: 0.0005 to 1.0 wt %, Zr: 0.0005 to 1.0 wt % and B: 0.0005 to 1.0 wt %.

4. The method of claim 1 , wherein, in the forming of the second passive film, the second passive film is formed to have a thickness of 2 to 4.5 nm.

5. The method of claim 1 , wherein, in the forming of the second passive film, the Cr/Fe oxide ratio of the second passive film is 1.5 or more in a region of 1.5 nm or less.

6. The method of claim 1 , wherein, in the forming of the second passive film, the Cr(OH) 3 /Cr oxide distribution of the second passive film has a ratio of 0 to 0.7 in a region of 1 nm.

7. The method of claim 1 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed on a steel plate after the bright-annealing or annealing-pickling of the stainless steel.

8. The method of claim 1 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed just before forming a flow path of the separator after the bright-annealing or annealing-pickling of the stainless steel.

9. The method of claim 1 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed just after forming a flow path of the separator after the bright-annealing or annealing-pickling of the stainless steel.

10. The method of claim 1 , wherein the contact resistance of the stainless steel is 10 mΩcm 2 or less under an operating environment of 60 to 150° C.

11. A preparation method of a stainless steel for a polymer fuel cell separator, comprising C: 0.02 wt % or less, N: 0.02 wt % or less, Si: 0.4 wt % or less, Mn: 0.2 wt % or less, P: 0.04 wt % or less, S: 0.02 wt % or less, Cr: 25.0 to 32.0 wt %, Cu: 0 to 2.0 wt %, Ni: 0.8 wt % or less, Ti: 0.5 wt % or less, Nb: 0.5 wt % or less, waste Fe and inevitably contained elements, in which a second passive film is formed on a surface of the stainless steel, the method comprising:

forming a first passive film on the surface of the stainless steel by bright-annealing or annealing-pickling the stainless steel;

removing the first passive film by pickling the stainless steel in a 10 to 20 wt % sulfuric acid solution at a temperature of 50 to 75° C. for a first processing time controlled based on a surface roughness Ra of the stainless steel, wherein the first processing time is increased as the surface roughness Ra is increased;

water-washing the stainless steel; and

forming the second passive film by performing a passivation treatment on the stainless steel in the mixture of a 10 to 20 wt % nitric acid and a 1 to 10 wt % fluorine acid at a temperature of 40 to 60° C. for a second processing time controlled based on the surface roughness Ra,

wherein, the first processing time is controlled according to the following expression:

99−3.18(1/ Ra )≦first processing time(second)≦153−3.18(1/ Ra ).

12. The method of claim 11 , wherein the stainless steel is a ferrite stainless steel further comprising Mo: 5.0 wt % or less.

13. The method of claim 11 , wherein the stainless steel further comprises one or two or more elements selected from the group consisting of V: 0.1 to 1.5 wt %, W: 0.1 to 2.0 wt %, La: 0.0005 to 1.0 wt %, Zr: 0.0005 to 1.0 wt % and B: 0.0005 to 1.0 wt %.

14. The method of claim 11 , wherein, in the forming of the second passive film, the second passive film is formed to have a thickness of 2 to 4.5 nm.

15. The method of claim 11 , wherein, in the forming of the second passive film, the Cr/Fe oxide ratio of the second passive film is 1.5 or more in a region of 1.5 nm or less.

16. The method of claim 11 , wherein, in the forming of the second passive film, the Cr(OH) 3 /Cr oxide distribution of the second passive film has a ratio of 0 to 0.7 in a region of 1 nm.

17. The method of claim 11 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed on a steel plate after the bright-annealing or annealing-pickling of the stainless steel.

18. The method of claim 11 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed just before forming a flow path of the separator after the bright-annealing or annealing-pickling of the stainless steel.

19. The method of claim 11 , wherein the removing of the first passive film, the water-washing and the forming of the second passive film are performed just after forming a flow path of the separator after the bright-annealing or annealing-pickling of the stainless steel.

20. The method of claim 11 , wherein the contact resistance of the stainless steel is 10 mΩcm 2 or less under an operating environment of 60 to 150° C.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 26, 2022
From: POSCO HOLDINGS INC.
To: POSCO CO., LTD
Reel/Frame 061777/0943 →
CHANGE OF NAME Recorded Sep 28, 2022
From: POSCO
To: POSCO HOLDINGS INC.
Reel/Frame 061561/0831 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 12, 2011
From: KIM, JONGHEE; JO, KIHOON; KIM, YOUNGHWAN; LEE, JEONGHE; LEE, YUNYONG; KIM, JINSUK; SEOK, JONGHEON
To: POSCO
Reel/Frame 026740/0453 →
Priority Claims (2)
KR 10-2008-0135141 · Dec 29, 2008 · national
KR 10-2009-0127397 · Dec 18, 2009 · national
Continuity (1)
Related Publication 20110294042A1 · Dec 1, 2011