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Method for producing electrocatalyst

Foreign code F110005741
File No. P04-010US
Posted date Sep 13, 2011
Country United States of America
Application number 66450605
Gazette No. 20080280753
Gazette No. 8491697
Date of filing Oct 6, 2005
Gazette Date Nov 13, 2008
Gazette Date Jul 23, 2013
International application number JP2005018558
International publication number WO2006038676
Date of international filing Oct 6, 2005
Date of international publication Apr 13, 2006
Priority data
  • P2004-294165 (Oct 6, 2004) JP
  • 2005WO-JP18558 (Oct 6, 2005) WO
Title Method for producing electrocatalyst
Abstract (US8491697)
[Problem]To provide a method for producing an electrocatalyst having no compositional scatter, wherein nano-level alloy catalyst molecules with an ordered particle size are supported in a highly dispersed state. [Means of Solution] The method includes the steps of preparing a reverse micelle solution by mixing two or more catalyst precursors selected from among metal salts and/or metal complexes, a solvent having hydrophilic groups and a non-aqueous solvent, forming alloy particles in the reverse micelle by adding a non-aqueous solution having a reducing action to the reverse micelle and heating, and supporting the alloy particles on a carrier.
Scope of claims [claim1]
1. A method for producing an electrocatalyst, comprising the steps of: preparing a reverse micelle solution by mixing two or more catalyst precursors selected from among metal salts and/or metal complexes, a solvent having hydrophilic groups and a non-aqueous solvent, in a state that the two or more catalyst precursors are mixed uniformly and enclosed together in single reverse micelles in the single reverse micelle solution; and
forming alloy particles from the two or more catalyst precursors selected from among metal salts and/or metal complexes in the reverse micelles by adding a reducing agent solution comprising LiB(C2H5)3H to said reverse micelle solution and heating to promote a reduction reaction;
after heating to promote the reduction reaction, treating the reverse micelles surrounding the alloy particles with a solvent comprising a lower alcohol to partially remove the reverse micelles;
uniformly supporting said alloy particles from which the reverse micelles are partially removed on a carrier; and
removing components of the reverse micelles from the alloy particles by heating the alloy particles supported uniformly on the carrier under an inert gas.
[claim2]
2. The method for producing an electrocatalyst according to claim 1, wherein said metal salt and metal complex contain a salt of a noble metal and base metal, and a metal complex of a noble metal and base metal.
[claim3]
3. The method for producing an electrocatalyst according to claim 2, wherein the noble metal contains platinum, palladium, rhodium, iridium, ruthenium or gold, the base metal is at least one metal selected from the group consisting of iron, tin, nickel, cobalt, manganese, chromium, vanadium, titanium, niobium, molybdenum, lead, and tungsten and the metal complex is at least one moiety selected from the group consisting of an amine complex, ethylene diamine complex and acetyl acetonate complex.
[claim4]
4. The method for producing an electrocatalyst according to claim 1, wherein said solvent having hydrophilic groups is a higher alcohol.
[claim5]
5. The method for producing an electrocatalyst according to claim 1, wherein said non-aqueous solvent is a higher ether.
[claim6]
6. The method for producing an electrocatalyst according to claim 1, wherein, in the step for preparing the reverse micelle solution, a higher aliphatic carboxylic acid and a higher aliphatic amine are mixed therewith.
[claim7]
7. The method for producing an electrocatalyst according to claim 1, wherein, in the step of forming the alloy particles from the two or more catalyst precursors selected from among metal salts and/or metal complexes in the reverse micelle by adding the reducing agent solution comprising LiB(C2H5)3H to said reverse micelle solution and heating to promote the reduction reaction, the heating temperature when promoting the reduction reaction is within a range of 200 deg. C. to 300 deg. C.
[claim8]
8. The method for producing an electrocatalyst according to claim 1, wherein the heating of alloy particles supported on the carrier to remove components of the reverse micelles therefrom is performed at 100 deg. C. to 400 deg. C.
[claim9]
9. The method for producing an electrocatalyst according to claim 1, wherein, in the step of preparing the reverse micelle solution, mixing the two or more catalyst precursors selected from among metal salts and/or metal complexes in a desired ratio in the single reverse micelle solution causes a compositional ratio of the alloy particles formed in the reverse micelle to correspond to a mixing ratio of the two or more catalyst precursors mixed in the single reverse micelle solution.
[claim10]
10. A method for producing an electrocatalyst, comprising the steps of: preparing a reverse micelle solution containing a carrier by mixing two or more catalyst precursors of metal salts and/or metal complexes, a solvent having hydrophilic groups, a non-aqueous solvent and the carrier, in a state that the two or more catalyst precursors are mixed uniformly and enclosed together in single reverse micelles in the single reverse micelle solution;
forming alloy particles from the two or more catalyst precursors selected from among metal salts and/or metal complexes in the reverse micelles by adding a reducing agent solution comprising LiB(C2H5)3H to said reverse micelle solution and heating to promote a reduction reaction, and uniformly supporting the alloy particles surrounded by the reverse micelles on the carrier; and
removing components of the reverse micelles from the alloy particles by heating the alloy particles supported uniformly on the carrier under an inert gas.
[claim11]
11. The method for producing an electrocatalyst according to claim 10, wherein said metal salt and metal complex contain a salt of a noble metal and base metal, and a metal complex of a noble metal and base metal.
[claim12]
12. The method for producing an electrocatalyst according to claim 11, wherein the noble metal contains platinum, palladium, rhodium, iridium, ruthenium or gold, the base metal is at least one metal selected from the group consisting of iron, tin, nickel, cobalt, manganese chromium, vanadium, titanium, niobium, molybdenum, lead and tungsten, and the metal complex is at least one moiety selected from the group consisting of an amine complex, ethylene diamine complex and acetyl acetonate complex.
[claim13]
13. The method for producing an electrocatalyst according to claim 10, wherein said solvent having hydrophilic groups is a higher alcohol.
[claim14]
14. The method for producing an electrocatalyst according to claim 10, wherein said non-aqueous solvent is a higher ether.
[claim15]
15. The method for producing an electrocatalyst according to claim 10, wherein, in the step for preparing the reverse micelle solution, a higher aliphatic carboxylic acid and a higher aliphatic amine are mixed therewith.
[claim16]
16. The method for producing an electrocatalyst according to claim 10, wherein, in the step of forming the alloy particles from the two or more catalyst precursors selected from among metal salts and/or metal complexes in the reverse micelle by adding the reducing agent solution comprising LiB(C2H5)3H to said reverse micelle solution and heating to promote the reduction reaction, the heating temperature when promoting the reduction reaction is within a range of 200 deg. C. to 300 deg. C.
[claim17]
17. The method for producing an electrocatalyst according to claim 10, wherein the heating of the alloy particles supported on the carrier to remove components of the reverse micelles therefrom is performed at 100 deg. C. to 400 deg. C.
[claim18]
18. A method for producing an electrocatalyst, comprising: preparing a reverse micelle solution by mixing two or more catalyst precursors selected from among metal salts and/or metal complexes, a solvent having hydrophilic groups and a non-aqueous solvent, in a state that the two or more catalyst precursors are mixed uniformly and enclosed together in single reverse micelles in the single reverse micelle solution;
forming alloy particles from the two or more catalyst precursors selected from among metal salts and/or metal complexes in the reverse micelles by adding a reducing agent solution comprising LiB(C2H5)3H to said reverse micelle solution and heating at 200 deg. C. to 300 deg. C. to promote a reduction reaction; and
after heating to promote the reduction reaction, separating and washing a deposit containing the alloy particles by mixing a solvent comprising a lower alcohol with the reverse micelles surrounding the alloy particles, and partially removing the components of the reverse micelles by redispersing the deposit in an organic solvent;
uniformly supporting said alloy particles from which the components of the reverse micelles are partially removed on a carrier; and
after the alloy particles are supported uniformly on the carrier, removing components of the remaining reverse micelles from the alloy particles by heating at 100 deg. C. to 400 deg. C. under an inert gas.
  • Inventor, and Inventor/Applicant
  • WATANABE MASAHIRO
  • UCHIDA HIROYUKI
  • YAMANASHI UNIVERSITY
IPC(International Patent Classification)
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