IP Library Granted Patent US 10,137,435
Granted Patent B2
US 10,137,435 · App. 14/390,550 · Granted Nov 27, 2018

Method for preparing a catalyst mediating H

Inventors: Vincent Artero (Quaix en Chartreuse, FR); Marc Fontecave (Saint Ismier, FR); Saioa Cobo (San Sebastian, ES); Pierre-Andre Jacques (Sainte Consorce, FR); Holger Dau (Berlin, DE); Jonathan Heidkamp (Mohorn, DE)
Assignees: COMMISSARIAT A L'ENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES; UNIVERSITE JOSEPH FOURIER
B01J23/75B01J23/755B01J31/16C25B1/02C25B11/0442C25B11/0478C25D3/12C25D5/006C25D7/12C25D9/08C25D9/10C25D9/12H01M4/8657H01M4/9016H01M4/9041H01M4/9075H01M4/9083B01J31/182B01J31/1805B01J31/1835B01J35/0013B01J37/16B01J37/345B01J37/348B01J2531/0244B01J2531/0247B01J2531/845B01J2531/847B01J2540/10B82Y30/00B82Y40/00Y02P20/135
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Quick Facts
Patent No.
US 10,137,435
App. No.
14/390,550
Granted
Nov 27, 2018
Kind
B2
Abstract

The present invention concerns a method for the preparation of a catalyst onto a solid support of a (semi-)conductive material consisting in depositing said catalyst onto said support from a near-neutral aqueous solution containing at least one nickel or cobalt organic complex and at least one basic oxoanion, by a method selected in the group consisting of reductive electrodeposition, photochemical electrodeposition and photoelectrochemical deposition. The present invention also concerns said catalyst and uses thereof.

Claims (20)

1. A method for the preparation of a catalyst onto a solid support of a conductive or semiconductive material, the method comprising:

depositing said catalyst onto said solid support from a near-neutral aqueous solution containing at least one nickel or cobalt organic complex and at least one basic oxoanion, using a method selected from the group consisting of reductive electrodeposition, photochemical electrodeposition, and photoelectrochemical deposition,

wherein the catalyst consists of elemental cobalt/nickel covered or coated by a cobalt/nickel oxo/hydroxo-oxoanion layer.

2. The method according to claim 1 , wherein the conductive or semiconductive material of said solid support is selected from the group consisting of a metallic material, a carbon material, a semiconductor or conductor metal oxide, nitride, and chalcogenide.

3. The method according to claim 1 , wherein the conductive or semiconductive material of said solid support is selected from the group consisting of silicon, brass, stainless steel, iron, copper, nickel, cobalt, aluminium, silver, gold, titanium, carbon black, single or multi-walled carbon nanotubes (CNT), fullerenic nanoparticles, graphite, glassy carbon, graphene, reduced graphene oxide, doped diamond, TiO 2 , NiO, ZnO, ZrO 2 , ITO, SnO 2 , WO 3 , Fe 2 O 3 , BiVO 4 , Ta 2 O 5 , Ta 3 N 5 , TaON, ZnS, ZnSe, CdS, CdSe, CdTe, ZnTe, and composites of these materials, possibly doped with other elements.

4. The method according to claim 1 , wherein the near-neutral aqueous solution has a pH of between 5 and 9.

5. The method according to claim 1 , wherein the near-neutral aqueous solution has a pH of between 6 and 8.

6. The method according to claim 1 , wherein the near-neutral aqueous solution has a pH of between 6.3 and 7.7.

7. The method according to claim 1 , wherein the near-neutral aqueous solution has a pH of between 6.5 and 7.5.

8. The method according to claim 1 , wherein the near-neutral aqueous solution has a pH of between 6.7 and 7.3.

9. The method according to claim 1 , wherein the near-neutral solution is an aqueous solution having a pH of 7.

10. The method according to claim 1 , wherein said cobalt or nickel organic complex is selected from the group consisting of cobalt or nickel dioxime/diimine complex; and cobalt or nickel amine/imine/pyridine complex.

11. The method according to claim 1 , wherein said cobalt or nickel organic complex is selected from the group consisting of [Co(DO)(DOH)pnCl 2 ] with (DOH)(DOH)pn representing N 2 ,N 2 ′-propanediylbis(2,3-butandione 2-imine 3-oxime); [Co(DO)(DOH)pnBr 2 ]; [Co((DO) 2 BF 2 )pnBr 2 ] with ((DO) 2 BF 2 )pn representing N 2 ,N 2 ′-propanediylbis(2,3-butandione 2-imine 3-oximato)-N 1 ,N 1′ -difluoroboryl [Co(MO)(MOH)pnCl 2 ] with (MOH)(MOH)pn representing N 2 ,N 2 ′-propanediylbis(1,2-propandione 2-imine 1-oxime); [Ni((CO) 2 BF 2 )pn](ClO 4 ); [Co(dmgBF 2 ) 2 (H 2 O) 2 ] with dmgH 2 representing dimethylglyoxime; [Co(dmgH) 2 pyCl]; [Co(dmgH) 2 (OH 2 ) 2 ]; [Co(dmgBF 2 ) 2 (DMF) 2 ]; [Co(dmgBF 2 ) 2 (CH 3 CN) 2 ]; [Co(dpgBF 2 ) 2 (H 2 O) 2 ] with dpgH 2 representing diphenylglyoxime; [Co(dpgBF 2 ) 2 (DMF) 2 ]; [Co(dpgBF 2 ) 2 (CH 3 CN) 2 ]; [Ni(dmgBF 2 ) 2 ]; [Ni(dmgH) 2 ] [Ni(DO)(DOH)pn](ClO 4 ); [Ni(MO)(MOH)pnCl]; [Ni((DO) 2 BF 2 )pn](ClO 4 ); [Co(DO)(DOH)pnBr(PPh 3 )]; [Co(DO)(DOH)pn(PPh 3 )]; [Co(dmg) 3 (BF) 2 ] + ; [Co(dpg) 3 (BF) 2 ] + ; [Co(dmg) 3 (BPh) 2 ] 0/1+ and [Co(dpg) 3 (BPh) 2 ] 0/1+ .

12. The method according to claim 1 , wherein said basic oxoanion is selected from the group consisting of a phosphate, carbonate, arsenate, borate, vanadate, chromate, phosphonate, phosphite, nitrate, nitrite, sulphate, sulphonate, molybdate, and tungstate.

13. The method according to claim 1 , wherein the reductive electrodeposition comprises applying to said solid support a potential below −0.4 V versus Ag/AgCl.

14. The method according to claim 1 , wherein the reductive electrodeposition comprises applying to said solid support a potential below −0.6 V versus Ag/AgCl.

15. The method according to claim 1 , wherein the reductive electrodeposition comprises applying to said solid support a potential below −0.8 V versus Ag/AgCl.

16. The method according to claim 1 , wherein the reductive electrodeposition comprises applying to said solid support a potential of about −1 V versus Ag/AgCl.

17. A method for mediating hydrogen evolution comprising implementing the catalyst obtained by the preparation method according to claim 1 .

18. The method according to claim 3 , wherein the conductive or semiconductive material is doped with one or n ore elements other than said selected material.

Assignments (3)
CORRECTIVE ASSIGNMENT TO CORRECT THE SIXTH INVENTORS' LAST NAME. PREVIOUSLY RECORDED ON REEL 034966 FRAME 0714. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT OF ASSIGNORS INTEREST.. Recorded May 17, 2017
From: ARTERO, VINCENT; FONTECAVE, MARC; COBO, SAIOA; JACQUES, PIERRE-ANDRE; DAU, HOLGER; HEIDKAMP, JONATHAN
To: COMMISSARIAT A L'ENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES; FREIE UNIVERSITAT BERLIN
Reel/Frame 042569/0703 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 12, 2015
From: FREIE UNIVERSITAT BERLIN
To: UNIVERSITE JOSEPH FOURIER
Reel/Frame 036772/0797 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 16, 2015
From: ARTERO, VINCENT; FONTECAVE, MARC; COBO, SAIOA; JACQUES, PIERRE-ANDRE; DAU, HOLGER; HEDIKAMP, JONATHAN
To: COMMISSARIAT A L'ENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES; FREIE UNIVERSITAT BERLIN
Reel/Frame 034966/0714 →
Priority Claims (1)
EP 12352001 · Apr 5, 2012 · regional
Continuity (1)
Related Publication 20150090604A1 · Apr 2, 2015
Cited By (2)
US 12,247,281 US 12,480,196