IP Library Granted Patent US 7,553,464
Granted Patent B2
US 7,553,464 · App. 10/914,362 · Granted Jun 30, 2009

Lanthanum tantalate photocatalysts

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Quick Facts
Patent No.
US 7,553,464
App. No.
10/914,362
Granted
Jun 30, 2009
Kind
B2
Abstract

A substantially pure phase LaTaO 4 photocatalyst is prepared by grinding precursors with mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls to a very fine particle size and calcining the ground precursors. The LaTaO 4 photocatalyst prepared by this method is useful in photolysis of water.

Claims (27)

1. A method of preparing a lanthanum tantalum material, comprising steps of

grinding a lanthanum compound and a tantalum compound with a mixture of at least two different sizes of high density yttrium-stabilized zirconia balls and

then calcining together the ground compounds to produce the lanthanum tantalum material, wherein the lanthanum tantalum material comprises a substantially pure phase LaTaO 4 .

2. A method according to claim 1 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least two sizes of yttrium-stabilized zirconia balls having a ratio of diameters of from about 1.5:1 to about 5:1.

3. A method according to claim 1 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least two sizes of yttrium-stabilized zirconia balls having a ratio of diameters of from about 1.5:1 to about 2.5:1.

4. A method according to claim 1 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least three sizes of zirconia balls.

5. A method according to claim 1 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least three sizes of yttrium-stabilized zirconia balls, in which the ratio of diameters of at least two of the sizes is from about 1.5:1 to about 2.5:1.

6. A method according to claim 1 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least a fraction of yttrium-stabilized zirconia balls having a first bead size with diameter of from about 8 mm to about 12 mm.

7. A method according to claim 6 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least a fraction of yttrium-stabilized zirconia balls having a second bead size with diameter of from about 2 mm to about 6 mm.

8. A method according to claim 7 , wherein the mixture of at least two different sizes of high-density yttrium-stabilized zirconia balls comprises at least a fraction of yttrium-stabilized zirconia balls having a third bead size of from about one-half to about one-fifth the diameter of the second bead size.

9. A method according to claim 1 , wherein the grinding step is carried out on a slurry of the compounds in a liquid selected from the group consisting of water and alcohols.

10. A method according to claim 1 , wherein the grinding step is carried out on a slurry of the compounds in a liquid selected from the group consisting of water, ethanol isopropanol, n-propanol, isobutanol, n-butanol, tert-butanol, ethylene glycol, diethylene glycol, an ethylene glycol monoalkyl ether, a propylene glycol monoalkyl ether, cyclohexanol, glycerol, lower molecular weight polyethylene glycols, sec-butanol, and combinations thereof.

11. A method according to claim 9 , wherein the step of grinding a mixture of precursor compounds is carried out in the presence of a protonic acid material.

12. A method according to claim 11 , wherein the protonic acid material comprises a member selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, boric acid, phosphoric acid, propionic acid, trifluoracetic acid, acetic acid, lactic acid, oxalic acid, phosphonic acid, methanesulfonic acid, ethanesulfonic acid, p-toluenesulfonic acid, dodecylbenzenesulfonic acid, citric acid, maleic acid, butyric acid, glycolic acid, phytic acid, formic acid, benzoic acid, acrylic acid, methacrylic acid, and combinations thereof.

13. A method according to claim 11 , wherein the protonic acid material comprises a member selected from the group consisting of nitric acid, acetic acid, and combinations thereof.

14. A method according to claim 11 , wherein the protonic acid material is included in an amount of about 0.1% to about 5% by volume liquid.

15. A method according to claim 1 , wherein the step of calcining together the ground compounds is carried out at a temperature in the range of about 1023 K to about 1223 K.

16. A method according to claim 1 , wherein the step of calcining together the ground compounds is carried out at a temperature in the range of about 1073 K to about 1173 K.

17. A method according to claim 1 , comprising a further step of adding a co-catalyst metal to the lanthanum tantalum material.

18. A method according to claim 17 , wherein the step of adding a co-catalyst is carried out by incipient wetness impregnation of the calcined lanthanum tantalum material with a soluble salt of the co-catalyst metal followed by calcining the impregnated material.

19. A method according to claim 18 , wherein the co-catalyst metal is a member selected from the group consisting of nickel, strontium, lanthanum, potassium, and barium.

20. A method according to claim 18 , wherein the co-catalyst metal is a member selected from the group consisting of alkali metals, alkaline earth metals, and transition metals.

21. A photocatalyst prepared according to the method of claim 18 , wherein the photocatalyst is a Sr/LaTaO 4 having a photocatalytic activity for water splitting of at least about 3000 micromoles hydrogen per gram catalyst per hour.

22. A process of water splitting, comprising a step of exposing the water to actinic radiation in the presence of a photocatalyst prepared according to the method of claim 1 .

23. A process of water splitting, comprising a step of exposing the water to actinic radiation in the presence of a photocatalyst prepared according to the method of claim 11 .

24. A process of water splitting, comprising a step of exposing the water to actinic radiation in the presence of a photocatalyst prepared according to the method of claim 16 .

25. A process of water splitting, comprising a step of exposing the water to actinic radiation in the presence of a photocatalyst prepared according to the method of claim 19 .

Assignments (13)
RELEASE OF SECURITY INTEREST Recorded Nov 7, 2014
From: WILMINGTON TRUST COMPANY
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 034371/0676 →
CHANGE OF NAME Recorded Feb 10, 2011
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: GM GLOBAL TECHNOLOGY OPERATIONS LLC
Reel/Frame 025780/0936 →
SECURITY AGREEMENT Recorded Nov 8, 2010
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: WILMINGTON TRUST COMPANY
Reel/Frame 025327/0001 →
RELEASE OF SECURITY INTEREST Recorded Nov 4, 2010
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025245/0442 →
RELEASE OF SECURITY INTEREST Recorded Nov 4, 2010
From: UAW RETIREE MEDICAL BENEFITS TRUST
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 025311/0770 →
SECURITY AGREEMENT Recorded Aug 28, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UAW RETIREE MEDICAL BENEFITS TRUST
Reel/Frame 023162/0001 →
SECURITY AGREEMENT Recorded Aug 27, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 023156/0052 →
RELEASE OF SECURITY INTEREST Recorded Aug 21, 2009
From: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023127/0468 →
RELEASE OF SECURITY INTEREST Recorded Aug 20, 2009
From: UNITED STATES DEPARTMENT OF THE TREASURY
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 023124/0429 →
SECURITY AGREEMENT Recorded Apr 16, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: CITICORP USA, INC. AS AGENT FOR BANK PRIORITY SECURED PARTIES; CITICORP USA, INC. AS AGENT FOR HEDGE PRIORITY SECURED PARTIES
Reel/Frame 022553/0446 →
SECURITY AGREEMENT Recorded Feb 4, 2009
From: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
To: UNITED STATES DEPARTMENT OF THE TREASURY
Reel/Frame 022201/0610 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 14, 2009
From: GENERAL MOTORS CORPORATION
To: GM GLOBAL TECHNOLOGY OPERATIONS, INC.
Reel/Frame 022102/0533 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 5, 2004
From: KIM, JIN D.; LI, WEI; OH, SE H.
To: GENERAL MOTORS CORPORATION
Reel/Frame 015343/0790 →