IP Library Granted Patent US 9,947,947
Granted Patent B2
US 9,947,947 · App. 14/629,317 · Granted Apr 17, 2018

Mixed metal borohydrides

Inventors: Allison M. Fisher (Cocoa, FL); Brian Elliot Hayden (Lyndhurat, GB); Jean-Philipe Soulie (Southsea, GB)
Assignee: INTELLIGENT ENERGY INC.
H01M8/04216C01B6/23C01B35/00
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Quick Facts
Patent No.
US 9,947,947
App. No.
14/629,317
Granted
Apr 17, 2018
Kind
B2
Abstract

The invention relates to mixed metal borohydrides used for solid hydrogen storage. The mixed metal borohydrides are synthesized through solution synthesis using multiple metal borohydrides. First and second precursor solutions are prepared and combined to create a mixture in which the mixed metal borohydride is formed. The solvent is removed, leaving the mixed metal borohydride. The first precursor solution consisting essentially of lithium borohydride, and the second precursor solution consisting essentially of a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium.

Claims (52)

1. A method of producing a mixed metal borohydride comprising:

preparing a first precursor solution consisting essentially of a homometallic borohydride compound and a first solvent, the homometallic borohydride being lithium borohydride;

preparing a second precursor solution consisting essentially of a second solvent and a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium;

combining the first and second precursor solutions to create a mixture;

forming the mixed metal borohydride in the mixture by stirring the mixture at room temperature; and

removing the first solvent and the second solvent from the mixture containing the mixed metal borohydride to produce a solid mixed metal borohydride; and,

wherein the second precursor solution consists essentially of the second solvent and sodium borohydride and titanium borohydride and,

wherein the solid mixed metal borohydride is Li 3 Ti(BH 4 ) 6 .

2. The method of claim 1 , wherein the first solvent and the second solvent are the same.

3. The method of claim 1 , wherein the first solvent, the second solvent, or both is diethyl ether.

4. The method of claim 1 ,

wherein a third precursor solution is prepared consisting essentially of a third solvent and a third borohydride compound, the third borohydride compound being different from the borohydride compound in the second precursor solution and containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium, and

wherein the third precursor solution is combined with the first and second precursor solutions to create the mixture.

5. The method of claim 1 , wherein the second precursor solution consists essentially of the second solvent and one or more of sodium borohydride, magnesium borohydride, calcium borohydride and titanium borohydride.

6. The method of claim 1 , wherein the second precursor solution consists essentially of the second solvent and calcium borohydride.

7. The method of claim 1 , wherein the solvent is removed from the mixture in vacuo.

8. The method of claim 1 , wherein the steps of preparing the precursor solutions are done under argon at room temperature.

9. The method of claim 1 , wherein a majority of the solid mixed metal borohydride comprises nanoparticles.

10. The method of claim 1 , wherein the solid mixed metal borohydride is coated.

11. The method of claim 10 , wherein the solid mixed metal borohydride is coated with an inert material.

12. A method of producing a mixed metal borohydride comprising:

preparing a first precursor solution consisting essentially of a homometallic borohydride compound and a first solvent, the homometallic borohydride being lithium borohydride;

preparing a second precursor solution consisting essentially of a second solvent and a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium;

combining the first and second precursor solutions to create a mixture;

forming the mixed metal borohydride in the mixture by stirring the mixture at room temperature; and

removing the first solvent and the second solvent from the mixture containing the mixed metal borohydride to produce a solid mixed metal borohydride; and

wherein the second precursor solution consists essentially of the second solvent and sodium borohydride and titanium borohydride.

13. The method of claim 12 , wherein the solid mixed metal borohydride contains less than 5 atomic weight percent of titanium.

14. A method of producing a mixed metal borohydride comprising:

preparing a first precursor solution consisting essentially of a homometallic borohydride compound and a first solvent, the homometallic borohydride being lithium borohydride;

preparing a second precursor solution consisting essentially of a second solvent and a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium;

combining the first and second precursor solutions to create a mixture;

forming the mixed metal borohydride in the mixture by stirring the mixture at room temperature; and

removing the first solvent and the second solvent from the mixture containing the mixed metal borohydride to produce a solid mixed metal borohydride; and,

wherein the second precursor solution consists essentially of the second solvent and sodium borohydride, calcium borohydride and titanium borohydride.

15. The method of claim 14 , wherein the solid mixed metal borohydride contains less than 5 atomic weight percent of titanium.

16. A method of producing a mixed metal borohydride comprising:

preparing a first precursor solution consisting essentially of a homometallic borohydride compound and a first solvent, the homometallic borohydride being lithium borohydride;

preparing a second precursor solution consisting essentially of a second solvent and a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium;

combining the first and second precursor solutions to create a mixture;

forming the mixed metal borohydride in the mixture by stirring the mixture at room temperature; and

removing the first solvent and the second solvent from the mixture containing the mixed metal borohydride to produce a solid mixed metal borohydride;

wherein the second precursor solution consists essentially of the second solvent and magnesium borohydride; and,

wherein the solid mixed metal borohydride is Li 2 Mg(BH 4 ) 4 .

17. A method of producing a mixed metal borohydride comprising:

preparing a first precursor solution consisting essentially of a homometallic borohydride compound and a first solvent, the homometallic borohydride being lithium borohydride;

preparing a second precursor solution consisting essentially of a second solvent and a borohydride compound containing one or more metal cations selected from the group of metals consisting of sodium, magnesium, calcium and titanium;

combining the first and second precursor solutions to create a mixture;

forming the mixed metal borohydride in the mixture by stirring the mixture at room temperature; and

removing the first solvent and the second solvent from the mixture containing the mixed metal borohydride to produce a solid mixed metal borohydride;

wherein the second precursor solution consists essentially of the second solvent and magnesium borohydride; and,

wherein the solid mixed metal borohydride is Li 3 Mg(BH 4 ) 5 .

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 1, 2026
From: INTELLIGENT ENERGY, INC.
To: INTELLIGENT ENERGY LIMITED
Reel/Frame 075150/0416 →
Continuity (5)
Continuation PCTUS2013054478 · Aug 12, 2013
Provisional Application 61717172 · Oct 23, 2012
Provisional Application 61782443 · Mar 14, 2013
Provisional Application 61692390 · Aug 23, 2012
Related Publication 20150166336A1 · Jun 18, 2015