Size and morphologically controlled nanostructures for energy storage

Patent metadata

Field	Value
Publication number	US-9586822-B2
Application number	US-201214348772-A
Country	US
Kind code	B2
Filing date	Oct 10, 2012
Priority date	Oct 10, 2011
Publication date	Mar 7, 2017
Grant date	Mar 7, 2017

Abstract

The disclosure relates to a process to synthesize nanostructures of a uniform size distribution and/or morphology, nanostructures resulting therefrom, and the use of the nanostructures in energy storage devices.

First claim

What is claimed is:

1. A method of synthesizing size and/or morphologically controlled nanostructures comprising mixing a first metal salt solution comprising a first metal salt and polyvinyl pyrrolidone in degassed water and triethylene glycol (TEG) with a second metal salt solution comprising a second metal salt and polyvinyl pyrrolidone in aqueous TEG and heating a reaction mixture comprising the first metal salt solution and comprising the second metal salt solution at room temperature or greater for at least 2 hours.

2. The method of claim 1 , further comprising, adjusting the pH of the solution comprising the first metal salt by adding either an acid or base, adjusting the pH of the solution comprising the second metal salt by adding either an acid or base and/or adjusting the pH of the reaction mixture by adding either an acid or base.

3. The method of claim 1 , wherein the first metal salt comprises a transition metal.

4. The method of claim 3 , wherein the transition metal is selected from the group consisting of manganese, iron, titanium, zinc, copper, cobalt and nickel.

5. The method of claim 4 , wherein the transition metal is iron.

6. The method of claim 1 , wherein the first metal salt comprises a first polyatomic anion.

7. The method of claim 6 , wherein the first polyatomic anion is selected from the group consisting of phosphate, sulfate, nitrate, molybdate, oxalates, chlorate, and carbonate.

8. The method of claim 7 , wherein the first polyatomic anion is sulfate.

9. The method of claim 1 , wherein the first metal salt is dissolved in one or more polar solvents.

10. The method of claim 1 , wherein the second metal salt comprises lithium.

11. The method of claim 1 , wherein the second metal salt comprises a second polyatomic anion.

12. The method of claim 11 , wherein the second polyatomic anion is selected from the group consisting of hydroxide, perchlorate, carbonate, diethyl carbonate, tetrafluoroborate, hexaflourophosphate, and triflate.

13. The method of claim 12 , wherein the second polyatomic anion is hydroxide.

14. The method of claim 1 , wherein the second metal salt is dissolved in one or more polar solvents.

15. The method of claim 1 , wherein the concentration of the first metal salt is equal to the concentration of the second metal salt.

16. The method of claim 1 , wherein the concentration of the first metal salt is greater than the concentration of the second metal salt.

17. The method of claim 1 , wherein the concentration of the first metal salt is less than the concentration of the second metal salt.

18. The method of claim 17 , wherein the concentration of the first metal salt is at least three times less than the concentration of the second metal salt.

19. The method of claim 2 , wherein the pH of the solution comprising the first metal salt, the pH of the solution of comprising the second metal salt, and/or the pH of the reaction mixture, is adjusted with either nonaqueous or aqueous acid.

20. The method of claim 19 , wherein the pH of the solution comprising the first metal salt is adjusted with nonaqueous polyprotic acid.

21. The method of claim 20 , wherein the nonaqueous polyprotic acid is phosphoric acid.

22. The method of claim 19 , wherein the pH of the reaction mixture is adjusted with aqueous polyprotic acid.

23. The method of claim 22 , wherein the aqueous polyprotic acid is aqueous sulfuric acid.

24. The method of claim 1 , wherein the reaction mixture is heated at room temperature or greater for at least 2 hours in a sealed reactor.

25. The method of claim 24 , wherein the reaction mixture is heated at 50° C. or greater for at least 2 hours in a sealed reactor.

26. The method of claim 25 , wherein the reaction mixture is heated at 100° C. or greater in a sealed reactor.

27. The method of claim 26 , wherein the reaction mixture is heated at 150° C. or greater for at least 2 hours in a sealed reactor.

28. The method of claim 27 , wherein the reaction mixture is heated at a temperature between 150° C. to 200° C. for 2 to 12 hours in a sealed reactor.

29. The method of claim 1 , wherein the method produces nanostructures that have a uniform size distribution.

30. The method of claim 29 , wherein the nanostructures have diameters of less than 100 nm.

31. The method of claim 1 , wherein the method produces nanostructures that have a uniform morphology.

32. The method of claim 31 , where the morphology is selected from the group consisting of nanoparticles, nanobelts, nanocubes, and nanoprisms.

Assignees

• Univ California

Inventors

• Kisailus David
• Zhu Jianxin

Classifications

• Y02E60/122

  Cross-Sectional Technologies · mapped topic

• C01B25/45 Primary

  containing plural metal, or metal and ammonium · CPC title

• H01M4/5825

  Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines · CPC title

• H01M10/0525

  Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries · CPC title

• H01M4/139

  Processes of manufacture · CPC title