Alkali metal silicate, alkali transition metal silicate, and method for synthesizing silicate

Patent metadata

Field	Value
Publication number	US-9472805-B2
Application number	US-201213595000-A
Country	US
Kind code	B2
Filing date	Aug 27, 2012
Priority date	Sep 1, 2011
Publication date	Oct 18, 2016
Grant date	Oct 18, 2016

Abstract

A method for synthesizing alkali metal silicate which can be easily microparticulated, a method for synthesizing, with the use of the alkali metal silicate, alkali transition metal silicate, and alkali metal silicate and alkali transition metal silicate which are synthesized by the synthesis methods are disclosed. The alkali metal silicate is synthesized by the following steps: forming a basic solution including an alkali metal salt; mixing the basic solution including the alkali metal salt with silicon particles to form a basic solution including the alkali metal silicate; and adding the basic solution including the alkali metal silicate to a poor solvent for the alkali metal silicate to precipitate the alkali metal silicate. Further, the alkali metal silicate is mixed with a microparticulated compound including a transition metal to form a mixture, and the mixture is subjected to heat treatment, whereby the alkali transition metal silicate is generated.

First claim

The invention claimed is:

1. A method for synthesizing a silicate microparticle, comprising the steps of:
adding dropwise of a first solution including alkali metal silicate to a second solution to precipitate the alkali metal silicate under stirring the second solution or under application of ultrasonic waves to the second solution,
wherein a solubility of the alkali metal silicate of the second solution is lower than a solubility of the alkali metal silicate of the first solution,
wherein a silicon atoms molar concentration of the first solution is higher than or equal to 0.1 mol/l and lower than or equal to 0.5 mol/l,
wherein a rate at which the dropwise of the first solution is added to the second solution is higher than or equal to 40 ml/h and lower than or equal to 80 ml/h, and
wherein a solvent of the second solution has affinity for a solvent of the first solution.

2. The method for synthesizing the silicate microparticle, according to claim 1 , further comprising the steps of:
collecting the precipitated alkali metal silicate; and
performing heat treatment on the collected alkali metal silicate.

3. The method for synthesizing the silicate microparticle, according to claim 1 , wherein the first solution including the alkali metal silicate is formed by dissolving silicon into a solution including an alkali metal salt of pH of 9 or more.

4. The method for synthesizing the silicate microparticle, according to claim 3 , wherein the first solution including the alkali metal salt is kept at a temperature of higher than or equal to 50° C. and lower than or equal to 70° C.

5. The method for synthesizing the silicate microparticle, according to claim 3 , wherein the first solution including the alkali metal salt is an alkali metal hydroxide aqueous solution.

6. The method for synthesizing the silicate microparticle, according to claim 1 , wherein the solvent of the second solution is ethanol.

7. The method for synthesizing the silicate microparticle, according to of claim 1 , wherein the alkali metal is lithium.

8. The method for synthesizing the silicate microparticle, according to claim 1 , further comprising the steps of:
mixing the precipitated alkali metal silicate with a microparticulated compound including a transition metal to form a mixture; and
performing heat treatment on the mixture to generate alkali transition metal silicate.

9. The method for synthesizing the silicate microparticle, according to claim 2 , further comprising the steps of:
mixing the alkali metal silicate subjected to the heat treatment with a microparticulated compound including a transition metal to form a mixture; and
performing second heat treatment on the mixture to generate alkali transition metal silicate.

10. The method for synthesizing the silicate microparticle, according to claim 8 , wherein the transition metal is manganese.

11. The method for synthesizing the silicate microparticle, according to claim 8 , wherein the microparticulated compound including the transition metal is a carbonate.

12. The method for synthesizing the silicate microparticle, according to claim 9 , wherein the transition metal is manganese.

13. The method for synthesizing the silicate microparticle, according to claim 9 , wherein the microparticulated compound including the transition metal is a carbonate.

14. The method for synthesizing the silicate microparticle, according to claim 8 , wherein the heat treatment performed on the mixture is performed under an inert gas atmosphere at a temperature of higher than or equal to 700° C. and lower than or equal to 1000° C.

15. The method for synthesizing the silicate microparticle, according to claim 9 , wherein the second heat treatment performed on the mixture is performed under an inert gas atmosphere at a temperature of higher than or equal to 700° C. and lower than or equal to 1000° C.

16. The method for synthesizing the silicate microparticle, according to claim 8 , wherein a specific surface area of the generated alkali transition metal silicate, measured by gas adsorption, is greater than or equal to 50 m 2 /g and less than or equal to 150 m 2 /g.

17. A method for manufacturing an electrode, comprising the steps of:
adding dropwise of a first solution including alkali metal silicate to a second solution to precipitate the alkali metal silicate under stirring the second solution or under application of ultrasonic waves to the second solution,
mixing the precipitated alkali metal silicate with a microparticulated compound including a transition metal to form a mixture;
performing heat treatment on the mixture to generate alkali transition metal silicate;
making a slurry by mixing the alkali transition metal silicate, a binder, and a conductive auxiliary agent;
putting the slurry on a current collector; and
drying the slurry on the current collector,
wherein a solubility of the alkali metal silicate of the second solution is lower than a solubility of alkali metal silicate of the first solution,
wherein a silicon atoms molar concentration of the first solution is higher than or equal to 0.1 mol/l and lower than or equal to 0.5 mol/l,
wherein a rate at which the dropwise of the first solution is added to the second solution is higher than or equal to 40 ml/h and lower than or equal to 80 ml/h, and
wherein a solvent of the second solution has affinity for a solvent of the first solution.

18. The method for synthesizing the silicate, according to claim 17 , further comprising the steps of:
collecting the precipitated alkali metal silicate; and
performing heat treatment on the collected alkali metal silicate.

19. The method for synthesizing the silicate, according to claim 17 , wherein the first solution including the alkali metal silicate is formed by dissolving silicon into a solution including an alkali metal salt of pH of 9 or more.

20. The method for synthesizing the silicate, according to claim 19 , wherein the first solution including the alkali metal salt is kept at a temperature of higher than or equal to 50° C. and lower than or equal to 70° C.

21. The method for synthesizing the silicate, according to claim 19 ,
wherein the first solution including the alkali metal salt is an alkali metal hydroxide aqueous solution.

22. The method for synthesizing the silicate, according to claim 17 ,
wherein the second solution is ethanol.

23. The method for synthesizing the silicate, according to of claim 17 ,
wherein the alkali metal is lithium.

24. The method for synthesizing the silicate, according to claim 17 , wherein the transition metal is manganese.

25. The method for synthesizing the silicate, according to claim 17 , wherein the microparticulated compound including the transition metal is a carbonate.

26. The method for synthesizing the silicate, according to claim 17 , wherein the heat treatment performed on the mixture is performed under an inert gas atmosphere at a temperature of higher than or equal to 700° C. and lower than or equal to 1000° C.

27. The method for synthesizing the silicate, according to claim 17 , wherein a specific surface area of the generated alkali transition metal silicate, measured by gas adsorption, is greater than or equal to 50 m 2 /g and less than or equal to 150 m 2 /g.

Assignees

• Motoyoshi Mako
• Kawakami Takahiro
• Yamakaji Masaki
• Semiconductor Energy Lab

Inventors

• Motoyoshi Mako
• Kawakami Takahiro
• Yamakaji Masaki

Classifications

• H01M4/5825 Primary

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

• C01P2006/12

  Surface area · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01B33/32

  Alkali metal silicates ({C01B33/24} , C01B33/26 take precedence) · CPC title