Method for preparing a titanium and niobium mixed oxide by solvothermal treatment; electrode and lithium accumulator comprising said mixed oxide

Patent metadata

Field	Value
Publication number	US-9559357-B2
Application number	US-201514666620-A
Country	US
Kind code	B2
Filing date	Mar 24, 2015
Priority date	Oct 17, 2012
Publication date	Jan 31, 2017
Grant date	Jan 31, 2017

Abstract

A method of preparing a titanium and niobium mixed oxide including the steps of: preparing a titanium and niobium mixed oxide in amorphous form by a solvothermal treatment of at least one titanium precursor and of at least one niobium precursor, mechanically crushing the titanium and niobium mixed oxide obtained at the end of the solvothermal treatment and calcinating the mixed oxide obtained after crushing.

First claim

The invention claimed is:

1. A method of preparing a titanium and niobium mixed oxide comprising the steps of:
preparing a titanium and niobium mixed oxide in amorphous form by a solvothermal treatment of at least one titanium precursor and of at least one niobium precursor;
mechanically crushing the titanium and niobium mixed oxide obtained at the end of the solvothermal treatment; and
calcinating the mixed oxide obtained after crushing.

2. The method of preparing a titanium and niobium mixed oxide of claim 1 , wherein the solvothermal treatment of the titanium and niobium precursors is performed at a temperature in the range from 200 to 250° C.

3. The method of preparing a titanium and niobium mixed oxide of claim 1 , wherein the mixed oxide in amorphous form is washed prior to the calcination step.

4. The method of preparing a titanium and niobium mixed oxide of claim 1 , wherein the calcination step is carried out at a temperature in the range from 700 to 1,200° C.

5. The method of preparing a titanium and niobium mixed oxide of claim 1 , wherein the titanium precursor is selected from the group comprising titanium oxysulfate (TiOSO 4 ); titanium isopropoxide (Ti(OCH(CH 3 ) 2 ) 4 ); titanium chloride (TiCl 4 ); titanium butoxide (Ti(OC 4 H 9 ) 4 ).

6. The method of preparing a titanium and niobium mixed oxide of claim 1 , wherein the niobium precursor is selected from the group comprising niobium chloride (NbCl 5 ); niobium ethoxide, Nb(OC 2 H 5 ) 5 .

7. A titanium and niobium mixed oxide obtained according to the method of claim 1 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

8. The titanium and niobium mixed oxide of claim 7 , wherein the mixed oxide has formula Ti X Nb 2y O (2X+5y) , wherein x is in the range from 1 to 2 and y is in the range from 1 to 12.

9. An electrode having its active material comprising at least one titanium and niobium mixed oxide of claim 7 .

10. A negative electrode having its active material comprising at least one titanium and niobium mixed oxide of claim 7 .

11. A lithium accumulator containing at least one electrode having its active material comprising at least one titanium and niobium mixed oxide of claim 7 .

12. A titanium and niobium mixed oxide obtained according to the method of claim 2 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

13. A titanium and niobium mixed oxide obtained according to the method of claim 3 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

14. A titanium and niobium mixed oxide obtained according to the method of claim 4 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

15. A titanium and niobium mixed oxide obtained according to the method of claim 5 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

16. A titanium and niobium mixed oxide obtained according to the method of claim 6 , wherein the mixed oxide has a specific surface in the range from 5 m 2 /g to 45 m 2 /g.

Assignees

• Commissariat Energie Atomique

Inventors

• Buannic Lucienne
• Colin Jean-François
• Daniel Lise

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• C01P2004/53

  bimodal size distribution · CPC title

• C01G33/00

  Compounds of niobium · CPC title

• H01M2220/30

  Batteries in portable systems, e.g. mobile phone, laptop · CPC title

• C01P2004/03

  obtained by SEM · CPC title