IP Library Granted Patent US 8,052,955
Granted Patent B2
US 8,052,955 · App. 12/912,506 · Granted Nov 8, 2011

Lithium-based materials and methods of forming the same

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Quick Facts
Patent No.
US 8,052,955
App. No.
12/912,506
Granted
Nov 8, 2011
Kind
B2
Abstract

Lithium-based materials and methods of forming the same. In at least one embodiment of a method of forming a lithium-based material of the present disclosure, the method comprises the steps of combining a first quantity of a first lithium-based component and a second quantity of a second lithium-based component with a titanium-based component to form a mixture, the first lithium-based component having a first melting point and the second lithium-based component having a second melting point higher than the first melting point of the first lithium-based component, and heating the mixture to a first temperature above the first melting point but below the second melting point for a period of time to form a resultant end product.

Claims (48)

1. A method of forming a lithium-based material, comprising the steps of:

combining a first quantity of a first lithium-based component and a second quantity of a second lithium-based component with a titanium-based component to form a mixture, the first lithium-based component having a first melting point and the second lithium-based component having a second melting point higher than the first melting point of the first lithium-based component; and

heating the mixture to a first temperature above the first melting point but below the second melting point for a period of time to form a resultant end product;

wherein the resultant end product comprises a lithium titanate having the formula:

Li 4 Ti 5 O 12-x

wherein x is greater than 0 and less than 12.

2. The method of claim 1 , further comprising the step of:

cooling the a resultant end product.

3. The method of claim 1 , wherein the first lithium-based component comprises lithium hydroxide and wherein the second lithium-based component comprises lithium carbonate.

4. The method of claim 3 , wherein the first quantity of lithium hydroxide is greater than the second quantity of lithium carbonate.

5. The method of claim 1 , wherein the first lithium-based component and the second lithium-based component are selected from the group consisting of lithium carbonate, lithium hydroxide, lithium oxide, and combinations thereof.

6. The method of claim 1 , wherein the titanium-based component is selected from the group consisting of titanium oxide and titanium dioxide.

7. The method of claim 1 , wherein the first lithium-based component comprises lithium hydroxide, and wherein the first temperature is above about 450° C. but below about 726° C.

8. The method of claim 1 , wherein the resultant end product is formed by way of a liquid-solid reaction between the first lithium-based component and the titanium-based component and by way of a solid-solid reaction between the second lithium-based component and the titanium-based component.

9. The method of claim 8 , wherein the liquid-solid reaction occurs at a faster rate than the solid-solid reaction.

10. The method of claim 1 , wherein the combining step is performed in a ceramic reactor, and wherein the heating step is performed in a muffle furnace.

11. The method of claim 1 , wherein the resultant end product comprises a lithium titanate.

12. A method of forming a lithium-based material, comprising the steps of:

combining a first quantity of a first lithium-based component and a second quantity of a second lithium-based component with a titanium-based component to form a mixture, the first lithium-based component having a first melting point and the second lithium-based component having a second melting point higher than the first melting point of the first lithium-based component;

heating the mixture to a first temperature below the first melting point and the second melting point and maintaining the mixture at the first temperature;

heating the mixture to a second temperature above the first melting point but below the second melting point and maintaining the mixture at the second temperature; and

heating the mixture to a third temperature above the first melting point and the second melting point and maintaining the mixture at the third temperature to form a resultant end product;

wherein the resultant end product comprises a lithium titanate having the formula:

Li 4 Ti 5 O 12-x

wherein x is greater than 0 and less than 12.

13. The method of claim 12 , further comprising the step of:

cooling the a resultant end product.

14. The method of claim 12 , wherein the first lithium-based component comprises lithium hydroxide and wherein the second lithium-based component comprises lithium carbonate.

15. The method of claim 14 , wherein the first quantity of lithium hydroxide is greater than the second quantity of lithium carbonate.

16. The method of claim 12 , wherein the first lithium-based component and the second lithium-based component are selected from the group consisting of lithium carbonate, lithium hydroxide, lithium oxide, and combinations thereof.

17. The method of claim 12 , wherein the titanium-based component is selected from the group consisting of titanium oxide and titanium dioxide.

18. The method of claim 12 , wherein the first temperature is below 450° C., the second temperature is between about 450° C. but below about 726° C., and wherein the third temperature is above 726° C.

19. The method of claim 18 , wherein the first temperature is about 150° C., and wherein the second temperature is about 950° C.

20. The method of claim 12 , wherein each of the heating steps include maintaining the mixture at the stated temperature for a period of time of about two hours.

21. A method of forming a lithium-based material, comprising the steps of:

combining a first quantity of lithium hydroxide component and a second quantity of lithium carbonate with a titanium-based component to form a mixture;

heating the mixture to a first temperature above a melting point of the lithium hydroxide but below a melting point of the lithium carbonate and maintaining the mixture at the first temperature; and

heating the mixture to a second temperature above the melting point of the lithium carbonate and maintaining the mixture at the second temperature to form a lithium titanate having the formula:

Li 4 Ti 5 O 12-x

wherein x is greater than 0 and less than 12.

22. The method of claim 12 , wherein the resultant end product is formed by way of a liquid-solid reaction between the first lithium-based component and the titanium-based component and by way of a liquid-solid reaction between the second lithium-based component and the titanium-based component.

23. The method of claim 12 , wherein the resultant end product comprises a lithium titanate.

24. A method of forming a lithium titanate having the following formula:

Li 4 Ti 5 O 12-x

wherein x is greater than 0 and less than 12, said method comprising the steps of:

providing a mixture of titanium oxide and a lithium-based component such that the lithium-based component and the titanium oxide are present in the provided mixture in amounts necessary to ensure an atomic ratio of lithium to titanium of 0.8, wherein the lithium-based component is selected from the group of a synthetic product, lithium carbonate powder and lithium hydroxide powder;

utilizing the provided mixture as a precursor for calcination; and,

sintering the mixture in a gaseous atmosphere comprising a reducing agent to form the lithium titanate.

Assignments (4)
PATENT SECURITY AGREEMENT Recorded Apr 5, 2012
From: ENER1, INC.; ENERDEL, INC.; ENERFUEL, INC.; NANOENER, INC.
To: WILMINGTON TRUST, NATIONAL ASSOCIATION
Reel/Frame 027999/0516 →
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENTS Recorded Apr 3, 2012
From: BZINFIN, S.A.
To: ENER1, INC.; ENERDEL, INC.; ENERFUEL, INC.; NANO ENER, INC.
Reel/Frame 027982/0854 →
SECURITY AGREEMENT Recorded Dec 13, 2011
From: ENERDEL, INC.; ENERFUEL, INC.; ENER1, INC.; NANOENER, INC.
To: BZINFIN S.A.
Reel/Frame 027370/0979 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 23, 2011
From: GORSHKOV, VADIM; VOLKOV, OLEG
To: ENERDEL, INC.
Reel/Frame 026957/0205 →