IP Library Granted Patent US 10,297,821
Granted Patent B2
US 10,297,821 · App. 15/273,825 · Granted May 21, 2019

Cathode-active materials, their precursors, and methods of forming

Inventors: Hongli Dai (Los Altos, CA); Christopher Johnson (Naperville, IL)
Assignee: Apple Inc.
H01M4/505C01G45/02C01G51/04C01G51/44C01G53/04C01G53/44H01M4/525C01P2004/03H01M2004/028
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Quick Facts
Patent No.
US 10,297,821
App. No.
15/273,825
Granted
May 21, 2019
Kind
B2
Abstract

Methods are presented for synthesizing a metal precursor for a cathode-active material. The methods include adding urea to a solution comprising dissolved ions of at least one transition metal selected from Mn, Co, and Ni. The methods also include increasing a pH of the aqueous solution to a threshold pH. The methods additionally include heating the aqueous solution to precipitate a compound that includes the at least one transition metal. Such heating may involve urea decomposition. Methods are also presented that include filtering the compound from the solution and contacting the compound with at least a lithium precursor to produce a reactant charge. In these methods, the reactant charge is calcined to produce the cathode-active material. Other methods are presented.

Claims (47)

1. A method for synthesizing a metal precursor for a cathode-active material, comprising:

adding urea to a solution comprising dissolved ions of at least one transition metal selected from Mn, Co, and Ni;

increasing a pH of the solution up to a pH at which seeds of a precipitate nucleate within the solution in which 99% of the urea is decomposed; and

at the pH, heating the solution to precipitate particles comprising the at least one transition metal.

2. The method of claim 1 , further comprising:

preparing the solution comprising at least one transition metal salt.

3. The method of claim 1 , wherein the solution is aqueous.

4. The method of claim 1 , wherein the pH is increased using a basic additive.

5. The method of claim 1 , wherein heating the solution comprises heating the solution to cause urea decomposition.

6. The method of claim 1 , wherein the at least one transition metal is a combination of Mn and Co.

7. A method for producing a cathode-active material comprising:

adding urea to a solution comprising dissolved ions of at least one transition metal selected from the Mn, Co, and Ni;

increasing a pH of the solution up to a pH at which seeds of a precipitate nucleate within the solution in which at least 99% of the urea is decomposed;

at the pH, heating the solution to cause urea decomposition;

precipitating particles comprising the at least one transition metal;

filtering the precipitated particles from the solution;

contacting the filtered particles with at least a lithium precursor to produce a reactant charge; and

calcining the reactant charge to produce the cathode-active material.

8. The method of claim 7 , further comprising:

preparing the solution using at least one transition metal salt.

9. The method of claim 7 , wherein filtering the precipitated particles comprises washing the precipitated particles.

10. The method of claim 9 , wherein the precipitated particles is are washed with at least deionized water.

11. The method of claim 7 , wherein filtering the precipitated particles comprises washing the precipitated particles and drying the precipitated particles.

12. The method of claim 11 , wherein the drying the precipitated particles comprises heating the precipitated particles.

13. The method of claim 7 , wherein the cathode-active material has a composition represented by LiMe 2 O 4 and wherein Me comprises Mn, Co, Ni, or any combination thereof.

14. The method of claim 7 ,

wherein the cathode-active material has a composition represented by Li 1+x Ni α Mn β Co γ M δ O 2 ;

wherein M is Mg, Zn, Al, Ga, B, Zr, Ti, or any combination thereof;

wherein 0≤x ≤0.4;

wherein 0 ≤α≤1;

wherein 0 ≤β≤1;

wherein 0 ≤γ≤1; and

wherein 0 ≤δ≤0.1.

15. The method of claim 14 , wherein the solution further comprises dissolved ions of Mg, Zn, Al, Ga, BO 3 , or any combination thereof.

16. The method of claim 14 , wherein the filtered particles are further contacted with a boron precursor, titanium precursor, a zirconium precursor, or any combination thereof, to produce the reactant charge.

17. A method for synthesizing a metal precursor for a cathode active material comprising:

adding urea to a solution comprising dissolved ions of Mn and Co;

increasing a pH of the solution up to a pH between 7.7 and 8.8;

heating the solution to a temperature below a boiling temperature of the solution to cause urea decomposition, thereby precipitating particles in the solution.

18. The method of claim 17 , further comprising:

preparing the solution using a manganese salt and a cobalt salt;

wherein the manganese salt and the cobalt salt are each selected from the group of salts consisting of chlorides, nitrates, sulfates, carbonates, oxalates, cyanates, thiocyanates, and acetates.

19. The method of claim 17 , wherein heating the solution comprises holding the solution at a temperature above 60° C.

20. The method of claim 17 , further comprising:

filtering the particles from the solution;

contacting the filtered particles with at least a lithium precursor to produce a reactant charge; and

calcining the reactant charge to produce the cathode-active material.

Assignments (4)
CONFIRMATORY LICENSE Recorded Jun 24, 2022
From: UCHICAGO ARGONNE, LLC
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 060302/0169 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2017
From: JOHNSON, CHRISTOPHER S.
To: UCHICAGO ARGONNE, LLC
Reel/Frame 042790/0131 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2017
From: UCHICAGO ARGONNE, LLC
To: APPLE INC.
Reel/Frame 042790/0165 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2017
From: DAI, HONGLI
To: APPLE INC.
Reel/Frame 042790/0287 →
Continuity (2)
Provisional Application 62235049 · Sep 30, 2015
Related Publication 20170092949A1 · Mar 30, 2017
Cited By (3)
US 12,206,097 US 12,206,100 US 12,249,707