# US 2024/0204276 A1 · Eutectic synthesis for upcycling of cathode materials

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- Number: US 2024/0204276 A1
- Document ID: US20240204276A1
- Status: Published application
- Kind: A1
- Application number: 18/536,523
- Filed: 2023-12-12
- Published: 2024-06-20
- Earliest claimed: 2022-12-15
- Applicants: UT-Battelle, LLC
- Inventors: Jianlin Li; Mengya Li; William B. Hawley
- Web page: https://patentgrep.com/patent/US20240204276A1

## CPC

- H01M 10/54: Reclaiming serviceable parts of waste accumulators
- C01G 53/42: containing alkali metals, e.g. LiNiO2
- H01M 4/505: of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
- H01M 4/525: of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2006/40: Electric properties
- Y02E 60/10: Energy storage using batteries
- Y02W 30/84: Recycling of batteries or fuel cells
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

A method of upcycling cathode active materials is provided. The method includes mixing two or more precursor materials at ambient temperature to form a first eutectic mixture. The method further includes mixing a cathode active material with the first eutectic mixture to form a second eutectic mixture. The method further includes subjecting the second eutectic mixture to a two-step calcination process. The two-step calcination process includes first calcining the second eutectic mixture at a first temperature for a first period of time to obtain an intermediate material and second, calcining the intermediate material at a second temperature for a second period of time to obtain an upcycled cathode active material. The second temperature is higher than the first temperature, and the upcycled cathode active material has a composition that is different than a composition of the cathode active material. A cathode active material formed by the method is also provided.

## Claims

### Claim 1

A method of upcycling cathode active materials, the method comprising:
mixing two or more precursor materials at ambient temperature to form a first eutectic mixture;
mixing a cathode active material with the first eutectic mixture to form a second eutectic mixture;
subjecting the second eutectic mixture to a two-step calcination process, wherein the two-step calcination process includes first calcining the second eutectic mixture at a first temperature for a first period of time to obtain an intermediate material and second calcining the intermediate material at a second temperature for a second period of time to obtain an upcycled cathode active material, wherein the second temperature is higher than the first temperature, and wherein the upcycled cathode active material has a composition that is different than a composition of the cathode active material.

### Claim 2 (depends on 1)

The method of claim 1, wherein the first temperature is in a range of 300 to 400° C.

### Claim 3 (depends on 1)

The method of claim 1, wherein the second temperature is in a range of 700 to 1000° C.

### Claim 4 (depends on 1)

The method of claim 1, wherein the first period of time is at least 4 hours.

### Claim 5 (depends on 1)

The method of claim 1, wherein the second period of time is at least 8 hours.

### Claim 6 (depends on 1)

The method of claim 1, wherein the two-step calcination process further comprises an intermediate step of muddling the second eutectic mixture after the first calcining and before the second calcining.

### Claim 7 (depends on 1)

The method of claim 1, wherein the first calcining is performed in ambient air.

### Claim 8 (depends on 1)

The method of claim 1, wherein the second calcining is performed in the presence of an oxygen (02) stream.

### Claim 9 (depends on 1)

The method of claim 1, wherein the precursor materials include lithium hydroxide and nickel nitrate.

### Claim 10 (depends on 1)

The method of claim 1, further comprising the step of sieving the upcycled cathode active material after the second calcining.

### Claim 11 (depends on 1)

The method of claim 1, wherein the cathode active material is obtained from one of or both of a spent battery and cathode scrap from a cathode manufacturing process.

### Claim 12 (depends on 1)

The method of claim 1, wherein the cathode active material comprises a lithium-bearing metal oxide.

### Claim 13 (depends on 1)

The method of claim 1, wherein the upcycled cathode active material has a nickel content that is greater than a nickel content of the cathode active material.

### Claim 14 (depends on 1)

The method of claim 1, wherein the upcycled cathode active material: (i) comprises substantially the same morphology as the cathode active material; (ii) is directly reusable in the preparation of a new composite electrode; or (iii) both (i) and (ii).

### Claim 15 (depends on 1)

The method of claim 1, further comprising preparing a new composite electrode using the upcycled cathode active material.

### Claim 16 (depends on 15)

The method of claim 15, further comprising preparing a new lithium-ion battery using the new composite electrode.

### Claim 17 (depends on 1)

A cathode active material formed by the method of claim 1.