# US 12,767,535 B2 · Process of synthesizing cathode material

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- Number: US 12,767,535 B2
- Document ID: US12767535B2
- Status: Granted
- Kind: B2
- Application number: 18/395,423
- Filed: 2023-12-22
- Published: 2024-06-27
- Granted: 2026-10-20
- Earliest claimed: 2022-12-23
- Assignees: Boston Global Technologies, LLC
- Applicants: Boston Global Technologies Limited; HK Institute of Boston Global Technologies Limited
- Inventors: Boshan Mo; Guiqing Huang; Ming Yi; ChunJiao Meng; Xiaopeng Ding; Youde Mo
- Web page: https://patentgrep.com/patent/US12767535B2

## CPC

- C01B 25/45: containing plural metal, or metal and ammonium
- H01M 4/5825: {Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines}
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/84: one phase coated with the other
- C01P 2006/40: Electric properties
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention provides a novel process of synthesizing a cathode material. A metal selected from Fe, Mn, Co, Ni, Cu, Zn, Al, Ca, Mg, Ti, V, Cr, Mo or any combination thereof is partially oxidized with an agent such as H3PO4. Then, the metal is fully oxidized with an oxidizing agent such as H2O2. Finally, preparation of the cathode material is completed. The process exhibits numerous technical merits such as less water consumption, less electricity usage, improved product purity, and less usage of base raw materials (e.g. NaOH, Na2CO3, NH3·H2O), among others.

## Claims

### Claim 1

A process of synthesizing a target cathode material, comprising:
(i) mixing a P source containing element P with a first metal source containing one or more metal elements selected from Fe, Mn, Co, Ni, Cu, Zn, Al, Ca, Mg, Ti, V, Cr, Mo or any combination thereof, to form a first intermediate material, wherein a portion of at least one element among said one or more metal elements is oxidized;
(ii) mixing and reacting the first intermediate material with an oxidizing agent to oxidize a remaining portion of said at least one element among said one or more metal elements, to form a second intermediate material without any further processing; and
(iii) immediately after the second intermediate material is produced in step (ii), mixing it with one or more add-on source materials selected from a P source containing element P, a first metal source containing one or more metal elements selected from Fe, Mn, Co, Ni, Cu, Zn, Al, Ca, Mg, Ti, V, Cr, Mo or any combination thereof, and a second metal source containing one or more elements selected from Li, Na, K or any combination thereof;
wherein said one or more add-on source materials are introduced in an amount or amounts that are needed for accomplishing a formula of the target cathode material; and
wherein said steps (i), (ii) and (iii) are conducted in one single container.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the second intermediate material produced in step (ii) is not centrifuged and washed before it is mixed with said one or more add-on source materials is step (iii).

### Claim 3 (depends on 1)

The process according to claim 1, wherein said P source in step (i) and step (iii) is selected from H3PO4, a salt of H2PO4−, a salt of HPO42−, a salt of PO43−, or any combination thereof; and wherein said first metal source in step (i) comprises a metallic powder of Fe, Mn, Co, Ni, Cu, Zn, Al, Ca, Mg, Ti, V, Cr, Mo or any combination thereof.

### Claim 4 (depends on 1)

The process according to claim 1, wherein said P source in step (i) comprises 5-55% H3PO4; and
wherein said first metal source in step (i) comprises iron powder and/or Mn powder.

### Claim 5 (depends on 1)

The process according to claim 1, wherein said oxidizing agent in step (ii) is selected from O2, H2O2, HNO3, KMnO4, NaMnO4, or any combination thereof.

### Claim 6 (depends on 1)

The process according to claim 1, wherein step (i) further includes heating the reaction mixture in the container to an elevated temperature for 1-10 hours; and step (ii) further includes maintaining the reaction mixture in the container at an elevated temperature.

### Claim 7 (depends on 1)

The process according to claim 1, wherein said first metal source in step (iii) comprises a metal compound selected from oxides, hydrogen carbonates, hydrogen sulfates, hydrogen oxalates, carbonates, sulfates, and oxalates of Fe, Mn, Co, Ni, Cu, Zn, Al, Ca, Mg, Ti, V, Cr, Mo or any combination thereof.

### Claim 8 (depends on 1)

The process according to claim 1, wherein said first metal source in step (iii) comprises a metal compound selected from FeO, Fe2O3, Fe3O4, FeC2O4, MnO, Mn2O3, Mn3O4, MnCO3, MnO2, CoO, Co2O3, and Co3O4.

### Claim 9 (depends on 1)

The process according to claim 1, wherein said second metal source in step (iii) comprises a metal compound selected from oxides, hydroxides, carbonates, hydrogen carbonates, phosphates, hydrogen phosphates, dihydrogen phosphates, nitrates, oxalates and hydrogen oxalates of Li, Na, K or any combination thereof.

### Claim 10 (depends on 1)

The process according to claim 1, wherein said second metal source in step (iii) comprises a metal compound selected from Li2O, LiOH, Li2CO3, LiHCO3, Li3PO4, Li2HPO4, LiH2PO4, Li2C2O4, LiHC2O4, LiNO3, Na2O, NaOH, Na2CO3, NaHCO3, Na3PO4, Na2HPO4, NaH2PO4, Na2C2O4, NaHC2O4, K2O, KOH, K2CO3, KHCO3, K3PO4, K2HPO4, KH2PO4, K2C2O4, KHC2O4, NaNO3, KCH3CO2, KHCO2, and KNO3.

### Claim 11 (depends on 1)

The process according to claim 1, wherein said P source and said first metal source in step (iii) are combined into a composite source.

### Claim 12 (depends on 11)

The process according to claim 11, wherein the composite source is a mixture of compounds.

### Claim 13 (depends on 1)

The process according to claim 1, wherein said P source and said second metal source in step (iii) are combined into a composite source.

### Claim 14 (depends on 13)

The process according to claim 13, wherein the composite source is selected from Li3PO4, Na3PO4, K3PO4, Li2HPO4, Na2HPO4, K2HPO4, LiH2PO4, NaH2PO4, and KH2PO4.

### Claim 15 (depends on 1)

The process according to claim 1, wherein said first metal source and said second metal source in step (iii) are combined into a composite source.

### Claim 16 (depends on 15)

The process according to claim 15, wherein the composite source is selected from KMnO4 and NaMnO4.

### Claim 17 (depends on 1)

The process according to claim 1, wherein step (iii) further comprises mixing the second intermediate material with a C source material.

### Claim 18 (depends on 17)

The process according to claim 17, further comprising milling or grinding the product from step (iii) to cream-like particles having an average size of 300~400 nm after step (iii) is completed.

### Claim 19 (depends on 18)

The process according to claim 18, further comprising drying the cream-like particles to produce dry particles in a powder form.

### Claim 20 (depends on 19)

The process according to claim 19, further comprising calcining the dry particles into a solid, grinding the solid into ground particles, and sieving the ground particles to collect nanosized carbon-coated cathode materials.
