# US 11,299,402 B2 · Precursor materials for li-ion battery cathode synthesis

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- Number: US 11,299,402 B2
- Document ID: US11299402B2
- Status: Granted
- Kind: B2
- Application number: 16/662,616
- Filed: 2019-10-24
- Published: 2021-04-29
- Granted: 2022-04-12
- Earliest claimed: 2019-10-24
- Assignees: CAMX Power LLC
- Applicants: CAMX Power LLC
- Inventors: Adrian W. Pullen; Suresh Sriramulu
- Web page: https://patentgrep.com/patent/US11299402B2

## CPC

- C01G 53/04: Oxides
- C01G 53/42: containing alkali metals, e.g. LiNiO2
- C01G 53/40: Complex oxides containing nickel and at least one other metal element
- H01B 1/08: oxides
- H01M 4/52: of nickel, cobalt or iron
- 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
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01P 2002/60: Compounds characterised by their crystallite size
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/82: by IR- or Raman-data
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- Y02E 60/10: Energy storage using batteries
- 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)
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- 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

## Abstract

Provided are particles for use as a precursor material for synthesis of Li-ion cathode active material of a lithium-ion cell comprising: a non-lithiated nickel oxide particle of the formula MOx wherein M comprises 80 at % Ni or greater and wherein x is 0.7 to 1.2, M optionally excluding boron in the MOx crystal structure; and a modifier oxide intermixed with, coated on, present within, or combinations thereof the non-lithiated nickel oxide particle, wherein the modifier oxide is associated with the non-lithiated nickel oxide such that a calcination at 500 degrees Celsius for 2 hours results in crystallite growth measured by XRD of 2 nanometers or less. Also provided are processes of forming electrochemically active particles using the precursors nickel oxides.

## Claims

### Claim 1

A particle for use as a precursor material for synthesis of Li-ion cathode active material of a lithium-ion cell comprising:
a non-lithiated nickel oxide particle of the formula MOx wherein M comprises 80 at % Ni or greater and wherein x is 0.7 to 1.2, M optionally excluding boron in the MOx crystal structure; and
boron oxide intermixed with, coated on, present within, or combinations thereof the non-lithiated nickel oxide particle, wherein the boron oxide is associated with the non-lithiated nickel oxide such that a calcination at 500 degrees Celsius for 2 hours results in crystallite growth measured by XRD of 2 nanometers or less.

### Claim 2 (depends on 1)

The particle of claim 1, wherein the nickel is present at 92 atomic percent or greater of total M.

### Claim 3 (depends on 1)

The particle of claim 1 wherein the nickel is present at 99 atomic percent or greater of total M.

### Claim 4 (depends on 1)

The particle of claim 1 wherein the boron oxide is present at less than 1 wt % relative to the non-lithiated nickel oxide particle.

### Claim 5 (depends on 4)

The particle of claim 4 wherein the boron oxide is present at 0.25 wt % or less.

### Claim 6 (depends on 1)

The particle of claim 1 wherein M comprises Ni and one or more elements of Mg, Sr, Co, Al, Ca, Cu, Zn, Mn, V, Ba, Zr, Ti, Nb, Ta, Cr, Fe, Mo, W, Hf, B, or any combination thereof.

### Claim 7 (depends on 1)

The particle of claim 1 wherein M comprises Ni and Co.

### Claim 8 (depends on 1)

The particle of claim 1 wherein the non-lithiated nickel oxide particle has an average crystallite size as measured by X-Ray Diffraction of less than 30 nm, optionally less than 25 nm, optionally less than 20 nm.

### Claim 9 (depends on 8)

The particle of claim 8 wherein Ni is present at 92 atomic percent or greater.

### Claim 10 (depends on 9)

The particle of claim 9 wherein M comprises Ni and one or more elements of Mg, Sr, Co, Al, Ca, Cu, Zn, Mn, V, Ba, Zr, Ti, Nb, Ta, Cr, Fe, Mo, W, Hf, B, or any combination thereof.

### Claim 11 (depends on 10)

The particle of claim 10 wherein the boron oxide is present at less than 1 wt % relative to the non-lithiated nickel oxide particle.

### Claim 12 (depends on 1)

The particle of claim 1 that is free of any component that is soluble in water at 1 atmosphere pressure and 25 degrees Celsius.