# US 2019/0375651 A1 · Process for Producing Lithiated Transition Metal Oxides

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- Number: US 2019/0375651 A1
- Document ID: US20190375651A1
- Status: Published application
- Kind: A1
- Application number: 16/000,931
- Filed: 2018-06-06
- Published: 2019-12-12
- Earliest claimed: 2018-06-06
- Assignees: BASF SE
- Applicants: BASF Corporation
- Inventors: William C. Mays; Diana F. Wong; Xue Liu; Benjamin Reichman; Martin Panchula; Gary Yacobian
- Web page: https://patentgrep.com/patent/US20190375651A1

## CPC

- C01D 15/02: Oxides; Hydroxides
- C01G 53/42: containing alkali metals, e.g. LiNiO2
- 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
- C01P 2004/50: Agglomerated particles
- C01P 2004/60: Particles characterised by their size
- C01P 2006/10: Solid density
- C01P 2006/11: Powder tap density
- C01P 2006/14: Pore volume
- Y02E 60/10: Energy storage using batteries
- C01D: COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides C01B17/22; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia and cyanogen, containing nitrogen and other non-metals C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; phosphides 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; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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)
- 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
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Provided are processes for the formation of electrochemically active materials such as lithiated transition metal oxides that solve prior issues with throughput and calcination. The processes include forming precursor materials into agglomerates prior to calcination. The use of the agglomerates improves gas flow into and out of the materials thereby improving calcination results, electrochemical properties of the resulting materials, and allows for use of high temperature kilns not previously suitable for such materials thereby lowering production costs.

## Claims

### Claim 1

A process for the formation of a lithiated transition metal oxide comprising:
intermixing a transition metal precursor and a lithium compound to form an active material precursor;
forming an agglomerate of the active material precursor by mixing the active material precursor with an agglomeration agent; and
heating the agglomerate to a temperature of 700° C. or greater in an oxidizing atmosphere, the heating for a calcination time sufficient to form a lithiated transition metal oxide.

### Claim 2 (depends on 1)

The process of claim 1 wherein the agglomeration agent comprises a saccharide, carboxymethyl cellulose, hydroxypropyl methylcellulose, hydroxypropyl cellulose, water, polyethylene glycol, polyvinylpyrrolidone, starch, molasses, or combinations thereof.

### Claim 3 (depends on 1)

The process of claim 1 wherein the agglomerate has a granule size of 500 μm or greater.

### Claim 4 (depends on 1)

The process of claim 1 wherein the agglomerate has a granule size of 500 μm to 15 mm.

### Claim 5 (depends on 1)

The process of claim 1 wherein the active material precursor further comprises a dry binder, an alkali-containing compound, a pore-forming compound, or combinations thereof.

### Claim 6 (depends on 1)

The process of claim 1 wherein the molar ratio of lithium to transition metal in the active material precursor is 0.8 to 1.1.

### Claim 7 (depends on 1)

The process of claim 1 wherein the agglomeration agent is present at 0.5 weight percent to 55 weight percent.

### Claim 8 (depends on 1)

The process of claim 1 wherein the transition metal precursor comprises Ni, Co, Mn, Al, Mg, Ti, Zr, Nb, Hf, V, Cr, Sn, Cu, Mo, W, Fe, Si, B, other transition metals, or rare earth elements.

### Claim 9 (depends on 1)

The process of claim 1 wherein the lithium compound is selected from the group consisting of lithium hydroxide, lithium oxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium acetate, lithium peroxide, lithium hydrogen carbonate, a lithium halide, and combinations thereof.

### Claim 10 (depends on 1)

The process of claim 1 wherein the active material precursor further comprises a pore former selected from the group consisting of a cellulose fiber, carbon, graphite, starch, polyether ether ketone, wood flour, a super absorbent, and combinations thereof.

### Claim 11 (depends on 1)

The process of claim 1 further comprising crushing the lithiated transition metal oxide.

### Claim 12 (depends on 1)

The process of claim 1 wherein the step of heating is within a belt furnace, vertical calciner, or grate kiln.

### Claim 13 (depends on 1)

The process of claim 1 wherein the oxidixing atmosphere is an oxygen enriched atmosphere.

### Claim 14 (depends on 1)

The process of claim 1 wherein the agglomerate has a tap density of 0.4 to 1.7.

### Claim 15 (depends on 1)

The process of claim 1 wherein the agglomerate has a bulk porosity of 50% to 95%.

### Claim 16 (depends on 1)

The process of claim 1 wherein the agglomerate has a pore volume fraction of 20% or greater.

### Claim 17 (depends on 1)

The process of claim 1 wherein the temperature is 700° C. to 1000° C.

### Claim 18 (depends on 1)

The process of claim 1 wherein the time is 1 to 60 hours.

### Claim 19

A process for the formation of a lithiated transition metal oxide comprising:
intermixing a nickel containing material and a lithium compound to form an active material precursor;
forming a plurality of agglomerates of the active material precursor by mixing the active material precursor with an agglomeration agent, the agglomerates having an average granule size of 500 μm to 8 mm; and
heating the agglomerate to a temperature of 700° C. or greater in an oxidizing atmosphere, the heating for a calcination time sufficient to form a lithiated transition metal oxide.

### Claim 20 (depends on 19)

The process of claim 19 wherein the nickel containing material comprises nickel monoxide, nickel hydroxide, nickel oxyhydroxide, nickel sesquioxide, nickel carbonate, nickel nitrate, or any combination thereof.

### Claim 21 (depends on 19)

The process of claim 19 wherein the nickel containing material further comprises Al, Co, Mn, or combinations thereof.

### Claim 22 (depends on 19)

The process of claim 19 wherein the lithium compound is selected from the group consisting of lithium hydroxide, lithium oxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium acetate, lithium peroxide, lithium hydrogen carbonate, a lithium halide, or combinations thereof.

### Claim 23 (depends on 19)

The process of claim 19 wherein the agglomeration agent is carboxymethyl cellulose, hydroxypropyl methylcellulose, hydroxypropyl cellulose, water, polyethylene glycol, polyvinylpyrrolidone, corn starch, or molasses.

### Claim 24 (depends on 23)

The process of claim 23 wherein the agglomeration agent is present at 0.5 weight percent to 35 weight percent of the agglomerate as a whole.

### Claim 25 (depends on 19)

The process of claim 19 wherein the active material precursor further comprises a pore forming agent.

### Claim 26 (depends on 19)

The process of claim 19 wherein the step of heating is within a belt furnace, vertical calciner, or grate kiln.