# US 12,006,228 B2 · Preparation method for high density aluminum doped cobalt oxide

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- Number: US 12,006,228 B2
- Document ID: US12006228B2
- Status: Granted
- Kind: B2
- Application number: 17/842,761
- Filed: 2022-06-16
- Published: 2022-10-06
- Granted: 2024-06-11
- Earliest claimed: 2019-12-17
- Assignees: Gem (Jiangsu) Cobalt Industry Co., Ltd.
- Applicants: GEM (Jiangsu) Cobalt Industry Co., Ltd.
- Inventors: Kaihua Xu; Zhenkang Jiang; Aiqing Zhang; Bingzhong Li; Chao Wang; Dongwei Xu
- Web page: https://patentgrep.com/patent/US12006228B2

## CPC

- C01G 51/04: Oxides
- 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 2002/54: one element only
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/74: by peak-intensities or a ratio thereof only
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2006/11: Powder tap density
- C01P 2006/12: Surface area
- C01P 2006/40: Electric properties
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- 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)
- 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

The present invention discloses a preparation method for high density aluminum doped cobalt oxide, which comprises following steps: 1) adding a cobalt salt solution, an alkaline solution and an oxidizer to a reactor for reaction; adding an aluminum cobalt solution to the reaction system for reaction; stopping adding the aluminum cobalt solution after D50 reaches 3.5-4.0 μm, stopping the reaction when D50 reaches the desired particle size, thus obtaining aluminiferous cobalt oxyhydroxide slurry; 2) aging, dehydrating, washing and drying the aluminiferous cobalt oxyhydroxide slurry, thus obtaining aluminiferous cobalt oxyhydroxide powder; 3) calcining the aluminiferous cobalt oxyhydroxide powder, thus obtaining the target object. With the method of the present invention, doped aluminum can be perfectly embedded into cobalt oxide lattices, thus effectively enhancing the tap density and uniformity of aluminum doped cobalt oxide and improving the cycle performance and charge-discharge performance of batteries.

## Claims

### Claim 1

A preparation method for high density aluminum doped cobalt oxide, comprising following steps:
step 1: adding a cobalt salt solution, an alkaline solution and an oxidizer to a reactor for coprecipitation reaction and obtain precipitation products; adding an aluminum cobalt solution to reaction system for reaction after the precipitation products' D50 reaches 2.0-2.5 μm; and stopping adding the aluminum cobalt solution after the precipitation products' D50 reaches 3.5-4.0 μm, keeping other conditions unchanged, continuing the reaction, and stopping the reaction when the precipitation products' D50 reaches a desired particle size, thus obtaining aluminiferous cobalt oxyhydroxide slurry;
step 2: aging, dehydrating, washing and drying the aluminiferous cobalt oxyhydroxide slurry obtained in step 1, thus obtaining aluminiferous cobalt oxyhydroxide powder; and
step 3: calcining the aluminiferous cobalt oxyhydroxide powder obtained in step 2, thus obtaining high density aluminum doped cobalt oxide.

### Claim 2 (depends on 1)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 1, wherein in step 1, a specific method of stopping adding the aluminum cobalt solution after the precipitation products' D50 reaches 3.5-4.0 μm, keeping other conditions unchanged, continuing the reaction, and stopping the reaction when D50 reaches the desired particle size is as follows:
after the precipitation products' D50 reaches 3.5-4.0 μm, stopping adding the aluminum cobalt solution and continuing adding the cobalt salt solution; after liquid in the reactor overflows, thickening the overflowing slurry, draining supernatant, returning the thick slurry to the reactor to continue reaction, and stopping the reaction when D50 reaches the desired particle size.

### Claim 3 (depends on 2)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 2, wherein in step 1, the feed rate of the cobalt salt solution is 220-260 L/h, the feed rate of the alkaline solution is 50-150 L/h, the feed rate of the oxidizer is 20-30 L/h, and the stirring rate during feeding is 300-600 rpm.

### Claim 4 (depends on 3)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 3, wherein in step 1, the concentration of cobalt ions in the cobalt salt solution is 120-140 g/L, the concentration of the alkaline solution is 80-150 g/L, and the oxidizer is one of air, oxygen or hydrogen peroxide.

### Claim 5 (depends on 4)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 4, wherein in step 1, the concentration of cobalt in the aluminum cobalt solution is 120-140 g/L, and the concentration ratio of cobalt ions to aluminum ions in the aluminum cobalt solution is 100:0.5-1.

### Claim 6 (depends on 5)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 5, wherein the cobalt salt solution and the aluminum cobalt solution both contain a complexing agent, and the concentration ratio of cobalt ions to the complexing agent in the cobalt salt solution is 0.04-0.1; and the concentration ratio of cobalt ions to the complexing agent in the aluminum cobalt solution is 0.04-0.1.

### Claim 7 (depends on 6)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 6, wherein in step 1, the reactor contains a base solution with the pH value of 9-11.

### Claim 8 (depends on 7)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 7, wherein in step 2, deionized water of 80-90° C. is used for washing, and the drying temperature is 120-180° C.

### Claim 9 (depends on 8)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 8, wherein in step 3, the calcining temperature is 500-750° C., and the calcining time is 10-20 h.

### Claim 10 (depends on 1)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 1, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 11 (depends on 2)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 2, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 12 (depends on 3)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 3, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 13 (depends on 4)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 4, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 14 (depends on 5)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 5, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 15 (depends on 6)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 6, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 16 (depends on 7)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 7, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 17 (depends on 8)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 8, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.

### Claim 18 (depends on 9)

The preparation method for high density aluminum doped cobalt oxide as claimed in claim 9, further comprising a step of washing and drying the high density aluminum doped cobalt oxide obtained in step 3.