Process for making cathode materials for lithium ion batteries

Patent metadata

Field	Value
Publication number	US-10468678-B2
Application number	US-201515318887-A
Country	US
Kind code	B2
Filing date	Jun 19, 2015
Priority date	Jun 30, 2014
Publication date	Nov 5, 2019
Grant date	Nov 5, 2019

Abstract

Process for making a particulate material of general formula (I), wherein the integers are defined as follows: M is selected from Al and Ti, x is in the range of from 0.015 to 0.03, a is in the range of from 0.3 to 0.6, b is in the range of from 0.05 to 0.35, c is in the range of from 0.2 to 0.5, d is in the range of from 0.001 to 0.03, with a+b+c+d=1 said process comprising the following steps: (a) co-precipitating a mixed hydroxide of nickel, cobalt and manganese from a solution of water-soluble salts of nickel, cobalt and manganese by contacting such solution with a solution of alkali metal hydroxide, (b) adding an aqueous solution of an aluminate or titanate and thereby co-precipitating a layer of a mixed hydroxide of nickel and cobalt and manganese and aluminum or titanium on the particles formed in step (a), (c) removing particles of (Nia Cob Mnc Ald)(OH)2+d or (Nia Cob Mnc Tid)(OH)2+2d so obtained and drying them in the presence of oxygen, (d) mixing the particles obtained in step (c) with at least one Li compound selected from Li2O, LiOH and Li2CO3, (e) calcining the mixture obtained according to step (d) at a temperature in the range of from 920 to 950° C.

First claim

The invention claimed is:

1. A process for making a particulate material of general formula (I):
Li 1+x (Ni a Co b Mn c M d ) 1−x O 2   (I),

wherein:
x is in the range of from 0.015 to 0.03,
a is in the range of from 0.3 to 0.6,
b is in the range of from 0.05 to 0.35,
c is in the range of from 0.2 to 0.5,
d is in the range of from 0.001 to 0.03, and
a+b+c+d=1,

said process comprising:
(a) co-precipitating a mixed hydroxide of nickel, cobalt and manganese from a solution of water-soluble salts of nickel, cobalt and manganese by contacting such solution with a solution of alkali metal hydroxide;
(b) adding an aqueous solution of an aluminate and thereby co-precipitating a layer of a mixed hydroxide of nickel and cobalt and manganese and aluminium on the particles formed in step (a);
(c) removing particles of (Ni a Co b Mn c Al d )(OH) 2+d so obtained and drying them in the presence of oxygen;
(d) mixing the particles obtained in step (c) with at least one Li compound selected from Li 2 O, LiOH and Li 2 CO 3 ; and
(e) calcining the mixture obtained according to step (d) at a temperature in the range of from 920 to 950° C.

2. The process of to claim 1 , wherein step (e) is performed in an oxygen-containing atmosphere.

3. The process of claim 1 , wherein in formula (I):
b is in the range of from 0.15 to 0.25,
c is in the range of from 0.2 to 0.35,
d is in the range of from 0.01 to 0.03, and
a+b+c+d=1.

4. The process of claim 1 , wherein the duration of step (e) is in the range of from 3 to 12 hours.

5. The process of claim 1 , further comprising, between steps (d) and (e) at least one pre-calcining step (e*) comprising:
(e*) heating the mixture obtained in step (d) at a temperature in the range of from 300 to 700° C. for a period of 2 to 24 hours,
and performing step (e) with the material obtained in step(s) (e*).

6. The process according to claim 1 , wherein said co-precipitating (a) is performed at a temperature in the range of from 10 to 85° C.

7. The process according to claim 1 , wherein said co-precipitating (a) is performed at a pH value in the range of from 8 to 12.

8. The process according to claim 5 , wherein the process comprises two precalcinations that include
heating the mixture obtained in (d) at a temperature in the range of from 300 to 400° C. for a period of 2 to 12 hours; and
subsequently heating the material so obtained at a temperature in the range of from 500 to 700° C. for a period of 2 to 12 hours.

Assignees

• Basf Se

Inventors

• Volkov Aleksei
• Lampert Jordan
• Ryll Thomas Michael
• Shin Ji-Yong
• Hoelzle Markus
• Eder Michael

Classifications

• C01P2004/32

  Spheres · CPC title

• C01P2006/12

  Surface area · CPC title

• H01M10/052

  Li-accumulators · CPC title

• H01M4/131

  Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title