US 11,929,502 B2
Stabilized lithium metal oxide electrode material and method of preparation
Albert L. Lipson, Forest Park, IL (US); and Jessica L. Durham, Frankfort, IL (US)
Assigned to UCHICAGO ARGONNE, LLC, Chicago, IL (US)
Filed by UCHICAGO ARGONNE, LLC, Chicago, IL (US)
Filed on Apr. 12, 2023, as Appl. No. 18/133,925.
Application 18/133,925 is a division of application No. 16/877,925, filed on May 19, 2020, granted, now 11,658,298.
Prior Publication US 2023/0268502 A1, Aug. 24, 2023
Int. Cl. H01M 4/525 (2010.01); H01M 4/04 (2006.01); H01M 4/36 (2006.01); H01M 10/0525 (2010.01); H01M 10/0568 (2010.01); H01M 10/0569 (2010.01); H01M 50/40 (2021.01)
CPC H01M 4/525 (2013.01) [H01M 4/0471 (2013.01); H01M 4/366 (2013.01); H01M 10/0525 (2013.01); H01M 10/0568 (2013.01); H01M 10/0569 (2013.01); H01M 50/40 (2021.01); H01M 2300/002 (2013.01)] 20 Claims
OG exemplary drawing
 
1. A method for preparing a stabilized layered lithium metal oxide material comprising the sequential steps of:
(a) continuously adding an alkali metal hydroxide solution, an aqueous ammonium hydroxide solution and an aqueous solution of metal salts comprising a nickel salt, a manganese salt, a cobalt salt, or a combination of two or more thereof, to a stirring reactor at a temperature of about 25 to 60° C., at hydroxide addition rates sufficient to maintain a constant pH of greater than or equal to 11 in the reactor, thereby coprecipitating metal hydroxide core precursor particles; and halting the additions of the solutions when the average particle size of the core precursor particles reaches a selected target size;
(b) continuously adding an aqueous coating solution comprising a manganese salt, a cobalt salt, or a combination thereof, to a stirring slurry of the core precursor particles formed in step (a) without addition of any hydroxide and without controlling the pH, at a temperature of about 25 to 60° C.; thereby coprecipitating cobalt and manganese hydroxide on the surface and interior of the core precursor particles to form coated precursor particles; and halting addition of the coating solution when the pH drops by a selected target level of about 0.1 to 1 pH units;
(c) recovering the coated precursor particles;
(d) mixing the recovered coated precursor particles with at least one molar equivalent of lithium hydroxide relative to the total moles of metal hydroxide in the coated precursor particles to produce a precursor mixture; and
(e) calcining the precursor mixture from step (d) at a temperature in the range of about 725 to 900° C. for about 4 to 50 hours, to form the stabilized lithium metal oxide material.