US 12,448,703 B2
Continuous hydrothermal manufacturing method for concentration-gradient monocrystalline battery material
YoungHo Shin, LaGrange Highlands, IL (US)
Assigned to UCHICAGO ARGONNE, LLC, Chicago, IL (US)
Filed by UCHICAGO ARGONNE, LLC, Chicago, IL (US)
Filed on Feb. 8, 2021, as Appl. No. 17/170,057.
Prior Publication US 2022/0251728 A1, Aug. 11, 2022
Int. Cl. C30B 29/22 (2006.01); C01D 15/02 (2006.01); C01G 53/44 (2025.01); C01G 53/50 (2025.01); C01G 53/82 (2025.01); H01M 4/505 (2010.01); H01M 4/525 (2010.01); H01M 10/0525 (2010.01); H01M 4/02 (2006.01)
CPC C30B 29/22 (2013.01) [C01D 15/02 (2013.01); C01G 53/44 (2013.01); C01G 53/50 (2013.01); C01G 53/82 (2025.01); H01M 4/505 (2013.01); H01M 4/525 (2013.01); H01M 10/0525 (2013.01); C01P 2004/80 (2013.01); C01P 2004/84 (2013.01); H01M 2004/021 (2013.01)] 13 Claims
OG exemplary drawing
 
1. A continuous method for preparing monocrystalline material, the method comprising:
a) supplying an aqueous metal salt solution and a lithium-containing basic aqueous solution having chelating agents, wherein both solutions are maintained separately at ambient temperature;
b) mixing the aqueous metal salt solution and the basic aqueous solution together using supercritical water, wherein the mixing occurs in a structure defining a central mixing axis, wherein the mixing is performed by injecting the supercritical water tangential to the central mixing axis to create a vortex mixture and the tangentially injected supercritical water establishes first hydrothermal reaction conditions to form lithiated monocrystalline particles, wherein each of the particles has a surface and a core; and
c) subjecting the monocrystalline particles with second hydrothermal reaction conditions to modify surfaces of the monocrystalline particles, wherein a second hydrothermal reaction temperature is lower than a first hydrothermal reaction temperature.