Process for making a particulate (oxy)hydroxide or oxide, particulate (oxy)hydroxide or oxide and use
AssigneeBASF SE
InventorsThorsten BEIERLING, Joop Enno FRERICHS, Zoltan BAAN
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Abstract
Disclosed herein are a process for making a particulate (oxy)hydroxide or oxide, a particulate (oxy)hydroxide or oxide, and a method of using the particulate (oxy)hydroxide or oxide. Also disclosed herein is a process for making a particulate (oxy)hydroxide or oxide of TM where TM represents metals, where the process is performed in a cascade of at least three stirred tank reactors.
Claims15
A process for making a particulate (oxy)hydroxide or oxide of TM wherein TM represents metals, wherein TM comprises nickel and at least one metal selected from the group consisting of cobalt and manganese and wherein the nickel content of TM is at least 80 mol-%, wherein said process is performed in a cascade of at least three stirred tank reactors and comprises the steps of:
- (a) providing an aqueous solution (α1) containing a water-soluble salt of Ni and, optionally, at least one metal selected from the group consisting of cobalt and manganese, and an aqueous solution (β1) containing an alkali metal hydroxide and, optionally, an aqueous solution (γ1) containing a complexing agent selected from the group consisting of ammonia, glycine, tartrate, citrate, and oxalate,
- (b) combining, in a first stirred tank reactor, solution (α1) and solution (β1) and, if applicable, solution (γ1), at a pH value in the range of from 11.0 to 13.5 and with an average energy input in the range of from 8 to 20 W/l, thereby creating slurried solid particles of a hydroxide of TM,
- (c) transferring the particles from step (b) as a slurry into a second stirred tank reactor,
- (d) providing an aqueous solution (α2) containing a water-soluble salt of Ni and at least one metal selected from the group consisting of cobalt and manganese, and an aqueous solution (β2) containing an alkali metal hydroxide and, optionally, an aqueous solution (γ2) containing a complexing agent selected from the group consisting of ammonia, glycine, tartrate, citrate, and oxalate,
- (e) combining solution (α2) and solution (β2) and, if applicable, solution (γ2), in said second stirred tank reactor at a pH value in the range of from 10.5 to 12.0 and with an average specific energy input in the range of from 2 to 8 W/l and by a factor of from 0.20 to 0.75 lower than in step (b), thereby growing the solid particles of a hydroxide of TM,
- (f) transferring the particles from step (e) as a slurry into a third stirred tank reactor,
- (g) combining solution (α2) and solution (β2) and, if applicable, solution (γ2), in said third stirred tank reactor at a pH value in the range of from 10.5 to 12.0,
- wherein the average specific energy input in step (g) is in the range of from 0.5 to 2 W/l and by a factor of 0.20 to 0.75 lower than in step (e), and wherein the pH values are determined at 23° C.
A particulate (oxy)hydroxide of TM with a core-shell structure and a span of the particle diameter distribution (D90−D10)/D50 below 0.30, wherein TM comprises nickel and at least one metal selected from the group consisting of cobalt and manganese and wherein the nickel content of TM is at least 80 mol-%, and wherein the particles are composed of primary particles and have a core and shell and a concentric layer between core and shell wherein the density of the concentric layer is higher than the density of the core and of the shell,
- and wherein said particulate (oxy)hydroxide has a total pore/intrusion volume in the range of from 0.033 to 0.1 ml/g, determined by N2 adsorption.
A particulate oxide of TM with a core-shell structure and a span of the particle diameter distribution (D90−D10)/D50 below 0.30, wherein TM comprises nickel and wherein the nickel content of TM is at least 80 mol %, and at least one metal selected from the group consisting of cobalt and manganese, and wherein the particles are composed of primary particles,
- and wherein said particulate oxide has a total pore/intrusion volume in the range of from 0.1 to 0.5 ml/g, determined by N2 adsorption.
A cathode active material of the general formula Li1+xTM1−xO2 with x being in the range of from −0.01 to +0.05 and with a core-shell structure and a span of the particle diameter distribution (D90−D10)/D50 below 0.30, wherein TM comprises nickel and at least one metal selected from the group consisting of cobalt and manganese, wherein the nickel content of TM is at least 80 mol %,
- wherein said cathode active material has a total pore/intrusion volume in the range of from 0.0035 to 0.01 ml/g, determined by N2 adsorption.
Dependencies are inferred from the claim text.