Method and apparatus for producing cathode particles

Patent metadata

Field	Value
Publication number	US-2020131046-A1
Application number	US-201816627932-A
Country	US
Kind code	A1
Filing date	Jul 13, 2018
Priority date	Jul 15, 2017
Publication date	Apr 30, 2020
Grant date	—

Abstract

A method for producing cathode particles is provided. The method includes: providing a plurality of precipitation zones from i=1 to N, wherein the precipitation zones are connected in series, each precipitation zone comprises a feed stream (ai) providing the precipitation cations, a feed stream (bi) providing the precipitation anions, a continuous outflow (ci) of precipitation particle slurry to the next precipitation zone, and a continuous inflow (ci−1) of precipitation particle slurry from the prior precipitation zone, and forming, in the precipitation zones, precipitated particles, and finally to form, in the precipitation zone N, precursor particles comprised of N layers, wherein layer i of each particle is precipitated and formed in the precipitation zone i, wherein N is not less than 3, and when i=1, there is no inflow (ci−1).

First claim

1 : A method comprising:
providing a plurality of precipitation zones from i=1 to N, wherein the precipitation zones are connected in series, each precipitation zone comprises a feed stream (a i ) providing precipitation cations, a feed stream (b i ) providing precipitation anions, a continuous outflow (c i ) of precipitation particle slurry to the next precipitation zone, and a continuous inflow (c i−1 ) of precipitation particle slurry from the prior precipitation zone, and forming, in the precipitation zones, precipitated particles, and finally to form, in the precipitation zone N, precursor particles comprised of N layers, wherein layer i of each particle is precipitated and formed in the precipitation zone i, and wherein N is not less than 3, and when i=1, there is no continuous inflow (c i−1 ).

2 : The method of claim 1 , wherein the precursor particles are further separated and dried under vacuum, N 2 , Ar or air for 3-24 hours between 80-200° C. to get dried precursor particles.

3 : The method of claim 2 , wherein the dried precursor particles are mixed with a lithium resource and calcined in an oxygen or air to form gradient multilayer core-shell cathode materials.

4 : The method of claim 3 , wherein the lithium resource is selected from LiOH*H 2 O, Li 2 CO 3 , LiNO 3 , lithium acetate, lithium metal or Li 2 O, the Li to metal cations ratio is between 0.5-1.5.

5 : The method of claim 3 , wherein the mixed precursor particles and lithium resource are calcined from 300-950° C., and multiple hold temperatures and ramp rates are used, at least one hold temperature from 300-500° C. for 2-12 hours occurs before another heating from 700-950° C. for 2-20 hours, the ramp rate during heating is from 0.5 to 10 degrees per minute.

6 : The method of claim 1 , wherein each precipitation zone is blanketed or bubbled by He, N2 or Ar gas.

7 : The method of claim 1 , wherein the precipitation cation is selected from Mg, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Al, or any combinations thereof, and cation resource is selected from sulfate, carbonate, chloride, nitrate, fluoride, oxide, hydroxide, oxyhydroxide, oxalate, carboxylate, acetate, phosphate, borate, or any combinations thereof.

8 : The method of claim 1 , wherein at least one precipitation zone has a different cation composition from the adjacent precipitation zone.

9 : The method of claim 1 , wherein the stream (b i ) is selected from NaOH, Na 2 CO 3 , NaHCO 3 , Na 2 C 2 O 4 , LiOH, Li 2 CO 3 , LiHCO 3 , Li 2 C 2 O 4 , KOH, K 2 CO 3 , KHCO 3 , K 2 C 2 O 4 or any combinations thereof.

10 : The method of claim 1 , wherein at least one precipitation zone further comprises an inlet stream (d i ) providing chelating agents, the chelating agent is selected from ammonia hydroxide, ammonium chloride, ammonium sulfate, ammonium dihydrogen phosphate, ethylene glycol, carboxylic acids, ammonium nitrate, glycerol, 1,3 propane-diol, urea, N,N′-dimethylurea, quaternary ammonia salts or any combinations thereof.

11 . (canceled)

12 : The method of claim 1 , wherein V i is the volume of the precipitation zone i, and it has the relationship of V 1 ≤V 2 ≤ . . . ≤V N .

13 : The method of claim 1 , wherein in the precipitation zones, d(ρ c,i V i )/dt=0, wherein ρ c,i is the fluid density of the outflow (c i ) of the precipitation zone i, V i is the volume of the precipitation zone i.

14 : The method of claim 1 , wherein the precursor particle is described by the formula (Ni x Mn y Co z Me 1-x-y-z )(CO 3 ) a (OH) 2-2a , and the precursor particle has an average composition within 0<a<1; x+y+z>0.95; x>0.7; z<0.35.

15 : The method of claim 1 , further comprising:
collecting the outflow (c i ) of non-steady state particles of the last precipitation zone N at the initial reaction stage; adding acid solution to dissolve the non-steady state particles to get a fluid; determining the concentration and composition of the fluid, and introducing the fluid into the feed stream (a i ).

16 : An apparatus for producing cathode particles, comprising a plurality of precipitation zones from i=1 to N configured to form precipitated particles in the precipitation zones, and finally to form precursor particles comprised of N layers in the precipitation zone N, wherein the precipitation zones are connected in series, each precipitation zone comprises a feed stream (a i ) providing precipitation cations, a feed stream (b i ) providing precipitation anions, a continuous outflow (c i ) of precipitation particle slurry to the next precipitation zone, and a continuous inflow (c i−1 ) of precipitation particle slurry from the prior precipitation zone, and wherein layer i of each particle is precipitated and formed in the precipitation zone i, and wherein N is not less than 3, and when i=1, there is no continuous inflow (c i−1 ).

Assignees

• Microvast Power Systems Co Ltd

Inventors

• Yonemoto Bryan
• Mattis Wenjuan Liu
• Zhang Zhifeng
• Zhang Xiao

Classifications

• H01M4/0497

  Chemical precipitation · CPC title

• C01G53/50

  of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2 · CPC title

• H01M4/525

  of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy · CPC title

• H01M4/1391

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

• H01B1/08 Primary

  oxides · CPC title