IP Library Granted Patent US 10,329,154
Granted Patent B2
US 10,329,154 · App. 14/567,220 · Granted Jun 25, 2019

Method for preparing a particulate cathode material

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Quick Facts
Patent No.
US 10,329,154
App. No.
14/567,220
Granted
Jun 25, 2019
Kind
B2
Abstract

A method for preparing an electrode material, said material comprising complex oxide particles having a non-powdery conductive carbon deposit on at least part of their surface, said method comprising: grinding into nanometer size complex oxide particles or particles of complex oxide precursors, wherein the grinding is performed in a bead mill on particles dispersed in a carrier solvent, adding an organic carbon precursor to the oxide particles or oxide precursor particles before, during or after said grinding, and pyrolysing the mixture thus obtained, selecting the size of the particles to grind, the size of the beads used to grind, and the size of the resulting particles such that: 0.004<MS(SP)/MS(B)<0.12 and 0.0025<MS(FP)/MS(SP)<0.25, wherein MS(SP) represents the mean size diameter of the particles before grinding, MS(FP) represents the mean size diameter of the particles after grinding, and MS(B) is the mean size diameter of the beads.

Claims (22)

1. A method for improving the electrochemical performance of previously synthesized lithium metal phosphate particles, said method comprising:

grinding said previously synthesized lithium metal phosphate particles into a particle size of from 5 nm to less than 1 micron, wherein the grinding is performed in a bead mill on particles dispersed in a carrier solvent, and such that:

0.004<MS(SP)/MS(B)<0.12,

0.0025<MS(FP)/MS(SP)<0.25

wherein MS(SP) represents the mean size diameter of the particles before grinding, MS(FP) represents the mean size diameter of the particles after grinding, and MS(B) is the mean size diameter of the beads;

adding an organic carbon precursor to the particles before, during or after said grinding; and

performing a pyrolysis on the organic carbon precursor and ground particles to obtain a non-powdery conductive carbon deposit on at least part of the surface of the particles,

wherein said organic carbon precursor is a monomer, said method comprising a further step performed after said grinding and before said pyrolysis, said further step being polymerizing or cross-linking the organic carbon precursor.

2. The method of claim 1 , wherein the carrier solvent is water or isopropanol.

3. The method of claim 1 , said method comprising a further step performed before said pyrolysis, said further step being aggregating the organic carbon precursor and the ground particles.

4. The method of claim 3 , wherein said aggregating is performed by flocculating, by spray drying, or by charge effect.

5. The method of claim 1 , wherein the mean size diameter of the beads is from 100 μm to 500 μm.

6. The method of claim 1 , said method comprising a further step performed before said grinding, said further step being adding an organic stabilizing agent to said previously synthesized lithium metal phosphate particles.

7. The method of claim 6 , wherein the organic stabilizing agent is selected from the group consisting of organic electrostatic or electrosteric stabilizers, surfactants, dispersant agents, self-adsorbing agents, and encapsulating agents.

8. The method of claim 6 , wherein the organic stabilizing agent is a conductive carbon precursor.

9. The method of claim 1 , wherein the particles before said grinding have a size of from 1 μm to 50 μm.

10. The method of claim 1 , wherein the previously synthesized lithium metal phosphate particles have an olivine structure, and wherein:

lithium is optionally partly replaced with not more than 10 atomic % Na or K;

the metal is Fe II or Mn II and is optionally partly replaced with not more than 50 atomic % of at least one metal selected from the group consisting of Mn, Fe, Ni and Co, and optionally replaced with not more than 10 atomic % of at least one aliovalent or isovalent metal different from Fe, Mn, Ni or Co; and

phosphate is optionally partly replaced with not more than 10 mol % of at least one group selected from SO and SiO 4.

11. The method of claim 10 , wherein the aliovalent or isovalent metal different from Fe, Mn, Ni or Co is at least one metal selected from the group consisting Mg, Mo, Nb, Al, Ta, Ge, La, Y, Yb, Sm, Ce, Hf, Cr, Zr, Bi, Zn, Ca and W.

12. The method of claim 1 , wherein the previously synthesized lithium metal phosphate particles have the formula LiFe 1-x Mn x PO 4 , wherein 0 ≤×≤0.5, or LiMnPO 4 .

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 23, 2024
From: JOHNSON MATTHEY PUBLIC LIMITED COMPANY
To: EPSILON CARBON PRIVATE LTD.
Reel/Frame 069664/0522 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 27, 2015
From: JOHNSON MATTHEY BATTERY MATERIALS LTD.
To: JOHNSON MATTHEY PUBLIC LIMITED COMPANY
Reel/Frame 036887/0839 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 26, 2015
From: CLARIANT (CANADA) INC.
To: JOHNSON MATTHEY BATTERY MATERIALS LTD.
Reel/Frame 036876/0653 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 11, 2014
From: LIANG, GUOXIAN; CHAREST, PATRICK; GAUTHIER, MICHEL; GUERFI, ABDELBAST; MICHOT, CHRISTOPHE; ZAGHIB, KARIM
To: PHOSTECH LITHIUM INC.
Reel/Frame 034480/0129 →
MERGER Recorded Dec 11, 2014
From: PHOSTECH LITIUM INC.
To: CLARIANT (CANADA) INC.
Reel/Frame 034480/0421 →