Method and apparatus for in-situ drying investigation and optimization of slurry drying methodology

Patent metadata

Field	Value
Publication number	US-9337470-B2
Application number	US-201213656020-A
Country	US
Kind code	B2
Filing date	Oct 19, 2012
Priority date	Oct 19, 2012
Publication date	May 10, 2016
Grant date	May 10, 2016

Abstract

A method of drying casted slurries that includes calculating drying conditions from an experimental model for a cast slurry and forming a cast film. An infrared heating probe is positioned on one side of the casted slurry and a thermal probe is positioned on an opposing side of the casted slurry. The infrared heating probe may control the temperature of the casted slurry during drying. The casted slurry may be observed with an optical microscope, while applying the drying conditions from the experimental model. Observing the casted slurry includes detecting the incidence of micro-structural changes in the casted slurry during drying to determine if the drying conditions from the experimental model are optimal.

First claim

What is claimed is:

1. A method of drying casted slurries comprising;
calculating drying conditions from a mathematical drying model for a cast slurry coating comprising a suspension of lithium-containing particles in a solvent and wherein said cast slurry coating has a top surface and an opposing bottom surface;
forming said cast slurry coating on a metal foil substrate suitable for a lithium-ion battery, wherein the opposing bottom surface of the cast slurry coating is in contact with said substrate;
positioning an infrared spot heater on one of either the top or opposing bottom surface of the cast slurry coating and positioning a thermal probe on an opposing side of the cast slurry coating, wherein the infrared spot heater controls the temperature of the cast slurry coating during drying and the thermal probe measures the temperature of the cast slurry coating during drying;
positioning a balance under the opposing bottom surface of the cast slurry coating to measure evaporation of the solvent by weight loss during drying;
and
drying the cast slurry coating under the drying conditions from the mathematical drying model while observing the cast slurry coating with an optical microscope of sufficient resolving power to observe microstructural changes in the cast slurry coating during drying.

2. The method of claim 1 , wherein the drying conditions result in a cast slurry coating that is free of cracking, free of delamination from the substrate, or a combination thereof.

3. The method of claim 1 , wherein said lithium-containing particles have a lithium-containing composition selected from the group consisting of lithium cobalt oxide (LCO), lithium iron phosphate (LFP), lithium manganese oxide (LMO), lithium nickel cobalt aluminum oxide (NCA), lithium titanate (LTO), lithium nickel manganese cobalt oxide (NMC) and combinations thereof.

4. The method of claim 1 , wherein said lithium-containing particles have a lithium-containing composition selected from the group consisting of LiCoO 2 , LiMn 2 O 4 , LiNiO 2 , LiFePO 4 , Li 2 FePO 4 F, LiCo 1/3 Ni 1/3 Mn 1/3 O 2 , Li(Li a Ni x Mn y Co z )O 2 , LiC 6 , Li 4 Ti 5 O 12 , Li 4.4 Si, Li 4.4 Ge, LiPF 6 , LiAsF 6 , LiClO 4 , LiBF 4 , LiCF 3 SO 3 and combinations thereof.

5. The method of claim 1 , wherein the forming of the cast slurry coating comprises a roll to roll casting method or a tape casting method.

6. The method of claim 1 , wherein the micro-structural changes being observed comprise protuberances, cracks, blisters, delamination and combinations thereof.

7. The method of claim 1 , wherein the metal in said metal foil substrate is selected from aluminum and copper.

Assignees

• Ut Battelle Llc

Inventors

• Armstrong Beth L
• Daniel Claus
• Howe Jane Y
• Kiggans Jr James O
• Sabau Adrian S
• Wood Iii David L
• Kalnaus Sergiy

Classifications

• H01M4/0435 Primary

  Rolling or calendering · CPC title

• H01M4/04 Primary

  Processes of manufacture in general · CPC title

• H01M4/0485

  Casting · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title