# US 8,465,556 B2 · Method of forming a solid state cathode for high energy density secondary batteries

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- Number: US 8,465,556 B2
- Document ID: US8465556B2
- Status: Granted
- Kind: B2
- Application number: 12/928,001
- Filed: 2010-12-01
- Published: 2012-06-07
- Granted: 2013-06-18
- Earliest claimed: 2010-12-01
- Assignees: Sisom Thin Films LLC
- Applicants: Isaiah O. Oladeji
- Inventors: Isaiah O. Oladeji
- Web page: https://patentgrep.com/patent/US8465556B2

## CPC

- H01M 10/058: Construction or manufacture
- H01M 4/0404: {by coating on electrode collectors}
- H01M 4/0419: {involving spraying}
- H01M 4/0435: {Rolling or calendering}
- H01M 4/0471: {involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis}
- H01M 4/049: {Manufacturing of an active layer by chemical means}
- H01M 4/1391: of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- H01M 10/054: Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
- H01M 10/26: Selection of materials as electrolytes
- H01M 10/28: Construction or manufacture
- H01M 4/625: {Carbon or graphite}
- H01M 10/052: Li-accumulators
- H01M 10/0562: Solid materials
- H01M 10/0566: Liquid materials
- Y02E 60/10: Energy storage using batteries
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- Y10T 29/49108: Electric battery cell making
- Y10T 29/49115: including coating or impregnating
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

A method for making a solid state cathode comprises the following steps: forming an alkali free first solution comprising at least one transition metal and at least two ligands; spraying this solution onto a substrate that is heated to about 100 to 400° C. to form a first solid film containing the transition metal(s) on the substrate; forming a second solution comprising at least one alkali metal, at least one transition metal, and at least two ligands; spraying the second solution onto the first solid film on the substrate that is heated to about 100 to 400° C. to form a second solid film containing the alkali metal and at least one transition metal; and, heating to about 300 to 1000° C. in a selected atmosphere to react the first and second films to form a homogeneous cathode film. The cathode may be incorporated into a lithium or sodium ion battery.

## Claims

### Claim 1

A method of forming a solid state cathode comprising the steps of:
a) forming a generally planar substrate;
b) forming a substantially alkali-free first solution comprising at least one transition metal and at least two ligands;
c) spraying said first solution onto said substrate while maintaining said substrate at a temperature between about 100 and 400° C. to form a first solid film containing said transition metal on said substrate;
d) forming a second solution comprising at least one alkali metal, at least one transition metal, and at least two ligands;
e) spraying said second solution onto said first solid film on said substrate while maintaining said substrate at a temperature between about 100 and 400° C. to form a second solid film containing said alkali metal and at least one transition metal; and,
f) heating to a temperature between about 300 and 1000° C. in a selected atmosphere to react said first and second films to form a homogeneous cathode film.

### Claim 2 (depends on 1)

The method of claim 1 wherein said first solution comprises:
at least one transition metal selected from the group consisting of: Mn, Co, Ni, Al, Fe, and Sn; and,
at least two ligands selected from the group consisting of: urea, acetic acid, citric acid, hydrochloric acid, sulfuric acid, nitric acid, lithium citrate, sodium citrate, triethanolamine, ethylenediamine, ammonia, nitrilotriacetic acid, phosphoric acid, and acetonitrile.

### Claim 3 (depends on 1)

The method of claim 1 wherein said second solution comprises:
an alkali metal selected from the group consisting of: Li and Na;
at least one transition metal selected from the group consisting of: Mn, Co, Ni, Al, Fe, and Sn; and,
at least two ligands selected from the group consisting of: urea, acetic acid, citric acid, hydrochloric acid, sulfuric acid, nitric acid, lithium citrate, sodium citrate, triethanolamine, ethylenediamine, ammonia, nitrilotriacetic acid, and acetonitrile.

### Claim 4 (depends on 1)

The method of claim 1 wherein said substrate is selected from the group consisting of: stainless steel foil, nickel foil, nickel-clad copper foil, and aluminum foil.

### Claim 5 (depends on 1)

The method of claim 1 wherein said homogeneous cathode film comprises a compound selected from the group consisting of:
LiMn2-xM1xO4 where M1 is selected from the group consisting of Al, Sn, Zn, and Fe, and 0≦x≦0.05;
LiCo1-xM2xO2 where M2 is selected from the group consisting of Ni and Al, and 0≦x≦0.5;
LiNi1-xM3xO2 where M3 is selected from the group consisting of Co and Al, and 0≦x≦0.5;
LiMnxNiyCozAltO2 where x+y+z+t=1, and 0≦(x, y, z, and t)≦1;
LiM4PO4 where M4 is selected from the group consisting of Fe, Co, Ni, and Mn;
NaMn2-xM5xO4 where M5 is selected from the group consisting of Al, Sn, Zn, and Fe, and 0≦x≦0.05;
NaCo1-xM6xO2 where M6 is selected from the group consisting of Ni and Al, and 0≦x≦0.5;
NaNi1-xM7xO2 where M7 is selected from the group consisting of Co and Al, and 0≦x≦0.5;
NaMnxNiyCozAltO2 where x+y+z+t=1, and 0≦(x, y, z, and t)≦1; and,
NaM8PO4 where M8 is selected from the group consisting of Fe, Co, Ni, and Mn.

### Claim 6 (depends on 1)

The method of claim 1 further comprising the step of calendaring to increase the density of said deposited films prior to heating step (f).

### Claim 7 (depends on 6)

The method of claim 6 wherein said calendaring comprises applying a mechanical pressure of at least 2000 psi.