# US 4,398,346 A · Method for lithium anode and electrochemical cell fabrication > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 4,398,346 A - Document ID: US4398346A - Status: Granted - Kind: A - Application number: 06/314,210 - Filed: 1981-10-23 - Granted: 1983-08-16 - Earliest claimed: 1981-10-23 - Assignees: Medtronic, Inc. - Inventors: Lloyd J. Underhill; William D. Helgeson - Web page: https://patentgrep.com/patent/US4398346A ## CPC - H01M 4/12: of consumable metal or alloy electrodes (use of alloy compositions as active materials H01M4/38) - H01M 6/182: {with halogenide as solid electrolyte} - H01M 6/50: Methods or arrangements for servicing or maintenance, e.g. for maintaining operating temperature (constructional details of current conducting connections for detecting conditions inside cells or batteries, e.g. details of voltage sensing terminals, H01M50/569) - Y02E 60/10: Energy storage using batteries - 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 - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract Method of preparing lithium anodes contacted with organic materials prior to association of the anode with a cathode material wherein the contacted anode is first subjected to a heat treatment. Upon incorporation of the improved anode into an electrochemical battery or cell and association of the heat treated anode with a suitable cathode material, the cell may be discharged under controlled conditions for a short time prior to its usual "burn-in" discharge. ## Claims ### Claim 1 A method of preparing an anode for an electrochemical cell comprising the steps of: providing a lithium anode element having an operative surface area to be associated with a cathode; contacting at least the operative surface area of the anode element with organic material, and heating the anode element and organic material together to a temperature between at least about 260.degree. F. and the melting temperature of the organic material. ### Claim 2 (depends on 1) The method of claim 1 wherein the anode element is held at the heating temperature for a predetermined period of time. ### Claim 3 (depends on 2) The method of claim 2 wherein the time is at least about one hour. ### Claim 4 (depends on 2) The method of claim 2 wherein the anode is cooled to room temperature after the heating step before any further preparation steps are carried out. ### Claim 5 (depends on 1) The method of claim 1 wherein the anode and contacting organic material are incorporated into a subassembly including an open cell container prior to the heating step and the entire subassembly is heated. ### Claim 6 (depends on 1) The method of claim 1 wherein the heating is by means of a forced air oven. ### Claim 7 (depends on 6) The method of claim 6 wherein the oven if preheated to a temperature between about 260.degree. F. and about 310.degree. F., the anode and contacting organic material are placed in the oven and heated to substantially the temperature at which the oven is maintained over a period of at least about 45 minutes to one hour and thereafter maintained at that temperature for at least about one hour. ### Claim 8 (depends on 7) The method of claim 7 wherein the anode element is removed from the oven following the heating step and cooled to room temperature before any further assembly operations are performed involving it. ### Claim 9 (depends on 1) The method of claim 1 wherein the organic material is in the form of a coating on the anode element. ### Claim 10 (depends on 1) The method of claim 1 wherein the organic material is in the form of a multi-layer coating on the anode element. ### Claim 11 (depends on 1) The method of claim 1 wherein the organic material is in the form of a self-supporting sheet. ### Claim 12 (depends on 1) The method of claim 1 wherein the heating temperature is about 295.degree. F..+-.about 10.degree. F. ### Claim 13 (depends on 12) The method of claim 12 wherein the heating is accomplished over a period of time of about two hours .+-.15 minutes. ### Claim 14 (depends on 1) The method of claim 1 wherein the heating temperature is between about 260.degree. F. and 310.degree. F. ### Claim 15 (depends on 1) The method of claim 1 wherein the organic material is a polyvinylpyridine polymer. ### Claim 16 (depends on 15) The method of claim 15 wherein the organic material is poly-2-vinylpyridine. ### Claim 17 (depends on 1) The method of claim 1 wherein the organic material is poly-2-vinylpyridine in the form of a coating on the operative surface area of the anode element and the heating temperature to which the coated anode is heated is about 295.degree. F..+-.about 10.degree. F. ### Claim 18 (depends on 17) The method of claim 17 wherein the heating is for a period of time of about 2 hours .+-.15 minutes. ### Claim 19 (depends on 17) The method of claim 17 wherein the coated anode element is held at the heating temperature for at least about one hour. ### Claim 20 (depends on 17) The method of claim 17 wherein the coated anode is incorporated into a subassembly including a cell container prior to the heating step and the entire subassembly is heated. ### Claim 21 A method of making an electrochemical cell wherein the anode includes an operative surface area and the cathode comprises a charge-transfer complex material, comprising the steps: providing a lithium anode element having an operative surface to be associated with a cathode in a cell; contacting at least the operative surface of the anode element with organic material; heating the anode element and organic material to a temperature between at least about 260.degree. F. and the melting temperature of the organic material; providing a cathode including a charge-transfer complex material, and assembling the anode and cathode in electrochemically operative relationship. ### Claim 22 (depends on 21) The method of claim 21 wherein a container is provided for the cell components, the anode and the contacting organic material are assembled into the container following which they are heated, and the cathode material is subsequently melted and poured into the container. ### Claim 23 (depends on 22) The method of claim 22 wherein the assembly is cooled prior to the addition of the cathode material. ### Claim 24 (depends on 21) The method of claim 21 wherein the cell is shorted across a resistor of about 0.1 to 0.2 ohms for a predetermined time following its assembly. ### Claim 25 (depends on 24) The method of claim 24 wherein the discharge is accomplished in two steps, the first step being discharge at a relatively high rate for a relatively short period of time; the second step being discharge at a relatively low rate for a relatively long period of time. ### Claim 26 (depends on 25) The method of claim 25 wherein the first step discharge is carried out across a resistor of about 0.1 to 0.2 ohms for a period of about one hour. ### Claim 27 (depends on 21) The method of claim 21 wherein the cathode comprises the reaction product of a mixture of polyvinylpyridine and iodine. ### Claim 28 (depends on 27) The method of claim 27 wherein the polyvinylpyridine is poly-2-vinylpyridine. ### Claim 29 (depends on 28) The method of claim 28 wherein the iodine and poly-2-vinylpyridine are present in a weight ratio greater than about 30:1. ### Claim 30 (depends on 29) The method of claim 29 wherein the weight ratio is about 50:1. ### Claim 31 (depends on 29) The method of claim 29 wherein the weight ratio is greater than 50:1. ### Claim 32 (depends on 29) The method of claim 29 wherein the weight ratio is about 100:1. ### Claim 33 (depends on 29) The method of claim 29 wherein the anode element is held at the heating temperature for a period of time. ### Claim 34 (depends on 33) The method of claim 33 wherein the time is at least about one hour. ### Claim 35 (depends on 33) The method of claim 33 wherein the anode is cooled to room temperature after the heating step before any further preparation steps are carried out on it. ### Claim 36 (depends on 21) The method of claim 21 wherein the anode and contacting organic material are incorporated into a subassembly including an open cell container prior to the heating step and the entire subassembly is heated. ### Claim 37 (depends on 21) The method of claim 21 wherein the heating is by means of a forced air oven. ### Claim 38 (depends on 37) The method of claim 37 wherein the oven is preheated to a temperature between about 260.degree. F. and about 310.degree. F., the anode and contacting organic material are placed in the oven and heated to substantially the temperature at which the oven is maintained over a period of about 45 minutes to about one hour and thereafter maintained at that temperature for about one hour. ### Claim 39 (depends on 39) The method of claim 39 wherein the anode element is removed from the oven following the heating step and cooled to room temperature before any further assembly operations are performed involving it. ### Claim 40 (depends on 21) The method of claim 21 wherein the organic material is in the form of a coating on the anode element. ### Claim 41 (depends on 21) The method of claim 21 wherein the organic material is in the form of a multi-layer coating on the anode element. ### Claim 42 (depends on 21) The method of claim 21 wherein the organic material is in the form of a self-supporting sheet. ### Claim 43 (depends on 21) The method of claim 21 wherein the heating temperature is about 295.degree. F..+-.about 10.degree. F. ### Claim 44 (depends on 21) The method of claim 21 wherein the heating temperature is between about 260.degree. F. and 310.degree. F. ### Claim 45 (depends on 21) The method of claim 21 wherein the organic material is a polyvinylpyridine polymer. ### Claim 46 (depends on 45) The method of claim 45 wherein the organic material is poly-2-vinylpyridine. ### Claim 47 (depends on 21) The method of claim 21 wherein the organic material is poly-2-vinylpyridine in the form of a coating on the operative surface area of the anode element and the heating temperature to which the coated anode is heated is about 295.degree. F..+-.about 10.degree. F. ### Claim 48 (depends on 47) The method of claim 47 wherein the coated anode element is held at the heating temperature for at least about one hour. ### Claim 49 (depends on 47) The method of claim 47 wherein the coated anode is incorporated into a subassembly including a cell container prior to the heating step and the entire subassembly is heated. ### Claim 50 (depends on 47) The method of claim 47 wherein the cell is discharged across a resistor of about 0.1 to 0.2 ohms for a predetermined time following its assembly. ### Claim 51 (depends on 50) The method of claim 50 wherein the discharge is accomplished in two steps, the first step being discharge at a relatively high rate for a relatively short period of time; the second step being discharge at a relatively low rate for a relatively long period of time. ### Claim 52 (depends on 47) The method of claim 47 wherein the cathode comprises the reaction product of a mixture of polyvinylpyridine and iodine. ### Claim 53 (depends on 47) The method of claim 47 wherein the polyvinylpyridine is poly-2-vinylpyridine. ### Claim 54 (depends on 47) The method of claim 47 wherein the iodine and poly-2-vinylpyridine are present in a weight ratio greater than about 30:1. ### Claim 55 (depends on 47) The method of claim 47 wherein the weight ratio is about 50:1. ### Claim 56 (depends on 47) The method of claim 47 wherein the weigth ratio is greater than 50:1. ### Claim 57 (depends on 47) The method of claim 47 wherein the weight ratio is about 100:1. ### Claim 58 (depends on 47) The method of claim 47 wherein the cell is discharged across a resistor of about 0.1 to 0.2 ohms for a predetermined time following its assembly. ### Claim 59 (depends on 54) The method of claim 54 wherein the resistance is about 0.1 ohms and the time is about one hour. ### Claim 60 (depends on 47) The method of claim 47 wherein the discharge is accomplished in two steps, the first step being discharge at a relatively high rate for a relatively short period of time; the second step being discharge at a relatively low rate for a relatively long period of time. ### Claim 61 (depends on 47) The method of claim 47 wherein the first step discharge is carried out across a resistor of about 0.1 to 0.2 ohms for a period of about one hour.