Method for testing one or a plurality of microbattery devices, and system implementing the testing method

Patent metadata

Field	Value
Publication number	US-11474155-B2
Application number	US-202117359594-A
Country	US
Kind code	B2
Filing date	Jun 27, 2021
Priority date	Jul 1, 2020
Publication date	Oct 18, 2022
Grant date	Oct 18, 2022

Abstract

A method for testing at least one energy micro-storage device includes an anode made of metallic lithium formed by electrodeposition of ions on a metal inert to lithium ions, the method comprising a succession of steps during the manufacture of said anode: a step of measuring the initial voltage OCV of the energy micro-storage device; a first charging step, comprising applying a current, measuring the voltage and the internal resistance of the device in order to verify the compliance of the measurements on a very low lithium layer thickness formed at the anode; a second charging stabilization step, comprising applying a current and measuring the voltage of the device in order to verify the compliance of the measurements on a low lithium layer thickness formed at the anode; a retention step with a zero current applied and measuring the voltage in order to confirm the compliance of the energy micro-storage device. A system for implementing the method is also provided.

First claim

The invention claimed is:

1. A method for testing at least one energy micro-storage device comprising an anode made of metallic lithium formed by electrodeposition of Li + ions on a metal inert to lithium ions, an electrolyte and a cathode, wherein said method comprises a sequence of testing steps during the manufacture of said anode, said sequence comprising:
a step of measuring (Ph-a) the initial voltage (OCV) of said device in open-circuit mode in order to obtain, at a time t 0 , the value of the initial voltage of said energy micro-storage device;
if said initial voltage is non-zero, a first charging step (Ph-b) comprising:
applying a current Ib for a time tb in order to charge a first portion of said device for a minimum charging time so as to form a first lithium layer thickness at the anode;
measuring the voltage Vb across the terminals of said device;

determining the internal resistance Rb;
if the voltage Vb is located within an interval Vb min -Vb max defined on the basis of the architecture of the component and if the resistance Rb is located within an interval Rb min -Rb max defined on the basis of the architecture of the component, a stabilization step (Ph-c) comprising:
continuing to apply at least one current Ic for a time tc in order to charge a second portion of said device for a second charging time tc so as to form a second lithium layer thickness at the anode;
measuring the voltage Vc across the terminals of said device;

if the voltage Vc is located within an interval Vc min -Vc max defined on the basis of the architecture of the component, a retention step (Ph-d) comprising:
applying a zero current for a time td;
measuring the voltage V across the terminals of the device over time;
determining the parameter Vd, where Vd=ΔV/Δt,

if Vd is located within an interval Vd min -Vd max defined on the basis of the architecture of the component, said device is tested as being valid.

2. The testing method according to claim 1 , wherein:
the first charging step comprises a series of measurements of voltages Vbi during periods Δtbi spaced by times Tbi in order to determine the curve Vbi as a function of time and in order to determine the value of the voltage Vb able to be defined as the maximum value of the voltages Vbi or the average of the voltages Vbi;
the resistance Rb may be determined after each time tbi by the ratio Vbi/Ic of the curve Vbi as a function of time t.

3. The testing method according to claim 2 , wherein the periods Δtbi are of the order of 10 seconds, the times Tbi being of the order of 0.1 second.

4. The testing method according to claim 1 , wherein the first thickness is of the order of a few nanometres and preferably from 1 to 2 nanometres.

5. The testing method according to claim 2 , wherein:
the stabilization step comprises a series of measurements of voltages Vci during periods Δtci spaced by times Tci in order to determine the value of the voltage Vc defined as the average of the voltages Vci.

6. The testing method according to claim 5 , wherein the periods Δtci are of the order of 50 seconds, the times Tci being of the order of 1 second.

7. The testing method according to claim 1 , wherein the second thickness is less than 10 nanometres and preferably equal to 5 nanometres.

8. The testing method according to claim 1 , wherein:
the retention step comprises a series of measurements of voltages Vdi during periods Δtdi spaced by times Tdi in order to determine the curve Vdi as a function of time;
the parameter Vd is determined by the gradient of the curve Vdi as a function of time t.

9. The testing method according to claim 8 , wherein the periods Δtdi are of the order of 10 seconds, the times Tdi being of the order of 1 second.

10. A system for testing at least one energy micro-storage device, implementing a method for testing at least one energy micro-storage device comprising an anode made of metallic lithium formed by electrodeposition of Li + ions on a metal inert to lithium ions, an electrolyte and a cathode, according to claim 1 , said testing method comprising a sequence of testing steps during the manufacture of said anode, said sequence comprising:
a step of measuring (Ph-a) the initial voltage (OCV) of said device in open-circuit mode in order to obtain, at a time t 0 , the value of the initial voltage of said energy micro-storage device;
if said initial voltage is non-zero, a first charging step (Ph-b) comprising:
applying a current Ib for a time tb in order to charge a first portion of said device for a minimum charging time so as to form a first lithium layer thickness at the anode;
measuring the voltage Vb across the terminals of said device;

determining the internal resistance Rb;
if the voltage Vb is located within an interval Vb min -Vb max defined on the basis of the architecture of the component and if the resistance Rb is located within an interval Rb min -Rb max defined on the basis of the architecture of the component, a stabilization step (Ph-c) comprising:
continuing to apply at least one current Ic for a time tc in order to charge a second portion of said device for a second charging time tc so as to form a second lithium layer thickness at the anode;
measuring the voltage Vc across the terminals of said device;

if the voltage Vc is located within an interval Vc min -Vc max defined on the basis of the architecture of the component, a retention step (Ph-d) comprising:
applying a zero current for a time td;
measuring the voltage V across the terminals of the device over time;
determining the parameter Vd, where Vd=ΔV/Δt,

if Vd is located within an interval Vd min -Vd max defined on the basis of the architecture of the component, said device is tested as being valid;
said testing system comprising:
a current generator connected to said device;
a voltmeter connected to said device;
a controller connected to said current generator and to said voltmeter.

11. The testing system according to claim 10 , wherein the current generator is programmable and the voltmeter is programmable.

12. The testing system according to claim 10 , wherein the controller comprises a timer, a memory and a processor.

13. An assembly of a plurality of systems for testing an energy micro-storage device (Dn), implementing the method according to claim 1 , each system comprising:
a current generator (An), possibly programmable, connected to said device (Dn);
a voltmeter (Vn), possibly programmable, connected to said device (Dn),
each current generator (An) and each voltmeter (Vn) being connected to a controller (Cn).

14. The assembly of a plurality of systems for testing an energy micro-storage device (Dn), implementing a method for testing at least one energy micro-storage device comprising an anode made of metallic lithium formed by electrodeposition of Li + ions on a metal inert to lithium ions, an electrolyte and a cathode, according to claim 1 , said testing method comprising a sequence of testing steps during the manufacture of said anode, said sequence comprising:
a step of measuring (Ph-a) the initial voltage (OCV) of said device in open-circuit mode in order to obtain, at a time t 0 , the value of the initial voltage of said energy micro-storage device;
if said initial voltage is non-zero, a first charging step (Ph-b) comprising:
applying a current Ib for a time tb in order to charge a first portion of said device for a minimum charging time so as to form a first lithium layer thickness at the anode;
measuring the voltage Vb across the terminals of said device;

determining the internal resistance Rb;

Assignees

• Commissariat Energie Atomique

Inventors

• Toffoli Alain
• Oukassi Sami

Classifications

• G01R31/3835 Primary

  involving only voltage measurements · CPC title

• G01R31/3648

  comprising digital calculation means, e.g. for performing an algorithm · CPC title

• G01R31/389 Primary

  Measuring internal impedance, internal conductance or related variables · CPC title

• H01M10/4285

  Testing apparatus · CPC title

• G01R31/385 Primary

  Arrangements for measuring battery or accumulator variables (for monitoring G01R31/382) · CPC title