Method for testing one or more microbattery devices and system for implementing the testing method - Patent Application 20070122999
A rapid, non-destructive testing method for 'Li-free' microbatteries using sequential voltage and charge phases addresses the inefficiencies of existing methods, enabling early defect identification and reducing manufacturing costs.
Patent Information
- Application Number
- JP2021097798
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-07-01
- Filing Date
- 2021-06-11
- Publication Date
- 2025-11-27
- Estimated Expiration
- 2041-06-11
AI Technical Summary
Existing electrical testing methods for 'Li-free' microbatteries are inadequate, as they require lengthy cycles that can cause structural changes and are not suitable for early identification of faulty devices, leading to high manufacturing costs and inefficiencies.
A non-degrading, rapid testing method involving sequential phases to measure initial voltage, charge, stabilize, and hold the microbattery, using programmable current generators and voltmeters to determine key parameters without full discharge, allowing early identification of faulty devices.
Enables rapid, non-destructive testing of 'Li-free' microbatteries, reducing manufacturing costs and identifying defects early in the process, without the need for full cycling, thus improving manufacturing efficiency.
Smart Images

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Abstract
Description
[Technical Field]
[0001] The field of the invention is that of electrical testing of electronic or technological devices manufactured using microelectronic techniques, ie integrated circuits, sensors, elementary devices (resistors, diodes, capacitors, etc.).
[0002] More specifically, it includes electrical test methods dedicated to a specific category of energy micro-storage components commonly referred to as microbatteries. [Background technology]
[0003] Microbatteries are fabricated by sequentially depositing the following on a substrate: (i) a first current collector, (ii) a first electrode, (iii) an electrolyte, (iv) a second electrode, and (v) a second current collector. To protect the device from chemical reactions with oxygen and water vapor, it is necessary to encapsulate it by depositing additional layers or adding a cover.
[0004] Generally, microbatteries can be divided into three categories depending on the type of negative electrode (or anode) that is often deposited on top of the electrolyte. - Li + An anode made of an ion storage material: this often includes an oxide of a transition metal (Vox, TiOx, NiOx, etc.) or a crystal forming material (Si, Ge, C or a mixture). - Anode made of metallic lithium: a layer of lithium is deposited in metallic form on a current collector. - Anode made of a metal inert to lithium: this configuration is often called "Li-free" with reference to the paper J.Electrochem.Soc.-2000-Neudecker-517-23. In this case, the anode made of metallic lithium is inert to the Li (evolved from the cathode) + Ions are formed during the first charge of the battery by electrodeposition between the electrolyte and the second current collector.
[0005] The last configuration is the most advantageous for microbatteries integrated on silicon substrates and when using microfabrication techniques: it offers the presence of lithium metal (which is the most effective anode due to its energy density, potential, and cyclability) without the drawbacks associated with its presence during processing (sensitivity to air, incompatibility with etching and photolithography solutions).
[0006] Generally, the most commonly used and most reliable sorting and electrical testing protocol is to (i) test the microbatteries through multiple complete charge-discharge cycles (from fully charged to fully discharged), and (ii) compare the capacity values, voltage profile, and internal resistance to reference values.
[0007] However, this approach has some limitations: in the context of microbatteries, and more specifically in the context of "Li-free" microbatteries, cycling leads to structural variations in the active stack, in this case the formation of metallic lithium, making it highly air-sensitive and difficult to accommodate in technological manufacturing processes.
[0008] The application of this method is still very rare, in that for larger batteries long test periods are required, which implies considerable costs.
[0009] The sorting can be based on one or more parameters of the microbattery without the need to cycle the microbattery. The most commonly used electrical parameters include: - Open-circuit voltage, or OCV. This voltage corresponds to the voltage measured on the microbattery at the end of its manufacture, before any electrical operation. This voltage generally indicates the state of charge of the microbattery. This is verified, for example, in the case of microbatteries whose anodes are made of metallic lithium or storage anodes. In the case of "Li-free" microbatteries, experiments have shown that the OCV has a large variability within a wafer and between wafers, and no correlation could be found between OCV and state of charge, as shown in Figure 1, which illustrates the OCV variation of microbattery components manufactured in a batch of seven wafers. The variability is large both within a wafer and between wafers. - The variability is related to the fact that the anode made of lithium is no longer formed at this stage, and the OCV measurement only provides information about the state of the electrolyte / electrode interface, without any relation to the state of charge or future electrical behavior. As a result, this parameter is not suitable for establishing all sorts of microbattery configurations. - Internal resistance: this corresponds to all resistive contributions occurring within the microbattery structure and is the sum of the electrolyte resistance and the charge transfer within the electrodes and at the interfaces. This parameter is not relevant for sorting in the case of "Li-free" microbatteries, for the same reasons explained above, since anodes made of metallic lithium are not formed.
[0010] The sorting challenge in this case is precisely to have electrical parameters that may be useful for sorting microbatteries, including "Li-free" microbatteries, without forcing cycling, at the risk of being able to perform the sorting only after the end of the manufacturing process. Specifically, cycling-based sorting requires encapsulation of the microbatteries, either in wafer form or after cutting and housing, in order to avoid, among other things, structural changes associated with the presence of metallic lithium and sensitivity to air. Intermediate sorting to reduce manufacturing costs and identify fault modes is not possible, and this is exactly what is needed in this case.
[0011] Patent document US 9209496 proposes a sorting method consisting in measuring the open circuit voltage or OCV of the battery, discharging it for a certain period of time and comparing the potential at the end of the discharge with the potential of the OCV. In the case of "Li-free" microbatteries, this sorting method proves to be unsuitable because (i) the OCV does not provide an indication of the state of the battery, and (ii) discharging a "Li-free" battery does not allow the potential to be corrected in a stable manner so that the microbattery is fully discharged during the test.
[0012] Patent document US6526361 proposes a sorting method that consists in applying a number of successive pulses (either current or voltage pulses) with a relaxation period between each pulse on the battery, measuring the associated voltage response, and performing sorting based on this response. This approach is not applicable to "Li-free" microbatteries, since it requires an initial state that is stable in terms of voltage.
[0013] The publications "A comparative study of sorting methods for lithium-ion batteries" by Xiaoyu Li et al., XP032671721 and "Fundamentals, impedance, and performance of solid-state Li-metal microbatteries" by Collins John et al., XP012247065 disclose methods for sorting lithium-ion batteries. [Prior art documents] [Patent documents]
[0014] [Patent Document 1] U.S. Patent No. 9,209,496 [Patent Document 2] U.S. Patent No. 6,526,361 [Non-patent literature]
[0015] [Non-Patent Document 1] J.Electrochem.Soc.-2000-Neudecker-517-23 [Non-patent document 2] A comparative study of sorting methods for Lithium-ion batteries, Xiaoyu Li et al, XP032671721 [Non-patent document 3] Fundamentals, impedance, and performance of solid-state LI-metal microbatteries, Collins John et al, XP012247065 Summary of the Invention [Problem to be solved by the invention]
[0016] In this context, and in order to overcome the problems mentioned above, the present invention relates to a test method particularly well suited for "Li-free" microbatteries, which are not compatible with known prior art methods, which allows to carry out non-degrading and rapid tests, and which may also be applied to one device or to multiple devices tested in parallel. [Means for solving the problem]
[0017] More precisely, the present invention is directed to the deposition of Li on a metal that is inert to lithium ions. + A method for testing at least one energy microstorage device comprising an anode made of metallic lithium formed by electrodeposition of ions, an electrolyte, and a cathode, said method comprising a sequence of testing steps during the manufacture of said anode, said sequence comprising: - a step Ph-a of measuring, at time t0, the initial voltage of said device in open circuit mode in order to obtain a value of the initial voltage OCV of said energy micro-storage device; if the initial voltage is not zero, applying a current Ib for a time tb to charge a first portion of the 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, a first charging step Ph-b, in which the determination of the internal resistance Rb is related to the considered state of charge of the device; - The voltage Vb is within a defined interval Vb based on the architecture of the component min ~Vb max and the resistance Rb is within the interval Rb defined based on the architecture of the component. min ~Rb max If it is within continuing to apply at least one current Ic for a time tc to charge a second portion of the 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; a stabilization step Ph-c, which comprises - The voltage Vc is determined based on the architecture of the component and is within a defined interval Vc min ~Vc max If it is within applying zero current for a time td; Measuring the voltage V across the device over time; determining a parameter Vd, where Vd=ΔV / Δt; Including, Vd is the interval Vd defined based on the architecture of the component min ~Vd max If the device is within A holding step Ph-d, Includes.
[0018] According to some variants of the invention, a first charging step comprising a series of measurements of the voltage Vbi for a period Δtbi at intervals of time Tbi in order to determine the curve Vbi as a function of time and to determine the value of the voltage Vb, which may be defined as the maximum value of the voltage Vbi or the average value of the voltage Vbi; The resistance Rb can be determined after each time tbi by the ratio Vbi / Ic of the curves Vbi as a function of time t.
[0019] According to some variants of the invention, the period Δtbi is of the order of 10 seconds and the time Tbi is of the order of 0.1 seconds.
[0020] According to some variants of the invention, the first thickness is of the order of a few nanometers, preferably between 1 and 2 nanometers.
[0021] According to some variants of the invention, A stabilization step comprises a series of measurements of the voltage Vci during periods Δtci spaced apart by times Tci to determine the value of the voltage Vc, defined as the mean value of the voltage Vci.
[0022] According to some variants of the invention, the periods Δtci are of the order of 50 seconds and the times Tci are of the order of 1 second.
[0023] According to some variants of the invention, the second thickness is less than 10 nanometers and preferably equal to 5 nanometers.
[0024] According to some variants of the invention, the holding step comprises a series of measurements of the voltage Vdi for a period Δtdi at intervals of time Tdi to determine the curve Vdi as a function of time; The parameter Vd is determined by the slope of the curve Vdi as a function of time t.
[0025] According to some variants of the invention, the period Δtdi is of the order of 10 seconds and the time Tdi is of the order of 1 second.
[0026] The present invention also provides a system for testing at least one energy micro-storage device implementing the testing method of the present invention, comprising: - a current generator connected to said device; - a voltmeter connected to said device; a control device connected to said current generator and said voltmeter.
[0027] According to some variations of the invention, the current generator is programmable and the voltmeter is programmable.
[0028] According to some variations of the invention, the control device includes a timer, a memory, and a processor.
[0029] The present invention also relates to an assembly of a plurality of systems for testing energy micro-storage devices implementing the method according to the invention, each system comprising: a current generator connected to said device, possibly programmable; a possibly programmable voltmeter connected to said device, - for the assembly of several systems, each current generator and each voltmeter being connected to a control device.
[0030] The present invention also relates to an assembly of a plurality of systems for testing energy micro-storage devices implementing the testing method according to the invention, each system comprising: a current generator connected to said device, possibly programmable; a possibly programmable voltmeter connected to said device, - for the assembly of several systems, each current generator and each voltmeter being connected to the same central control device.
[0031] According to some variations of the invention, the test system is such that each controller or central controller includes a timer, a memory and a processor.
[0032] The test system of the present invention includes a memory, and each control device manages the test phase for each test system, and a central control device records the voltage measurement results in the memory of each control device, and the central control device records the measurement results in its own memory. collect The system may include a central control unit.
[0033] The invention will be better understood and other advantages will become apparent on reading the following description, given without limitation, and by means of the accompanying drawings, in which: [Brief explanation of the drawings]
[0034] [Figure 1]The variation of the OCV, more precisely the Henry diagram, of a microbattery component manufactured in a batch of seven wafers, whose ordinate is the nominal function of x, is illustrated and is described in detail in the literature accessible via the following link: http: / / www.modulad.fr / numero-35 / Excelense-grenier-35 / DiagrammedeHenry.pdf. [Figure 2] 1 illustrates the evolution of the terminal voltage of a microbattery device as a function of time throughout the steps of a testing method according to the present invention. [Figure 3] 1 illustrates a flow chart including all of the successive testing phases in a testing method according to the present invention. [Figure 4] 1 illustrates an example of a system for testing multiple energy micro-storage devices according to the present invention, each device connected to a controller. [Figure 5] 1 illustrates an example of a system for testing multiple energy micro-storage devices according to the present invention, each connected to the same central controller. DETAILED DESCRIPTION OF THE INVENTION
[0035] Generally, the testing method proposed in this invention aims to overcome the various above-mentioned drawbacks by using a non-degrading, rapid testing technique that can be advantageously applied to a single device or to multiple devices tested in parallel.
[0036] The test method of the present invention uses the test sequence described below, which allows concluding as early as possible about a faulty device by chaining the various steps together after checking the decision criteria in the previous steps.
[0037] Energy micro-storage devices are hereafter referred to as micro-batteries.
[0038] It will be described in relation to an example of a lithium-based microbattery including a metal anode, possibly made of a metal, e.g., made of titanium, and possibly including a solid electrolyte, e.g., made of LiPON (lithium phosphate oxynitride), and a cathode, possibly made of, e.g., LiCoO2.
[0039] This technique is advantageous because it applies four phases to each device under test that are triggered in sequence when validation criteria are met. These four phases, described below, are referred to as the initial OCV voltage measurement phase, the charge phase, the stabilization phase, and the hold phase. Figure 2 illustrates the chaining of these phases together by showing the evolution of the voltage across the device under test as a function of time in one example of a method described in more detail below.
[0040] This testing phase sequence is described in detail later in this specification and is also illustrated by the flow chart shown in FIG.
[0041] The test system may be implemented on a device, or several test systems may be implemented in parallel on a set of devices. The means used to implement the inventive test method, according to a first variant of the invention, may in particular be the following means for testing each device Dn, only one of which is shown in Figure 4: These means include a programmable current generator An, a programmable voltmeter Vn, and a control device Cn. The device Dn has an anode connection Dn-anode and a cathode connection Dn-cathode, the current generator An has a positive connection An-H and a negative connection An-L, and the voltmeter has a positive connection Vn-H and a negative connection Vn-L.
[0042] The test method involves performing testing of a microbattery device by connecting the current generator connection An-H, the voltmeter connection Vn-H with the microbattery device connection Dn-anode, and connecting the current generator connection An-L, the voltmeter connection Vn-L with the same microbattery device connection Dn-cathode. This basic system can be repeated multiple times to test multiple devices.
[0043] Each basic system can be driven by a control device Cn including a processor Pn, a timer Crn and a memory Mn, which is connected to each voltmeter Vn and each current generator An and is an integral part of the system, as also shown in Figure 4. In this case, all of the control devices Cn of the multiple test systems are themselves connected to a central control device Cc to drive all of the test systems. This configuration has the advantage of increasing the flexibility of the algorithms used and making them easier to implement.
[0044] According to another variant of the invention, as shown in FIG. 5, multiple systems can be driven by a central control unit Cc including a timer Crc and a memory Mc connected to all voltmeters Vn and all current generators An.
[0045] The control means can therefore be provided by a central control device or by a set of individual control devices. In either case, the control device used contains in its memory Mn or Mc the characteristic times at which voltage measurements are carried out by the voltmeter Vn and time measurements are carried out by the timer Crn or timer Crc. The control device used records these time and voltage measurements in its memory Mn or Mc.
[0046] If there is only a central control unit Cc, it manages the test sequences of the multiple test systems and records the measurement results in its memory Mc. If there is a control unit Cn associated with each test system, each control unit Cn manages the test sequences of each test system and records the measurement results in its memory Mn, and then the central control unit stores all the measurement results. collect and records them in its memory Mc.
[0047] The test method according to the present invention begins with a first phase Ph-a, which involves measuring the initial voltage OCV of each device using a voltmeter Vn connected to each device. These measurements are recorded in the memory Mn of each control device Cn of each system or in the memory Mc of the central control device Cc, respectively. This first phase makes it possible to obtain the parameter OCV (open circuit voltage) of each device, for example, based on the voltage measurement at this time t0. Only a measurement value equal to zero is useful in the case of "Li-free" microbatteries, since this indicates a short-circuit mode failure and makes it possible to stop testing the component in question. Phase Ph-a, continued in the flowchart of FIG. 3, illustrates this first phase, which can be conclusive and allows testing of the defective device to be stopped.
[0048] Then, during the second phase Ph-b, called the charging phase, each current generator An connected to each device Dn applies a current Ib to each device starting at time t0. This current allows a minimal portion of the device to be charged, which has the effect of not damaging the device. More specifically, this action is performed by Li + It consists in initiating the transfer of ions and forming a continuous nanometer-thick (e.g., 1-2 nm) lithium layer at the anode, thus changing it from a "Li-free" to a metallic Li configuration without structurally affecting the component, which makes it possible to ensure both the relevance of subsequent sorting and the possibility of carrying out this sorting at any point in the manufacturing process.
[0049] This second phase makes it possible to obtain the parameter Vb, for example by extracting the maximum voltage obtained from the measurements recorded during this phase. The component determines whether the voltage Vb falls within an interval V defined based on the architecture of the component. bmin ~V bmax If it is within the interval V, it is considered to be a match. bmin ~V bmax is essentially defined by the redox couple involved, more specifically by the potential of the cathode (or positive electrode) relative to an electrode made of metallic lithium. For example, in the case of a cathode made of LiCoO2, this interval corresponds to 3.85-3.89 V, whereas for Li4Ti5O 12 For a cathode made with , this interval corresponds to 1.4 to 1.6 V. Phase Ph-b, carried over in the flowchart of FIG. 3, illustrates this second phase, which can be confirmatory and allows testing to continue or stop if devices that do not meet expectations are deemed non-compliant.
[0050] Next, during the third phase Ph-c, called the stabilization phase, the charging phase Ph-b process continues for different predetermined times, which can be, for example, 50 seconds at 1-second intervals, during which the current generators An connected to each device Dn continue to apply a current Ic (which can be equal to Ib) to each device Dn. This step aims to adjust the nanometer Li layer thickness to the requirements of the electrical test. Several thicknesses may be useful. The maximum sufficient thickness can typically be less than 10 nm, preferably less than 5 nm. Note that the total thickness of metallic lithium to be used in the case of complete cycling corresponds to 5000 nm, and the fraction used for the test is approximately 1 / 1000.
[0051] This is a major benefit of the method as it allows validation testing to be performed from the very beginning of the formation of the metallic lithium electrode, and does not require the manufacturing process to be terminated in order for the microbattery device to be testable.
[0052] This third phase makes it possible to obtain the parameter Vc, for example by taking the average of the voltage values obtained from the measurements recorded during this phase. The component determines whether the parameter Vc is measured within an interval V, defined based on the architecture of the component. cmin ~V cmax If it is within the range, it is considered to be in conformance. cmin ~V cmax The determination of Ic* time is essentially related to the theoretical variation of the potential of the microbattery after injecting an amount of charge corresponding to Ic* time. This amount is very small (less than 0.1% of the total charge the microbattery can store) and for a functional microbattery, V cmin ~V cmax The value of V bmin ~V bmax The potential difference between the two ranges is substantially similar (+ / - 10%) to the value of . In the case of a non-functional microbattery, the difference between the two potential ranges will be greater. Phase Ph-c, continued in the flowchart of Figure 3, illustrates this third phase, which can be confirmatory, making it possible to continue or stop the test if a device that does not meet the expected value is considered non-compliant.
[0053] During this phase, other parameters can be considered, such as the slope, i.e., delta V. cmin ~V cmax ) / Ic gives an estimate of the internal resistance of the microbattery in exactly this state of charge, and in the same way, V cmin and V cmax The difference, or ratio, between V cmin / V cmaxcan provide information about the charging kinetics of the microbattery. Then, during a fourth phase Ph-d, called the holding phase, the current generators apply zero current, and the process of phases Ph-b and Ph-c continues for a predetermined time, for example, 10 seconds, with 1-second intervals. This fourth phase makes it possible to obtain the parameter Vd, for example, by extracting the slope (derivative) of the voltage versus time curve obtained from measurements recorded during this phase. The component determines whether the parameter Vd is measured within a defined interval V based on the component's architecture. dmin ~V dmax If it is within the range, it is considered compliant. Phase Ph-d included in the flowchart of Figure 3 illustrates this fourth phase, which makes it possible to conclude that the device under test is compliant. This phase makes it possible to evaluate the kinetics and relaxation amplitude of the microbattery after the preceding charging phase. Ideally, the relaxation is limited to a drop in potential corresponding to Ic * Rint (internal resistance), a value that is very small in view of the low current Ic used. Ideally: Vb=Vc=Vd.
[0054] All previously obtained parameters may also be processed using statistical laws to characterize multiple elements.
[0055] With the exemplary predetermined value given in phases Ph-a to Ph-d being 1 minute 10 seconds, the test method according to the invention is advantageous since it makes it possible to obtain a set of parameters characterizing several devices at once on the currently manufactured devices (directly on the wafer) and to do this without destroying the devices, and then to terminate the manufacturing steps. [Explanation of symbols]
[0056] An electric current generator An-H positive connection An-L negative connection Cc Central Control Unit Cn control device Crc Timer Crn Timer Dn Device Ib current IC current MC Memory Mn Memory Ph-a measurement steps Ph-b First charging step Ph-c stabilization step Ph-d retention step Pn Processor Rb internal resistance Rb min ~Rb max interval Rint Internal resistance t time t0 time tb time Tbi Time tc time Tci time td time Tdi time V Voltage Vb min ~Vb max interval Vc min ~Vc max interval Vd min ~Vd max interval Vb voltage Vbi voltage Vc voltage Vci voltage Vd parameter Vdi curve Vn voltmeter Vn-H positive connection Vn-L negative connection △tbi period △tci period △tdi period
Claims
1. Li on a metal inactive to lithium ions + 1. A method for testing at least one energy microstorage device comprising an anode made of metallic lithium formed by electrodeposition of ions, an electrolyte, and a cathode, the method comprising a sequence of testing steps during the manufacture of the anode comprised in the energy microstorage device, the sequence comprising: a step (Ph-a) of measuring, at time t0, the initial voltage (OCV) of said energy micro-storage device in open circuit mode in order to obtain the value of said initial voltage of said energy micro-storage device; if said initial voltage is not zero, applying a current Ib for a time tb to charge a first portion of the energy micro-storage device for a first charging time so as to form a first lithium layer thickness at the anode; measuring the voltage Vb across the terminals of said energy micro-storage device, determining therefrom the internal resistance Rb of the energy micro-storage device; a first charging step (Ph-b); - the voltage Vb between the terminals is min ~Vb max When the internal resistance Rb is within the interval Rb min ~Rb max If it is within continuing to apply at least one current Ic for a time tc to charge a second portion of the energy micro-storage 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 energy micro-storage device; a stabilization step (Ph-c) comprising: - the voltage Vc between the terminals is min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of said energy micro-storage device over time; determining a parameter Vd, where Vd=ΔV / Δt; ○ Vd is the interval Vd min ~Vd max the energy micro-storage device is tested as valid if a holding step (Ph-d); A method comprising:
2. the first charging step comprises a series of measurements of the measured voltage for a period Δtbi at intervals of time Tbi in order to determine the curve of the voltage as a function of time and to determine the value of the voltage Vb across its terminals, which may be defined as the maximum of the measured voltages or as the average of the measured voltages; the internal resistance Rb can be determined after each time tbi by the ratio Vbi / Ic of the curves Vbi as a function of time t, where Ic is the at least one current; 10. A method for testing at least one energy micro-storage device according to claim 1.
3. 3. The method for testing at least one energy micro-storage device according to claim 2, wherein said period Δtbi is on the order of 10 seconds and said time Tbi is on the order of 0.1 seconds.
4. 3. The method for testing at least one energy micro-storage device according to claim 1 or 2, wherein the thickness of the first lithium layer is on the order of a few nanometers, or between 1 nanometer and 2 nanometers.
5. A method for testing at least one energy micro-storage device according to any one of claims 2 to 4, wherein the stabilization step comprises a series of measurements of the measured voltage for a period Δtci, spaced apart by a time Tci, in order to determine a value of the terminal voltage Vc defined as the average value of the measured voltages.
6. 6. The method for testing at least one energy micro-storage device according to claim 5, wherein said period Δtci is on the order of 50 seconds and said time Tci is on the order of 1 second.
7. A method for testing at least one energy micro-storage device according to any one of claims 1 to 6, wherein the thickness of said second lithium layer is less than 10 nanometers or equal to 5 nanometers.
8. said holding step comprises a series of measurements of the measured voltage for a period Δtdi at intervals of time Tdi in order to determine the curve of the voltage as a function of time; said parameter Vd is determined by the slope of said voltage curve as a function of time t; A method for testing at least one energy micro-storage device according to any one of claims 1 to 7.
9. 9. The method for testing at least one energy micro-storage device according to claim 8, wherein said period Δtdi is on the order of 10 seconds and said time Tdi is on the order of 1 second.
10. The method of claim 1, wherein Li is deposited on a metal inactive to lithium ions. + 1. A system for testing at least one energy micro-storage device, the system implementing a method for testing at least one energy micro-storage device comprising an anode made of metallic lithium formed by electrodeposition of ions, an electrolyte, and a cathode, the method for testing comprising a sequence of testing steps during the fabrication of the anode, the sequence comprising: a step (Ph-a) of measuring, at time t0, the initial voltage (OCV) of the energy micro-storage device in open circuit mode to obtain said value; if said initial voltage is not zero, applying a current Ib for a time tb to charge a first portion of the energy micro-storage device for a first charging time so as to form a first lithium layer thickness at the anode; measuring the voltage Vb across the terminals of said energy micro-storage device, determining the internal resistance Rb; a first charging step (Ph-b); - the voltage Vb between the terminals is min ~Vb max When the internal resistance Rb is within the interval Rb min ~Rb max If it is within continuing to apply at least one current Ic for a time tc to charge a second portion of the energy micro-storage 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 energy micro-storage device; a stabilization step (Ph-c) comprising: - the voltage Vc between the terminals is min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of said energy micro-storage device over time; determining said parameter Vd, where Vd=ΔV / Δt; ○ Vd is the interval Vd min ~Vd max the energy micro-storage device is tested as valid if a holding step (Ph-d); Including, said system for testing comprising: a current generator connected to said energy micro-storage device; a voltmeter connected to said energy micro-storage device; a control device connected to said current generator and to said voltmeter; 1. A system for testing, comprising:
11. 11. The system for testing of claim 10, wherein the current generator is programmable and the voltmeter is programmable.
12. 12. The system for testing according to claim 10 or 11, wherein the control device comprises a timer, a memory, and a processor.
13. 10. An assembly of a plurality of systems for testing energy micro-storage devices (Dn) implementing the method according to any one of claims 1 to 9, each system comprising: a current generator (An) connected to said energy micro-storage device (Dn); a voltmeter (Vn) connected to said energy micro-storage device (Dn), An assembly of several systems, each current generator (An) and each voltmeter (Vn) connected to a control device (Cn).
14. The method of claim 1, wherein Li is deposited on a metal inactive to lithium ions. + 1. An assembly of a plurality of systems for testing energy micro-storage devices (Dn), implementing a method for testing at least one energy micro-storage device comprising an anode made of metallic lithium formed by electrodeposition of ions, an electrolyte and a cathode, said method for testing comprising a sequence of testing steps during the manufacture of said anode, said sequence comprising: a step (Ph-a) of measuring, at time t0, the initial voltage (OCV) of the energy micro-storage device in open circuit mode to obtain said value; if said initial voltage is not zero, applying a current Ib for a time tb to charge a first portion of the energy micro-storage device for a first charging time so as to form a first lithium layer thickness at the anode; measuring the voltage Vb across the terminals of said energy micro-storage device, determining the internal resistance Rb; a first charging step (Ph-b); - the voltage Vb between the terminals is min ~Vb max When the internal resistance Rb is within the interval Rb min ~Rb max If it is within continuing to apply at least one current Ic for a time tc to charge a second portion of the energy micro-storage 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 energy micro-storage device; a stabilization step (Ph-c) comprising: - the voltage Vc between the terminals is min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of said energy micro-storage device over time; determining said parameter Vd, where Vd=ΔV / Δt; ○ Vd is the interval Vd min ~Vd max the energy micro-storage device is tested as valid if a holding step (Ph-d); Each system includes: a current generator (An) connected to said energy micro-storage device (Dn); a voltmeter (Vn) connected to said energy micro-storage device (Dn), each current generator (An) and each voltmeter (Vn) is connected to the same central control unit (Cc); Assembly of multiple systems.
15. 15. The system for testing of claim 14, wherein each controller or the central controller includes a timer, a memory, and a processor.
16. 16. A system for testing according to claim 15, comprising a central control unit (Cc) including a memory (Mc), each control unit (Cn) managing the test phase for each test system and recording voltage measurement results in the memory (Mn) of each control unit (Cn), and retrieving the voltage measurement results so as to record them in its own memory (Mc).
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