Method for testing one or more micro-battery devices and system implementing test method

JP2022013743A5Active Publication Date: 2025-05-14COMMISSARIAT A LENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES
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Patent Information

Application Number
JP2021097798
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2020-07-01
Filing Date
2021-06-11
Publication Date
2025-05-14
Estimated Expiration
2041-06-11

AI Technical Summary

Technical Problem

Existing methods for testing 'Li-free' microbatteries are inadequate as they require cycling, which causes structural changes and sensitivity to air, making intermediate sorting difficult and costly, and existing electrical parameters like OCV and internal resistance are not suitable for reliable classification.

Method used

A non-degrading, rapid testing method involving sequential phases: measuring initial OCV, charging to form a lithium layer, stabilizing, and evaluating voltage parameters to determine device compatibility without damaging the microbattery.

Benefits of technology

Enables reliable, rapid sorting of 'Li-free' microbatteries at any stage of manufacturing, reducing costs and identifying faults without structural changes, using parameters that correlate with the battery's state of charge and performance.

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Abstract

To provide a method for testing one or more micro-battery devices and a system implementing the test method.SOLUTION: The present invention relates to a method for testing at least one energy micro-storage device. The method includes a series of steps performed during manufacture of an anode, comprising: a step of measuring an initial voltage OCV of the energy micro-storage device; a first charging step including applying current and measuring a voltage and an internal resistance of the device in order to verify that measurement values are in conformity, with thickness of a very thin lithium layer formed on the anode; a second charging stabilization step including applying current and measuring the voltage of the device in order to verify that a measurement value is in conformity, with thickness of the thin lithium layer formed on the anode; and a holding step of applying zero current and measuring the voltage in order to confirm that the energy micro-storage device is in conformity.SELECTED DRAWING: Figure 2
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Description

[Technical Field]

[0001] The field of this invention is the field of electrical testing of electronic or scientific and technological devices manufactured using microelectronics technology, namely integrated circuits, sensors, and basic devices (resistors, diodes, capacitors, etc.).

[0002] More specifically, it includes electrical test methods dedicated to a particular category of energy microstorage components, commonly known as microbatteries. [Background technology]

[0003] Microbatteries are manufactured by continuously 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 seal it by depositing an additional layer or adding a cover.

[0004] Generally, microbatteries can be classified into three categories depending on the type of negative electrode (or anode), which is often deposited on top of the electrolyte. - Li + Anodes made from ion storage materials: These often contain transition metal oxides (Vox, TiOx, NiOx, etc.) or crystal-forming materials (Si, Ge, C, or mixtures). - Anode made of metallic lithium: A lithium layer is deposited on the current collector in metallic form. - Anode made of a lithium-inert metal: This configuration is often referred to as "Li-free," with reference to the paper J.Electrochem.Soc.-2000-Neudecker-517-23. In this case, the anode made of metallic lithium contains Li (emitted 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 final configuration is most advantageous for microbatteries integrated into a silicon substrate and when using microfabrication techniques. This configuration provides the presence of lithium metal (which is the most effective anode due to its energy density, potential, and cyclability) without the drawbacks associated with the presence of lithium metal during the process (sensitivity to air, etching, and incompatibility with photolithography solutions).

[0006] Generally, the most commonly used and reliable sorting and electrical testing protocols are (i) testing microbatteries over multiple full charge-discharge cycles (from full charge to full discharge), and (ii) comparing capacity values, voltage profiles, and internal resistances to reference values.

[0007] However, this method has several limitations. In the context of microbatteries, more specifically in the context of "Li-free" microbatteries, cycling leads to variations in the structure of the active stack, in this case the formation of metallic lithium, which becomes highly sensitive to air and difficult to control in the technical manufacturing process.

[0008] For larger batteries, this method is still very rarely applied because it requires a longer testing period, which means considerable costs.

[0009] Sorting can be based on one or more parameters of the microbattery without the need to cycle the microbatteries. The most commonly used electrical parameters include: - Open-circuit voltage, or OCV. This voltage corresponds to the voltage measured in the microbattery before electrical operation at the end of manufacturing. This voltage generally indicates the charge state of the microbattery. This is verified, for example, in the case of microbatteries fabricated with metallic lithium or storage anodes. In the case of "Li-free" microbatteries, experiments have shown that the OCV exhibits large variability both within a single wafer and between wafers, and no correlation was found between the OCV and the charge state, as shown in Figure 1 illustrating the OCV variation of microbattery components manufactured in a batch of seven wafers. The variability is large both within a single wafer and between wafers. - The variability is related to the fact that the lithium-based anode no longer forms at this stage, and the OCV measurement provides only information about the state of the electrolyte / electrode interface, without relating to the charge state or future electrical behavior. Consequently, this parameter is not suitable for establishing all sorting of microbattery configurations. - Internal resistance: This corresponds to the contribution of all resistance occurring within the structure of the microbattery, and is the sum of the resistance of the electrolyte and the charge transfer within and at the electrodes. This parameter is not suitable for sorting in the case of "Li-free" microbatteries for the same reasons explained above, as an anode made of metallic lithium is not formed.

[0010] The challenge of sorting in this case is precisely to have the electrical parameters necessary to classify microbatteries, including "Li-free" microbatteries, without forcing the execution of cycling, even at the risk that sorting can only be performed after the end of the manufacturing process. Specifically, to avoid structural changes associated with the presence of metallic lithium and sensitivity to air, sorting based on cycling requires the microbatteries to be sealed either on the wafer or after being cut and placed in a housing. This reduces manufacturing costs and makes it impossible to perform intermediate sorting to identify fault modes, which is precisely what is needed in this case.

[0011] U.S. Patent Document 9,209,496 proposes a sorting method that involves measuring the open-circuit voltage (OCV) of a battery, discharging it for a certain period of time, and comparing the potential at the end of the discharge with the OCV. In the case of "Li-free" microbatteries, this sorting method is clearly unsuitable because (i) the OCV does not provide an indication of the battery's state, and (ii) discharging a "Li-free" battery does not allow for a stable correction of the potential so that the microbattery is completely discharged during the test.

[0012] U.S. Patent Publication No. 6,526,361 proposes a sorting method comprising applying a series of consecutive pulses (either current pulses or voltage pulses) with a relaxation period between each pulse to a battery, measuring the associated voltage response, and performing sorting based on this response. Because this method requires a stable initial state with respect to voltage, it is not applicable to "Li-free" microbatteries.

[0013] The documents "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

Patent Document 2

Non-Patent Documents

[0015]

Non-Patent Document 1

Non-Patent Document 2

Non-Patent Document 3

Summary of the Invention

Problems to be Solved by the Invention

[0016] In this context, and to overcome the problems described above, the present invention relates to a test method particularly well suited to "Li-free" microbatteries that is incompatible with known prior art methods. This method enables non-degrading and rapid testing, and the method may also be applied to a single device or to multiple devices being tested in parallel. [Means for solving the problem]

[0017] More precisely, the present invention relates to Li on a metal inert to lithium ions. + A method for testing at least one energy microstorage device comprising an anode made of metallic lithium formed by electrodepositing ions, an electrolyte, and a cathode, wherein the method includes a sequence of test steps during the fabrication of the anode, the sequence of which is: - To obtain the value of the initial voltage OCV of the energy microstorage device, step Ph-a is performed to measure the initial voltage of the device in open-circuit mode at time t0, - If the initial voltage is not zero, ○ To charge the first part of the device for a minimum charging time such that the thickness of the first lithium layer is formed at the anode, a current Ib is applied for a period of time tb. This includes measuring the terminal voltage Vb of the aforementioned device, The determination of the internal resistance Rb is related to the charge state of the device under consideration, in a first charging step Ph-b, - Voltage Vb is defined based on the architecture of the components. min ~Vb max This is the case when the resistor Rb is within the interval Rb defined based on the architecture of the component. min ~Rb max If it is inside, ○ To charge the second part of the device during a second charging time tc, such that the thickness of the second lithium layer is formed at the anode, at least one current Ic is continuously applied for a period of time tc. Measuring the voltage Vc between the terminals of the device; including a stabilization step Ph-c; - When the voltage Vc is within the interval Vc min ~Vc max defined based on the architecture of the component, applying zero current for a time td; measuring the voltage V between the terminals of the device over time; determining a parameter Vd, where Vd = △V / △t; including; - When Vd is within the interval Vd min ~Vd max defined based on the architecture of the component, the device is tested as being valid; a holding step Ph-d; including.

[0018] According to some variations of the present invention, - A first charging step includes a series of measurements of the voltage Vbi during a period △tbi within an interval of time Tbi to determine a curve Vbi as a function of time and to determine a value of the voltage Vb that can be defined as the maximum value of the voltage Vbi or the average value of the voltage Vbi; - The resistance Rb can be determined by the ratio Vbi / Ic of the curve Vbi as a function of time t after each time tbi.

[0019] According to some variations of the present invention, the period △tbi is on the order of 10 seconds and the time Tbi is on the order of 0.1 seconds.

[0020] According to some variations of the present invention, the first thickness is on the order of a few nanometers, preferably from 1 nanometer to 2 nanometers.

[0021] According to some variations of the present invention, - The stabilization step includes a series of measurements of the voltage Vci during a period Δtci at time intervals Tci to determine the value of the voltage Vc, which is defined as the average value of the voltage Vci.

[0022] According to some modifications of the present invention, the period Δtci is on the order of 50 seconds, and the time Tci is on the order of 1 second.

[0023] According to some modifications of the present invention, the second thickness is less than 10 nanometers, preferably equal to 5 nanometers.

[0024] According to some variations of the present invention, - The holding step includes a series of measurements of the voltage Vdi during the period Δtdi at intervals of time 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.

[0025] According to some modifications of the present invention, the period △tdi is on the order of 10 seconds, and the time Tdi is on the order of 1 second.

[0026] The present invention also provides a system for testing at least one energy microstorage device that implements the test method of the present invention, - A current generator connected to the aforementioned device, - A voltmeter connected to the aforementioned device, - The present invention relates to a system including the current generator and a control device connected to the voltmeter.

[0027] According to some modifications of the present invention, the current generator is programmable and the voltmeter is programmable.

[0028] According to some modifications of the present invention, the control device includes a timer, memory, and a processor.

[0029] The present invention also provides an assembly of multiple systems for testing an energy microstorage device implementing the method according to the present invention, wherein each system is - A current generator connected to the device, which may be programmable in some cases, - Including, in some cases a programmable voltmeter connected to the device, - This relates to an assembly of multiple systems, each of which is connected to a control device.

[0030] The present invention also provides an assembly of multiple systems for testing energy microstorage devices that implement the test method according to the present invention, wherein each system is - A current generator connected to the device, which may be programmable in some cases, - Including, in some cases a programmable voltmeter connected to the device, - This relates to an assembly of multiple systems in which each current generator and each voltmeter is connected to the same central control unit.

[0031] According to some modifications of the present invention, the test system is configured such that each control unit or central control unit includes a timer, memory, and a processor.

[0032] The test system of the present invention includes a central control unit that includes a memory, where each control unit manages the test phase for each test system, and where each control unit records voltage measurement results in the memory of each control unit, and the central control unit may include a central control unit that recovers the measurement results so that the measurement results are recorded in its own memory.

[0033] The present invention will be better understood and other advantages will become apparent by reading the following description, which is provided without limitation, and by looking at the accompanying drawings. [Brief explanation of the drawing]

[0034] [Figure 1]The variation in OCV of microbattery components manufactured in a batch of seven wafers, more precisely illustrated as a Henry graph, where the vertical axis of the figure is a Normit function of x, 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] The gradual change in the terminal voltage of the microbattery device as a function of time over all steps of the test method according to the present invention is illustrated. [Figure 3] A flowchart illustrating all the consecutive test phases in the test method according to the present invention is shown. [Figure 4] An example of a system for testing multiple energy microstorage devices according to the present invention is illustrated, with each device connected to a control device. [Figure 5] An example of a system for testing multiple energy microstorage devices according to the present invention is illustrated, with each device connected to the same central control unit. [Modes for carrying out the invention]

[0035] In general, the test methods proposed in this invention aim to overcome various of the aforementioned drawbacks by using non-degrading and rapid test techniques. Advantageously, this technique can be applied to a single device or to multiple devices being tested in parallel.

[0036] The test method of the present invention uses the test sequence described later, and after confirming the judgment criteria in the previous step, it chains various steps together to enable conclusions about defective devices as early as possible.

[0037] Energy microstorage devices will henceforth be referred to as microbatteries.

[0038] This is described in relation to an example of a lithium-based microbattery, which in some cases includes a metal anode made of a metal, for example, titanium, and in some cases a solid electrolyte made of, for example, LiPON (lithium oxynitride phosphate), and in some cases a cathode made of, for example, LiCoO2.

[0039] This technique is advantageous because it applies four phases to each device under test, which are triggered sequentially when the confirmation criteria are met. These four phases, described later, are called the initial OCV voltage measurement phase, the charging phase, the stabilization phase, and the holding phase. Figure 2 illustrates how these phases are chained together by showing the gradual change in the terminal voltage of the device under test as a function of time in an example of the method described in more detail below.

[0040] The sequence of this testing phase is described in detail in the following sections of this specification and is also illustrated by the flowchart shown in Figure 3.

[0041] The test system may be implemented on a device, or multiple test systems may be implemented in parallel on a set of devices. The means used to implement the test method of the present invention, according to a first modification of the present invention, specifically for testing each device Dn, can be the following means, of which only one of these devices Dn is shown in Figure 4. These means include a programmable current generator An, a programmable voltmeter Vn, and a control device Cn. Device Dn has an anode connection Dn-anode and a cathode connection Dn-cathode, current generator An has a positive connection An-H and a negative connection An-L, and voltmeter has a positive connection Vn-H and a negative connection Vn-L.

[0042] The test method involves connecting the current generator's connector An-H and the voltmeter's connector Vn-H to the microbattery device's connector Dn-anode, and then connecting the current generator's connector An-L and the voltmeter's connector Vn-L to the same microbattery device's connector Dn-cathode, thereby performing a test on the microbattery device. This basic system can be repeated multiple times to test multiple devices.

[0043] Each basic system can be driven by a control unit Cn, which includes a processor Pn, a timer Crn, and memory Mn. This control unit is connected to each voltmeter Vn and each current generator An, and forms an integrated part of the system, as shown in Figure 4. In this case, to drive all of the test systems, all of the control unit Cn of multiple test systems are themselves connected to a central control unit Cc. This configuration is advantageous in that it improves the flexibility of the algorithms used and makes implementation easier.

[0044] According to another modification of the present invention, as shown in Figure 5, multiple systems can be driven by a central control unit Cc which includes 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 unit or by a set of individual control units. In either case, the control unit used has a memory Mn or Mc containing characteristic time measurements, where voltage measurements are performed by a voltmeter Vn and time measurements are performed by a timer Crn or timer Crc. The control unit used records these time and voltage measurements in its memory Mn or Mc.

[0046] If only a central control unit Cc exists, it manages the test sequences of 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 sequence of each test system and records the measurement results in its memory Mn, and then the central control unit retrieves all the measurement results and records them in its memory Mc.

[0047] The test method according to the present invention begins with a first phase Ph-a, which includes measuring the initial voltage OCV of each device using a voltmeter Vn connected to each device, and these measurements are recorded in the memory Mn of each control unit Cn of each system, or in the memory Mc of the central control unit Cc. This first phase makes it possible to obtain the parameter OCV (open-circuit voltage) of each device based on the voltage measurement at this time t0, for example. Only measurements equal to zero are useful in the case of a "Li-free" microbattery, as this indicates a short-circuit mode malfunction and makes it possible to stop testing on the problematic component. Phase Ph-a, which is followed by the flowchart in Figure 3, illustrates this first phase, which can be confirmed and allows testing of a faulty device to be stopped.

[0048] Next, 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 for charging a minimal portion of the device, which has the effect of not damaging the device. More specifically, this operation is performed by Li + This involves initiating ion migration to form a continuous nanometer-thick (e.g., 1-2 nm) layer of lithium at the anode, thus transforming the material from "Li-free" to a metallic Li configuration without structurally affecting the constituent elements. This ensures both relevance to post-process sorting and the possibility of performing 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 is defined by the interval V based on the architecture of the component. bmin ~V bmax If it is within the range, it is considered to be compatible. Interval V bmin ~V bmax This is essentially defined by the redox pair involved, and 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 3.85-3.89V, compared to Li4Ti5O 12 In the case of a cathode fabricated using this method, this interval corresponds to 1.4-1.6V. Phase Ph-b, which follows in the flowchart of Figure 3, illustrates this second phase, which can be confirmed, allowing testing to continue or stop if a device that does not meet expectations is deemed non-compliant.

[0050] Next, during the third phase Ph-c, called the stabilization phase, the charging phase Ph-b process is continued for different predetermined times, which can be, for example, 50 seconds at 1-second intervals, with each current generator An connected to each device Dn continuously applying a current Ic (which may be equal to Ib) to each device Dn. This step aims to adjust the nanometer thickness of the Li layer to suit the requirements of the electrical test. Having several different thicknesses can be beneficial. The maximum sufficient thickness can typically be less than 10 nm, preferably less than 5 nm. Note that the total thickness of metallic lithium used in a complete cycling case corresponds to 5000 nm, and the proportion used for testing is approximately 1 / 1000.

[0051] This is a major advantage of this method, as it makes it possible to perform confirmation testing from the very beginning of the formation of the metallic lithium electrode, eliminating the need to terminate the manufacturing process to allow testing of the microbattery device.

[0052] This third phase makes it possible to obtain the parameter Vc, for example, by extracting the average of the voltage values ​​obtained from the measurements recorded during this phase. The component is defined by the interval V based on the architecture of the component. cmin ~V cmax If it is within the scope, it is considered compliant. V cmin ~V cmax The determination of is essentially related to the theoretical variation in 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 amount of charge the microbattery can store), and for a functional microbattery, V cmin ~V cmax The value of is V bmin ~V bmax The values ​​are substantially similar (+ / -10%). In the case of non-functional microbatteries, the difference between the two potential ranges becomes larger. Phase Ph-c, which follows in the flowchart of Figure 3, illustrates this third phase, which can be confirmed, allowing testing to continue or stop if a device that does not meet the expected values ​​is considered non-compliant.

[0053] During this phase, other parameters, such as the gradient, i.e., delta V, can be considered. Gradient (V cmin ~V cmax The value of ) / Ic can be used to estimate the internal resistance of the microbattery in this charging state, and in the same way, V cmin and V cmax The difference between, or ratio V cmin / V cmaxThis can provide information about the kinetics of microbattery charging. Next, during the fourth phase Ph-d, called the holding phase, the current generators each apply zero current, continuing the processes of phases Ph-b and Ph-c for a predetermined time of 10 seconds, for example, at 1-second intervals. This fourth phase makes it possible to obtain the parameter Vd, for example, by extracting the slope (derivative) of the voltage-time curve obtained from the measurements recorded during this phase. The components determine that the parameter Vd is determined at intervals V defined based on the architecture of the components. dmin ~V dmax If within this range, it is considered conforming. Phase Ph-d, included in the flowchart of Figure 3, illustrates this fourth phase, which allows us to conclude that the device under test is conforming. This phase allows us to evaluate the kinetics and relaxation amplitude of the microbattery after the preceding charging phase. Ideally, relaxation is limited to a potential drop equivalent to Ic*Rint (internal resistance), which is very small in light of the low current Ic used. Ideally, Vb = Vc = Vd.

[0054] To characterize multiple elements, all previously obtained parameters may also be processed using statistical laws.

[0055] If the exemplary predetermined value given in phases Ph-a to Ph-d is set to 1 minute and 10 seconds, the test method according to the present invention is advantageous because it becomes possible to obtain a set of parameters characterizing multiple devices at once on the currently manufactured device (directly on the wafer), and to do so without destroying the device, after which the manufacturing step can be terminated. [Explanation of symbols]

[0056] An electric current generator An-H Plus connection An-L Negative Connection Cc Central Control Unit Cn control unit Crc Timer Crn Timer Dn device Ib current IC current Mc Memory Mn memory Steps to measure pH Ph-b First charging step Ph-c stabilization step Ph-d holding 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 Plus 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, comprising, during the manufacture of the anode, a sequence of testing steps 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 device; if said 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, Determine the internal resistance Rb. a first charging step (Ph-b); said voltage Vb is within a defined interval Vb based on the architecture of the component min ~Vb max and the resistance Rb is within an 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 the device; a stabilization step (Ph-c) comprising: said voltage Vc is within an interval Vc defined based on said architecture of said component; min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of the device over time; determining a parameter Vd, where Vd=ΔV / Δt; Vd is a distance Vd defined based on the architecture of the component min ~Vd max If the device is within a holding step (Ph-d); 10. A method comprising the sequence comprising:

2. the first charging step comprises a series of measurements of the voltage Vbi during a period Δtbi, spaced apart by a time Tbi, in order to determine a 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; said resistance Rb can be determined after each time tbi by the ratio Vbi / Ic of said curves Vbi as a function of time t; The test method of claim 1.

3. 3. A test method 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 testing method according to claim 1, wherein the first thickness is on the order of a few nanometers, preferably between 1 and 2 nanometers.

5. A test method according to any one of claims 2 to 4, wherein the stabilization step comprises a series of measurements of the voltage Vci for a period Δtci, spaced apart by a time Tci, in order to determine the value of the voltage Vc defined as the average value of the voltage Vci.

6. 6. A test method 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. Test method according to any one of claims 1 to 6, wherein said second thickness is less than 10 nanometers, preferably equal to 5 nanometers.

8. said holding step comprises a series of measurements of said voltage Vdi for a period Δtdi at intervals of time Tdi in order to determine the curve Vdi as a function of time; said parameter Vd is determined by the slope of said curve Vdi as a function of time t; The test method according to any one of claims 1 to 7.

9. 9. A test method 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 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 testing method 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 of said device in open circuit mode in order to obtain said value of said initial voltage (OCV) 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 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 the device, determining the internal resistance Rb; a first charging step (Ph-b); said voltage Vb is within an interval Vb defined based on said architecture of said component; min ~Vb max and the resistance Rb is within an 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 the device; a stabilization step (Ph-c) comprising: said voltage Vc is within an interval Vc defined based on said architecture of said component; min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of the device over time; determining said parameter Vd, where Vd=ΔV / Δt; Vd is a distance Vd defined based on the architecture of the component min ~Vd max If the device is within a holding step (Ph-d); Including, the test system 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; 1. A test system comprising:

11. 11. The test system of claim 10, wherein the current generator is programmable and the voltmeter is programmable.

12. 12. The test system of claim 10 or 11, wherein the control device includes 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), possibly programmable, connected to said device (Dn); a voltmeter (Vn), possibly programmable, connected to said 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 testing 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 said value of said initial voltage (OCV) 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 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 the device, determining the internal resistance Rb; a first charging step (Ph-b); said voltage Vb is within an interval Vb defined based on said architecture of said component; min ~Vb max and the resistance Rb is within an 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 the device; a stabilization step (Ph-c) comprising: said voltage Vc is within an interval Vc defined based on said architecture of said component; min ~Vc max If it is within applying zero current for a time td; measuring the voltage V across the terminals of the device over time; determining said parameter Vd, where Vd=ΔV / Δt; Vd is a distance Vd defined based on the architecture of the component min ~Vd max If the device is within a holding step (Ph-d); Each system includes: 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) is connected to the same central control unit (Cc); Assembly of multiple systems.

15. A test system according to any one of claims 10 to 14, wherein each controller or the central controller comprises a timer, a memory and a processor.

16. 16. A test system according to claims 13 and 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 measurements in the memory (Mn) of each control unit (Cn), and recovering the measurements so as to record them in its own memory (Mc).