CN115656235A - Use method of all-solid-state lithium ion in-situ testing device - Google Patents

Abstract

The invention relates to the technical field of battery testing, in particular to a method for using an all-solid-state lithium ion in-situ testing device suitable for neutron diffraction experiments. The temperature control system used in the temperature control system is selected as follows: Titanium-zirconium alloy, because titanium-zirconium alloy has no diffraction peak for neutron diffraction, and the insulation treatment of positive electrode, negative electrode and titanium-zirconium alloy battery shell is made of glass fiber, which will produce tiny messy neutrons after neutron diffraction Diffraction background, which has almost no effect on the regular neutron diffraction signals produced by the positive and negative plates, which is very important for the acquisition of neutron diffraction peaks of the positive and negative plates, and will not affect their signals. In addition, it is not Although the parts in direct contact will affect the material, a layer of shielding device-boron nitride is placed on the periphery, so that the neutrons incident in this direction will be absorbed by the boron nitride and will not generate diffraction signals on the relevant materials.

Description

A method of using an all-solid-state lithium ion in-situ testing device

technical field

The invention relates to the technical field of battery testing, in particular to a method for using an all-solid-state lithium ion in-situ testing device suitable for neutron diffraction experiments.

Background technique

In recent years, with the rapid development of advanced communication terminals, electric vehicles, large-scale energy storage and other fields, the demand for high energy density secondary batteries is very urgent. Among various commercial rechargeable and discharge chemical energy storage devices, lithium-ion batteries have the highest energy density.

Solid-state battery technology is one of the solutions that can achieve high energy density and high safety at the same time. All-solid-state lithium batteries use solid-state electrolytes that do not contain organic solvents, which are non-volatile, non-flammable, stable under high temperature and air conditions, and The advantages of wide electrochemical window, high mechanical strength, and prevention of short circuit caused by lithium dendrites can greatly improve safety; on the other hand, solid-state batteries can use metal lithium as the negative electrode material, which greatly improves the energy density of the battery.

Neutron experimental technology has unique and irreplaceable advantages in the research on the above key scientific issues. Neutrons interact with matter differently than electrons and X-rays. The interaction between neutrons and atomic nuclei is a short-range interaction, and the scattering length has no obvious change law with the atomic number. Therefore, neutron scattering is more sensitive and accurate in detecting light elements (such as hydrogen, lithium, oxygen, etc.) than other methods. In addition, the seed has good penetrability, which is very suitable for non-destructive real-time in-situ characterization of the battery in service and working state. Therefore, neutron technology has irreplaceable unique advantages in the research of solid-state lithium battery materials and devices.

The spallation neutron source is a large-scale research platform for neutron scattering research and application. Provide an advanced research platform on key issues of many major strategic needs.

The neutron scattering spectrometer is a device suitable for neutron scattering experiments, mainly studying the microstructure and motion of matter. This invention is mainly experimented with a general-purpose powder diffraction spectrometer and a small-angle scattering spectrometer.

The General Purpose Powder Diffraction Spectrometer (GPPD) is an elastic scattering spectrometer, which is mainly used to study the crystal structure and magnetic structure of substances. GPPD uses neutron time-of-flight technology, selects the appropriate distance from the moderator to the sample (30m), and has three sets of detectors with different angles. Low-angle detectors (30°) are suitable for determining the structure of larger crystals; high-angle backscatter detectors (150°) are suitable for studies with higher resolution, and the resolution can reach 0.2%; medium-angle detectors (90° ) can effectively avoid the scattering of the sample cavity. Suitable for structural research in special sample environments.

的脉冲中子束，测量样品I(q)-q散射强度曲线，并通过模型拟合获得样品中纳米尺度不均匀结构信息。CSNS 小角散射谱仪采用经典点聚焦针孔相机几何，由准直器和中子光阑限束实现中子束的准直与聚焦。谱仪采用短直束线设计，总长度为16 米，样品到慢化器表面的距离为12米，到探测器(可移动)的距离可在2～4米范围内调整。其测量的Q范围为

可用于探测物质体系在1～100nm尺度内的微观和介观结构。相对于同步辐射，具备独特的衬度变换技术。可通过同位素替代(如氘代)实现对材料结构中某些特殊区域或片段的“标记”和选择性观测。The CSNS small-angle scatterometer is a general-purpose time-of-flight small-angle scatterometer, which uses the

The pulsed neutron beam of the sample is used to measure the I(q)-q scattering intensity curve of the sample, and the nanoscale inhomogeneous structure information in the sample is obtained through model fitting. The CSNS small-angle scattering spectrometer adopts the classic point-focusing pinhole camera geometry, and the neutron beam is collimated and focused by the collimator and the neutron aperture to limit the beam. The spectrometer adopts a short straight beamline design with a total length of 16 meters. The distance from the sample to the surface of the moderator is 12 meters, and the distance from the detector (movable) can be adjusted within the range of 2 to 4 meters. Its measured Q range is

It can be used to detect the microscopic and mesoscopic structure of the material system in the scale of 1-100nm. Compared with synchrotron radiation, it has unique contrast transformation technology. The "marking" and selective observation of some special regions or fragments in the material structure can be achieved by isotope substitution (such as deuterium).

At present, there are few in-situ devices for neutron diffraction experiments on all-solid-state lithium-ion batteries on the market, and the experimental conditions required for all-solid-state lithium-ion batteries in the only device are not covered enough. For example, the patent "A battery in-situ Test Device" (application publication number: CN213658936U), although the patent includes a temperature control system and a charging and discharging system, but it lacks the necessary vacuum environment, and it cannot match the connection device in the sample environment of the general powder spectrometer and the small angle scattering spectrometer Moreover, it is cumbersome to replace, and it has a wide range of applications, resulting in no relevant optimization for neutron diffraction experiments, and the materials selected for some parts will have an adverse effect on neutron diffraction experiments.

There is an urgent need to design a special in-situ test device for neutron diffraction experiments that can be used for all-solid-state lithium-ion batteries. It has a preload effect and can be adapted to different sample sizes.

Contents of the invention

The present invention aims at one or more problems in the prior art, and provides a method for using an all-solid-state lithium ion in-situ testing device suitable for neutron diffraction experiments of all-solid-state lithium-ion batteries.

In one aspect of the present invention, an all-solid-state lithium ion in-situ test device is proposed, which is suitable for in-situ test of all-solid-state lithium-ion batteries in neutron diffraction experiments.

In another aspect of the present invention, a method for using an all-solid lithium ion in-situ test device is proposed, which mainly includes the following steps:

S1: Assemble the battery body in the glove box and take it out of the glove box;

S2: install the heating rod and the thermistor in the top gasket and the bottom gasket of the battery body respectively;

S3: Next, mount the battery body on the lower end of the connecting rod by hooking the top case and the bottom case through the upper compression nut and the lower compression nut to obtain the battery assembly;

S4: The battery assembly is installed on the lower end of the sample rod, and then the upper end of the sample rod is installed on the mounting flange of the connection assembly;

S5: Fix and install the test device as a whole on the six-dimensional adjustment table of the spectrometer sample;

S6: The temperature controller is electrically connected to the heating rod and the thermistor, and then the charging and discharging system is electrically connected to the junction slot, and connected to the PC terminal outside the spectrometer scattering chamber through the data cable.

S7: Start the temperature controller, heat the positive electrode and negative electrode to reach the ambient temperature required for the experiment, start the charge and discharge test system, and leave the scattering room after confirming that it is correct;

S8: Turn on the neutron beamline switch of the spectrometer to realize the conduction of the neutron beam;

S9: According to the predetermined experiment plan, start the experiment and save the relevant data.

In another aspect of the present invention, an application of an all-solid-state lithium ion in-situ test device is proposed, which includes neutron diffraction analysis, which is a special experimental method for neutron diffraction experiments.

The beneficial effects of the present invention are:

1. In the temperature control system used, the material of the parts in contact with the positive electrode and negative electrode is titanium-zirconium alloy, because titanium-zirconium alloy has no diffraction peak for neutron diffraction, and at the same time, the positive electrode, negative electrode and titanium-zirconium alloy battery shell The insulation treatment uses glass fiber, which will produce a tiny messy neutron diffraction background after neutron diffraction, which has almost no effect on the regular neutron diffraction signals produced by the positive and negative electrodes, which will affect the positive and negative electrodes. The acquisition of the neutron diffraction peak is very important, and it will not affect its signal. In addition, although the components that are not in direct contact have an impact material, a layer of shielding device-boron nitride is covered on the periphery, so that the incident direction Neutrons will be absorbed by boron nitride and will not produce diffraction signals on related materials;

2. The connection device used is suitable for the general powder diffraction spectrometer and small angle diffraction spectrometer of China Spallation Neutron Source, and is also suitable for other spectrometers, so as to avoid repeated design of supporting connection devices by experimenters;

3. When replacing the sample, it is not necessary to completely dismantle the battery body. It is only necessary to remove the bottom PEEK compression nut, bottom titanium-zirconium alloy gasket, PEEK insulating sleeve and large O-ring, without other cumbersome operations. ;

4. When the position of the experimental sample is calibrated, the time for the centering of the sample and the neutron beam is less, because before the start of the experiment, the positions of the positive electrode and the negative electrode are calibrated in advance, and lines are drawn outside the battery body to facilitate the adjustment of the spectrum. At the same time, in order not to change the position of the sample when replacing the positive electrode or negative electrode, the small O-shaped sealing ring is installed on the lower part of the top titanium-zirconium alloy, and the insulation between the top titanium-zirconium alloy and the battery case Use the form of sticking Capton tape to prevent the position of the positive or negative electrode from changing;

5. The all-solid-state lithium ion in-situ testing device used in the present invention consists of fewer parts and is convenient for production and processing. The assembly form of the battery device adopts the method of thread and hook, which is easy to operate and is beneficial to the use in actual life and production. , and in order to keep the pressing mechanism in close contact with the surface of the current collector during the charging and discharging process of the battery, the original spring is changed to a thread preloading structure, so as to reduce the number of parts of the battery device and make the overall device more compact;

6. The all-solid-state lithium ion in-situ test device of the present invention is sealed with an O-ring, the upper part uses two small O-rings, and the lower part adopts a large O-ring. At the same time, the charging and discharging of the positive and negative plates And the heating lead is transferred from the electrode itself to the titanium-zirconium alloy gasket in contact with it, eliminating the influence of pores on the sealing performance;

7. The all-solid-state lithium ion in-situ test device of the present invention is matched with a controllable temperature environment and an in-situ charge and discharge device, and the temperature range is 20-100°C, which meets the test environment of most batteries;

8. The operation of replacing positive electrode/negative electrode and positive electrode/negative electrode is realized by matching titanium-zirconium alloy gaskets of different thicknesses.

Description of drawings

Figure 1 is a schematic diagram of the principle architecture of the all-solid-state lithium-ion in-situ test device in use;

Fig. 2 is a structural schematic diagram of an all-solid-state lithium ion in-situ test device;

3 is a schematic isometric side view of the connecting device in the all-solid-state lithium ion in-situ testing device;

4 is a schematic cross-sectional view of a battery body in an all-solid-state lithium ion in-situ testing device;

Fig. 5 is a schematic diagram of the position of the heating rod and the negative electrode junction slot in the all-solid-state lithium ion in-situ test device;

Fig. 6 is a schematic diagram of the position of the thermistor and the positive junction slot in the all-solid-state lithium ion in-situ test device.

Detailed ways

The method of using the all-solid-state lithium ion in-situ testing device of the present invention will be further described in detail below in conjunction with specific embodiments and accompanying drawings.

Example 1

Referring to Fig. 1, a non-limiting embodiment of the present invention is an all-solid-state lithium ion in-situ test device, which is detachably installed on a six-dimensional adjustment table of a spectrometer sample for neutron diffraction analysis. An experimental device dedicated to sub-diffraction experiments.

Referring to Fig. 1, a non-limiting embodiment of the present invention, a kind of all-solid-state lithium ion in-situ testing device specifically comprises sample device 1, detector device 2, temperature control system 3, charging and discharging system 6 and light source 5, and sample device 1 can be It is disassembled and installed on the six-dimensional adjustment table of the sample environment of the spectrometer, the temperature control system 3 is arranged outside the sample device 1, the charging and discharging system 6 is electrically connected with the sample device 1, and the detector device 2 is arranged outside the sample device 1, The light source 5 is used to generate a neutron beam.

Referring to Fig. 2, a non-limiting embodiment of the present invention, the sample device 1 includes a connection assembly 7, a sample rod 15 and a battery assembly 8, the connection assembly 7 is detachably installed on the sample six-dimensional adjustment table of the spectrometer, and the battery assembly 8 passes through the sample The rod and 15 communicate with the connection assembly 7;

In addition, the length of the sample rod 15 depends on the height between the six-dimensional adjustment stage of the sample environment of the spectrometer and the central beam line of the spectrometer.

Referring to FIG. 3 , a non-limiting embodiment of the present invention, the connection assembly 7 includes an annular connection flange 9 and a mounting flange 10 for installing a sample rod, and the connection assembly 7 is detachably installed on the spectrum through the connection flange 9 On the six-dimensional adjustment table of the instrument sample, the installation flange 10 is installed at the center of the ring of the connection flange 9, and the outer diameter of the installation flange 10 is equal to the inner diameter of the connection flange 9 to improve the sealing performance; then, the installation method The flange 10 is provided with a guide portion 14 that facilitates the installation of the sample rod 15, and at least two small eyebolts 11 and guide pins 12 are respectively provided on the upper surface of the mounting flange 10 for fixing and installing the sample rod on the mounting flange 10. The upper surface of the connecting flange 9 is provided with at least two large lifting eye screws 13 for moving the connecting flange 9 .

With reference to Fig. 4, a non-limiting embodiment of the present invention, battery assembly 8 comprises top shell 19, link bar 21, battery body and bottom shell 17, and the top of top shell 19 is provided with for link bar 21 to protrude outward from top shell 19 The through hole, the inner diameter of the through hole is equal to the outer diameter of the link rod 21, and the end of the link rod 21 is an open groove, the outer diameter of which is less than or equal to the inner diameter of the top case 19, so that the top case 19 can be hooked on the end of the link rod 21 In order to improve the sealing performance of the battery assembly 8, one end of the link rod 21 communicates with the sample rod 15, and the other end presses against the upper part of the battery body through the upper compression nut 20, and the bottom case 17 passes through the lower compression nut 16 Compress the lower part of the battery body, and at the same time, the battery body is arranged between the top case 19 and the bottom case 17; then, the battery body includes a shell 18, a top gasket 22, a bottom gasket 29, an insulating sleeve 28, a positive electrode sheet 25, Negative electrode sheet 24 and glass fiber 26, one end of casing 18 is pressed against the lower end of link rod 21 by upper compression nut 20, and the other end is pressed on bottom case 17 by lower compression nut 16, then, top gasket 22 and the bottom gasket 29 are detachably installed in the shell 18, and are arranged between the upper compression nut 20 and the lower compression nut 16; the positive electrode sheet 25, the negative electrode sheet 24 and the glass fiber 26 are arranged on the top gasket 22 and the bottom gasket 29, and the glass fiber 26 is wrapped on the outside of the positive electrode sheet 25 and the negative electrode sheet 24; more specific description: the top gasket 22 and the negative electrode sheet are arranged from top to bottom in the casing 18 24. Positive plate 25 and bottom gasket 29.

In the process of this embodiment, it should be noted that: both the top case 19 and the bottom case 17 are made of boron nitride; the connecting rod 21 is made of aluminum; The compression nut 16 is made of PEEK; the top gasket 22 and the bottom gasket 29 are both titanium-zirconium alloy gaskets.

Referring to FIG. 4 , in a non-limiting embodiment of the present invention, at least one O-ring is provided between the top gasket 22 and the bottom gasket 29 and the housing 18, and an insulating sleeve 28 is provided between the bottom gasket 19 and the housing 18. , for the sake of clarity, at least two O-shaped upper sealing rings 23 are arranged between the top gasket 22 and the casing 18 , and at least one O-shaped lower sealing ring 27 is arranged between the bottom gasket 29 and the casing 18 . Further speaking: the insulating sleeve 28 is stepped, and adopts PEEK, and is wrapped on the outside of the bottom gasket 29, so the lower sealing ring 27 is arranged between the step of the insulating sleeve 28 and the step of the shell 18, and the top The side of the gasket 22 is provided with a groove for embedding the sealing ring 23, and the glass fiber 26 is wrapped on the outside of the negative electrode sheet 24 and the positive electrode sheet 25 to isolate the contact between the negative electrode sheet 24 and the positive electrode sheet 25 and the casing.

It can be seen that the top gasket 22, the bottom gasket 29 and the casing 18 jointly form a sealed cavity for providing the sample environment conditions for the positive electrode sheet 25 and the negative electrode sheet 24 vacuum requirements, and the top gasket 22, the bottom gasket 29 The connection with the housing 18 is vacuum-tight through an insulating sleeve 28 , an upper sealing ring 23 and a lower sealing ring 27 .

Therefore, before the battery assembly 8 is assembled, it is necessary to carry out the calibration work at the sample place, first determine the position of the lower surface of the top 22, that is, the position of the upper surface of the negative electrode sheet 24, and draw the same position on the outer surface of the casing 18. Line operation, which is the reference for rough adjustment of the position of the battery assembly 8, and finally the fine adjustment is carried out through the signal received by the detector device 2 after the neutron diffraction of the positive electrode sheet 25 and the negative electrode sheet 24 inside the battery assembly 8.

Those skilled in the art can easily understand that the top shell (top boron nitride) 19 and the bottom shell (bottom boron nitride) 17 together constitute the shielding body of the battery assembly 8, which is used to shield the positive electrode sheet 25 and the negative electrode sheet 24. The neutron diffraction signal produced by other materials avoids the influence on the neutron diffraction background. The parts and components of the battery assembly 8 close to the positive electrode sheet 25 and the negative electrode sheet 24 are selected from titanium-zirconium alloy except glass fiber 26, so that the neutron diffraction peak is almost is zero, the glass fiber 26 will produce a tiny messy neutron diffraction background after neutron diffraction, which can hardly affect the regular neutron diffraction signals produced by the positive electrode sheet 25 and the negative electrode sheet 24, and the PEEK insulating sleeve 28, Although the lower sealing ring 27 and the upper sealing ring 23 affect the background of neutron diffraction, there are boron nitride 17 and 19 outside them, which will absorb neutrons and will not generate neutron signals.

In addition, the insulation treatment between the top gasket 22 and the casing 18 is also pasted with Capton tape, and the insulation between the casing 18 and the positive electrode sheet 25 and the negative electrode sheet 24 is realized by glass fiber 26, and both the upper and lower ends of the casing PEEK compression nuts 20 and 16 are used for compression, and they all have an insulating effect to prevent accidental touch by the experimenter during the experimental test and cause danger.

1 to 6, a non-limiting embodiment of the present invention, the temperature control system 3 includes a temperature controller, a heating rod 30 and a thermistor 33, the heating rod 30 is arranged on the top gasket, and the thermistor 33 is arranged on the bottom On the gasket, the temperature controller is electrically connected with the heating rod 30 and the thermistor 33 respectively. The temperature controller does not need an additional power supply, and can be directly connected to the civil electricity through a plug.

Referring to FIG. 5 , which is a non-limiting embodiment of the present invention, the top gasket 22 is provided with a first groove for installing a heating rod 30 and a negative terminal slot 31 for a lead wire of the negative electrode sheet 24 .

Correspondingly, the connecting rod 21 is provided with a lead hole for electrically connecting with the lead wire of the heating rod 30 and the negative junction groove 31.

Referring to FIG. 6 , which is a non-limiting embodiment of the present invention, the bottom gasket 29 is provided with a second groove for installing a thermistor 33 and a positive connection slot 32 for the lead wire of the positive electrode sheet 25 .

Referring to Figures 1 to 6, a non-limiting embodiment of the present invention, the heating rod 30 heats the positive electrode sheet 25 and the negative electrode sheet 24 respectively by means of heat transfer to reach the temperature required for the reaction, and the temperature continues to transfer, through the thermistor 33 Realize feedback adjustment to ensure the sample ambient temperature needs.

1 to 6, the thermistor 33 is a platinum thermal resistance.

Referring to Figures 1 to 6, the temperature range of the temperature controller is 20°C to 100°C.

Referring to Figures 1 to 6, the charging and discharging system 6 includes a battery testing system and a PC terminal 4 electrically connected to the battery testing system. Charge and discharge conditions and test content are set.

Referring to FIG. 1 , the detector device 2 is used to receive the signal from the light source 5 scattered/diffraction by the cell.

Example 2

Based on solid-state lithium-ion battery testing, the method of using the above-mentioned all-solid-state lithium-ion in-situ testing device mainly includes the following steps,

S1: In the glove box, put the shell, top gasket, bottom gasket, positive electrode sheet, negative electrode sheet, glass fiber, insulating sleeve, upper compression nut, lower compression nut, upper sealing ring and lower sealing ring, etc. Assemble the battery body and take it out of the glove box;

S2: Install the heating rod 30 and the thermistor 33 of the temperature control system 3 in the top gasket 22 and the bottom gasket 29 respectively, and connect the positive terminal slot 32 in the top gasket 22 and the negative electrode in the bottom gasket 29 The slots 31 are respectively connected with the charge and discharge system 6, and the link rod 21 is connected with the battery assembly 8 through thread fit;

S3: The top boron nitride 19 and the bottom boron nitride 17 are respectively mounted on the lower end of the link rod 21 through the upper compression nut 20 and the lower compression nut 16 to obtain the battery assembly 8;

S4: The battery assembly 8 is threadedly connected to the lower end of the sample rod 15 through the link rod 21, and the upper end of the sample rod 15 is installed on the mounting flange 10 of the connection assembly 7 through the guide part;

S5: The experimenter fixed and installed the test device as a whole on the six-dimensional adjustment table of the sample environment of the spectrometer;

S6: The temperature controller is electrically connected to the heating rod 30 and the thermistor 33 respectively, and then, the charging and discharging system 6 is electrically connected to the positive junction slot 32 and the negative junction slot 31 respectively, and is connected to the outside of the spectrometer scattering chamber through the data line PC terminal 4 for connection;

S7: Start the temperature controller, heat the positive electrode sheet 25 and the negative electrode sheet 24 to reach the ambient temperature required for the experiment, start the charging and discharging system 6, and leave the scattering chamber after confirming that it is correct;

S8: Turn on the neutron beamline switch of the spectrometer to realize the conduction of the neutron beam;

S9: According to the predetermined experiment plan, start the experiment and save the relevant data.

Referring to Figures 1 to 6, compared with the prior art, the method for using the all-solid lithium ion in-situ testing device of the present invention has the following beneficial effects:

1. In the temperature control system used, the material of the parts in contact with the positive electrode and negative electrode is titanium-zirconium alloy, because titanium-zirconium alloy has no diffraction peak for neutron diffraction, and at the same time, the positive electrode, negative electrode and titanium-zirconium alloy battery shell The insulation treatment uses glass fiber, which will produce a tiny messy neutron diffraction background after neutron diffraction, which has almost no effect on the regular neutron diffraction signals produced by the positive and negative electrodes, which will affect the positive and negative electrodes. The acquisition of the neutron diffraction peak is very important, and it will not affect its signal. In addition, although the components that are not in direct contact have an impact material, a layer of shielding device-boron nitride is covered on the periphery, so that the incident direction Neutrons will be absorbed by boron nitride and will not produce diffraction signals on related materials;

2. The connection device used is suitable for the general powder diffraction spectrometer and small angle diffraction spectrometer of China Spallation Neutron Source, and is also suitable for other spectrometers, so as to avoid repeated design of supporting connection devices by experimenters;

3. When replacing the sample, it is not necessary to completely dismantle the battery body. It is only necessary to remove the bottom PEEK compression nut, bottom titanium-zirconium alloy gasket, PEEK insulating sleeve and large O-ring, without other cumbersome operations. ;

4. When the position of the experimental sample is calibrated, the time for the centering of the sample and the neutron beam is less, because before the start of the experiment, the positions of the positive electrode and the negative electrode are calibrated in advance, and lines are drawn outside the battery body to facilitate the adjustment of the spectrum. At the same time, in order not to change the position of the sample when replacing the positive electrode or negative electrode, the small O-shaped sealing ring is installed on the lower part of the top titanium-zirconium alloy, and the insulation between the top titanium-zirconium alloy and the battery case Use the form of sticking Capton tape to prevent the position of the positive or negative electrode from changing;

5. The all-solid-state lithium ion in-situ testing device used in the present invention consists of fewer parts and is convenient for production and processing. The assembly form of the battery device adopts the method of thread and hook, which is easy to operate and is beneficial to the use in actual life and production. , and in order to keep the pressing mechanism in close contact with the surface of the current collector during the charging and discharging process of the battery, the original spring is changed to a thread preloading structure, so as to reduce the number of parts of the battery device and make the overall device more compact;

6. The all-solid-state lithium ion in-situ test device of the present invention is sealed with an O-ring, the upper part uses two small O-rings, and the lower part adopts a large O-ring. At the same time, the charging and discharging of the positive and negative plates And the heating lead is transferred from the electrode itself to the titanium-zirconium alloy gasket in contact with it, eliminating the influence of pores on the sealing performance;

7. The all-solid-state lithium ion in-situ test device of the present invention is matched with a controllable temperature environment and an in-situ charge and discharge device, and the temperature range is 20-100°C, which meets the test environment of most batteries;

8. The operation of replacing positive electrode/negative electrode and positive electrode/negative electrode is realized by matching titanium-zirconium alloy gaskets of different thicknesses.

In describing the present invention, it is to be understood that terms such as "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top" , "bottom", "inner", "outer" and other indicated orientations or positional relationships are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying the referred device Or that an element must have a particular orientation, be constructed and operate in a particular orientation, and thus should not be construed as limiting the invention.

In the present invention, unless otherwise clearly specified and limited, terms such as "installation", "connection", "connection" and "fixation" should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection , or integrated; it can be mechanically connected or electrically connected; it can be directly connected or indirectly connected through an intermediary, and it can be the internal communication of two components or the interaction relationship between two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in the present invention according to specific situations.

The above-mentioned embodiments are only specific embodiments of the present invention, and their descriptions are relatively specific and detailed, but should not be construed as limiting the patent scope of the present invention. It should be noted that, for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present invention, and these obvious replacement forms all belong to the protection scope of the present invention.

Claims (3)

1. The utility model provides an all solid-state lithium ion normal position testing arrangement which characterized in that: the testing device is suitable for in-situ testing of the all-solid-state lithium ion battery for neutron diffraction experiments.

2. The use method of the all-solid-state lithium ion in-situ test device is characterized by comprising the following steps of:

s1: assembling a battery body in the glove box, and taking the battery body out of the glove box;

s2: respectively installing a heating rod and a thermistor in a top gasket and a bottom gasket of a battery body;

s3: then, the top shell and the bottom shell are hung and mounted at the lower end of the chain connecting rod through an upper compression nut and a lower compression nut to obtain a battery assembly;

s4: the battery assembly is arranged at the lower end of the sample rod, and then, the upper end of the sample rod is arranged on the mounting flange of the connecting assembly;

s5: the whole testing device is fixedly arranged on a spectrometer sample six-dimensional adjusting table;

s6: the temperature controller is respectively electrically connected with the heating rod and the thermistor, and then, the charging and discharging system is electrically connected with the wiring slot and is connected with a PC end outside the spectrometer scattering chamber through a data line.

S7: starting a temperature controller, heating the positive plate and the negative plate to reach the environmental temperature required by the experiment, starting a charge-discharge testing system, and leaving a scattering chamber after confirming no error;

s8: opening a neutron beam switch of the spectrometer to realize conduction of neutron beams;

s9: the experiment was started according to a predetermined experimental protocol and the relevant data was saved.

3. The application of the all-solid-state lithium ion in-situ testing device is characterized by comprising neutron diffraction analysis, wherein the all-solid-state lithium ion in-situ testing device is a special experimental device for neutron diffraction experiments.

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