CN115656235A - Use method of all-solid-state lithium ion in-situ testing device - Google Patents
Use method of all-solid-state lithium ion in-situ testing device Download PDFInfo
- Publication number
- CN115656235A CN115656235A CN202211259407.7A CN202211259407A CN115656235A CN 115656235 A CN115656235 A CN 115656235A CN 202211259407 A CN202211259407 A CN 202211259407A CN 115656235 A CN115656235 A CN 115656235A
- Authority
- CN
- China
- Prior art keywords
- solid
- lithium ion
- state lithium
- neutron
- battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to the technical field of battery testing, in particular to a use method of an all-solid-state lithium ion in-situ testing device suitable for a neutron diffraction experiment, wherein a component material in a temperature control system, which is in contact with a positive plate and a negative plate, is selected from titanium-zirconium alloy, the titanium-zirconium alloy has no diffraction peak on neutron diffraction, and simultaneously glass fibers are adopted for insulating the positive plate, the negative plate and a titanium-zirconium alloy battery shell, and can generate a tiny disordered neutron diffraction background after the neutron diffraction, so that regular neutron diffraction signals generated by the positive plate and the negative plate are hardly influenced, the acquisition of the neutron diffraction peaks of the positive plate and the negative plate is vital, the signals cannot be influenced, and in addition, the component which is not in direct contact can influence the materials, but a layer of shielding device-boron nitride is covered on the periphery, so that neutrons incident to the direction can be absorbed by the boron nitride, and diffraction signals cannot be generated on related materials.
Description
Technical Field
The invention relates to the technical field of battery testing, in particular to a using method of an all-solid-state lithium ion in-situ testing device suitable for a neutron diffraction experiment.
Background
With the rapid development of the fields of advanced communication terminals, electric vehicles, large-scale energy storage and the like in recent years, the demand for high-energy-density secondary batteries is very urgent. Among the various commercially available rechargeable electrochemical energy storage devices, lithium ion batteries possess the highest energy density.
The all-solid-state lithium battery adopts a solid electrolyte without containing an organic solvent, has the advantages of non-volatility, nonflammability, stability under the conditions of high temperature, air and the like, wide electrochemical window, high mechanical strength, short circuit prevention caused by lithium dendrites and the like, and can greatly improve the safety; on the other hand, the solid-state battery can adopt metal lithium as a negative electrode material, so that the energy density of the battery is greatly improved.
Neutron experimental techniques have unique and irreplaceable advantages in the research of the above-mentioned key scientific problems. Neutrons act in a different manner than electrons and X-rays. The interaction of neutrons with atomic nuclei is a short-range interaction, the scattering length of which does not change significantly with atomic number. Thus, neutron scattering is more sensitive and accurate in detecting light elements (e.g., hydrogen, lithium, oxygen, etc.) than other methods. In addition, the seeds have good penetrability and are very suitable for performing real-time in-situ characterization of the non-destructive battery service in the working state. Therefore, the neutron technology has irreplaceable unique advantages in the research of solid lithium battery materials and devices.
The spallation neutron source is a large-scale research platform for neutron scattering research and application, and provides an advanced research platform for advanced research in fields of material science and technology, physics, chemistry and chemical engineering, resource environment, new energy, life science, medicine, nano science and the like and key problems for solving the requirements of a plurality of national major strategies.
The neutron scattering spectrometer is suitable for a neutron scattering experiment device, and is mainly used for researching the microstructure and the motion of a substance. The invention mainly performs experiments on a general powder diffraction spectrometer and a small-angle scattering spectrometer.
General purpose powder diffraction spectrometer (GPPD) belongs to elastic scattering spectrometer, mainly used for studying crystal structure and magnetic structure of substance. GPPD uses a time-of-flight technique of neutrons, selects the appropriate moderator-to-sample distance (30 m), and has three sets of detectors at different angles. A low angle detector (30 °) suitable for determining the structure of larger crystals; the high-angle backscatter detector (150 ℃) is suitable for the research with higher resolution, and the resolution can reach 0.2%; the medium angle detector (90 °) can effectively avoid scattering of the sample cavity. Is suitable for structural research in special sample environment.
The CSNS small angle scatterometer is a general-purpose time-of-flight small angle scatterometer, which utilizes the light emitted from a coupled liquid hydrogen moderator
The scattering intensity curve of the sample I (q) -q is measured, and the nanoscale inhomogeneous structure information in the sample is obtained through model fitting. The CSNS small-angle scattering spectrometer adopts the geometry of a classical point focusing pinhole camera, and realizes the collimation and focusing of neutron beams by a collimator and a neutron diaphragm. The spectrometer is designed with a short straight beam, the total length is 16 m, the distance from the sample to the surface of the moderator is 12 m, and the distance to the detector (movable) can be adjusted within the range of 2-4 m. Measured Q range of
Can be used for detecting the microscopic and mesoscopic structures of a physical system in the scale of 1-100 nm. Compared with synchrotron radiation, the method has a unique contrast transformation technology. "tagging" and selective observation of certain specific regions or segments in the material structure can be achieved through isotopic substitution (e.g., deuteration).
At present, in the market, there are few in-situ devices for performing neutron diffraction experiments on all-solid-state lithium ion batteries, and the experimental conditions required by only devices for all-solid-state lithium ion batteries are not covered enough, for example, in a patent "a battery in-situ testing device" (application publication no: CN 213658936U), although the patent has a temperature control system and a charging and discharging system, the device lacks a necessary vacuum environment, and cannot be matched with a connecting device and is cumbersome to replace in a sample environment of a general powder spectrometer and a small-angle scattering spectrometer, and the application range is wide, so that there is no related optimization for the neutron diffraction experiments, and materials selected by parts of components can adversely affect the neutron diffraction experiments.
It is urgently needed to design a special in-situ testing device for neutron diffraction experiments, which can be used for all-solid-state lithium ion batteries, is simple in sample replacement, has a temperature control system, a charge and discharge system and a vacuum environment, has a pre-pressing effect on positive and negative levels of the batteries, and can adapt to different sample sizes.
Disclosure of Invention
The invention provides a using method of an all-solid-state lithium ion in-situ testing device special for a neutron diffraction experiment of an all-solid-state lithium ion battery, aiming at one or more problems in the prior art.
In one aspect of the invention, an all-solid-state lithium ion in-situ test device is provided, which is suitable for in-situ test of an all-solid-state lithium ion battery of a neutron diffraction experiment.
In another aspect of the present invention, a method for using an all-solid-state lithium ion in-situ test apparatus is provided, which mainly includes the following steps:
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 component 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 component;
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.
In another aspect of the invention, an application of the all-solid-state lithium ion in-situ test device is provided, and the application comprises neutron diffraction analysis, which is an experiment method special for neutron diffraction experiments.
The invention has the beneficial effects that:
1. the adopted temperature control system selects the material of the component contacted with the positive plate and the negative plate as the titanium-zirconium alloy has no diffraction peak for neutron diffraction, and simultaneously, the insulation treatment of the positive plate, the negative plate and the titanium-zirconium alloy battery shell adopts glass fiber, the glass fiber can generate tiny disordered neutron diffraction background after neutron diffraction, the glass fiber hardly has influence on the regular neutron diffraction signals generated on the positive plate and the negative plate, which is vital for obtaining the neutron diffraction peak of the positive plate and the negative plate and can not influence the signals of the positive plate and the negative plate, and in addition, the component which is not in direct contact has influence on the material, but a layer of shielding device-boron nitride is covered on the periphery, so that neutrons incident to the direction can be absorbed by the boron nitride and can not generate diffraction signals on related materials;
2. the adopted connecting device is suitable for a general powder diffraction spectrometer and a small-angle diffraction spectrometer of a Chinese spallation neutron source, is also suitable for other spectrometers, and avoids experimenters from repeatedly designing a matched connecting device;
3. when the sample is replaced, the battery body does not need to be completely removed, only the bottom PEEK compression nut, the bottom titanium-zirconium alloy gasket, the PEEK insulating sleeve and the large O-shaped sealing ring need to be removed, and other complicated operations are not needed;
4. when the position of an experimental sample is calibrated, the time for aligning the sample with a neutron beam is reduced, because the positions of a positive plate and a negative plate are calibrated in advance before the experiment begins, and lines are drawn outside a battery body so as to adjust the environmental displacement table of the spectrometer sample to be aligned, meanwhile, in order to replace the positive plate or the negative plate, the position of the sample is not changed, a small O-shaped sealing ring is arranged at the lower part of the top titanium-zirconium alloy, and the insulation between the top titanium-zirconium alloy and the battery shell adopts a form of sticking a Capton adhesive tape so as to prevent the position of the positive plate or the negative plate from being changed;
5 the invention adopts the full solid state lithium ion in-situ test device which comprises fewer parts and is convenient for production and processing, the battery device adopts a screw thread and hanging mode in the assembly form, is convenient for operation and is beneficial to the use in the following actual life and production, and in order to ensure that the pressing mechanism which keeps close contact with the surface of the current collector in the charging and discharging process of the battery is changed into a screw thread prepressing structure from the original spring, the number of the parts of the battery device is reduced, and the whole device is more compact;
6. the all-solid-state lithium ion in-situ testing device adopts O-shaped sealing rings for sealing, the upper part adopts two small O-shaped sealing rings, the lower part adopts 1 large O-shaped sealing ring, and meanwhile, the charging and discharging of the positive plate and the negative plate and the heating lead are transferred to the titanium zirconium alloy gasket contacted with the positive plate and the negative plate from the electrodes, so that the influence of pores on the sealing performance is eliminated;
7. the all-solid-state lithium ion in-situ testing device disclosed by the invention is matched with a controllable temperature environment and an in-situ charging and discharging device, the temperature range is 20-100 ℃, and the testing environment of most batteries is met;
8. the operation of replacing the positive plate/the negative plate and the positive plate/the negative plate is realized by matching the titanium zirconium alloy gaskets with different thicknesses.
Drawings
FIG. 1 is a schematic diagram of a schematic structure of an all-solid-state lithium ion in-situ testing apparatus;
FIG. 2 is a schematic structural diagram of an all-solid-state lithium ion in-situ testing device;
FIG. 3 is an isometric side view of a connection device in an all-solid-state lithium ion in-situ test device;
fig. 4 is a schematic cross-sectional view of a battery body in an all-solid-state lithium ion in-situ testing apparatus;
FIG. 5 is a schematic diagram of the positions of a heating rod and a negative electrode wiring groove in the all-solid-state lithium ion in-situ testing device;
FIG. 6 is a schematic diagram of the positions of the thermistor and the positive electrode wiring groove in the all-solid-state lithium ion in-situ testing device.
Detailed Description
The following describes in detail a method for using the all-solid-state lithium ion in-situ test apparatus according to the present invention with reference to 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 testing apparatus, which is integrally and detachably mounted on a spectrometer sample six-dimensional adjusting table, is used for neutron diffraction analysis, and is a special experimental apparatus for neutron diffraction experiments.
Referring to fig. 1, a non-limiting embodiment of the present invention is an all-solid-state lithium ion in-situ testing apparatus, which specifically includes a sample apparatus 1, a detector apparatus 2, a temperature control system 3, a charging and discharging system 6, and a light source 5, wherein the sample apparatus 1 is detachably mounted on a spectrometer sample environment six-dimensional adjusting table, the temperature control system 3 is disposed outside the sample apparatus 1, the charging and discharging system 6 is electrically connected to the sample apparatus 1, the detector apparatus 2 is disposed outside the sample apparatus 1, and the light source 5 is used for generating neutron beam current.
Referring to fig. 2, in a non-limiting embodiment of the present invention, the sample apparatus 1 includes a connection assembly 7, a sample rod 15 and a battery assembly 8, the connection assembly 7 is detachably mounted on the spectrometer sample six-dimensional adjustment table, and the battery assembly 8 is connected to the connection assembly 7 through the sample rod and 15;
in addition, the length of the sample rod 15 depends on the height of the spectrometer sample environment between the six-dimensional stage to the center beam streamline of the spectrometer.
Referring to fig. 3, in a non-limiting embodiment of the present invention, the connection assembly 7 includes a circular connection flange 9 and a mounting flange 10 for mounting the sample rod, the connection assembly 7 is detachably mounted on the spectrometer sample six-dimensional adjustment table through the connection flange 9, the mounting flange 10 is mounted at the center of the circular ring of the connection flange 9, and the outer diameter of the mounting flange 10 is equal to the inner diameter of the connection flange 9, so as to improve the sealing performance; then, the mounting flange 10 is provided with a guide portion 14 for facilitating the mounting of the sample rod 15, the upper surface of the mounting flange 10 is respectively provided with at least two small lifting ring screws 11 and guide pins 12 for fixing and mounting the sample rod on the mounting flange 10, and the upper surface of the connecting flange 9 is provided with at least two large lifting ring screws 13 for moving the connecting flange 9.
Referring to fig. 4, in a non-limiting embodiment of the present invention, the battery assembly 8 includes a top case 19, a link rod 21, a battery body and a bottom case 17, a through hole for the link rod 21 to extend outward from the top case 19 is formed at the top of the top case 19, the inner diameter of the through hole is equal to the outer diameter of the link rod 21, the end of the link rod 21 is an open-type groove, the outer diameter of the open-type groove is smaller than or equal to the inner diameter of the top case 19, so that the top case 19 is hung above the end of the link rod 21 to improve the sealing performance of the battery assembly 8, one end of the link rod 21 is connected to the sample rod 15, the other end is pressed against the upper portion of the battery body through an upper pressing nut 20, the bottom case 17 is pressed against the lower portion of the battery body through a lower pressing nut 16, and the battery body is disposed between the top case 19 and the bottom case 17; then, the battery body comprises a shell 18, a top gasket 22, a bottom gasket 29, an insulating sleeve 28, a positive plate 25, a negative plate 24 and glass fibers 26, one end of the shell 18 is pressed against the lower end of the link rod 21 through an upper compression nut 20, the other end of the shell is pressed against the bottom shell 17 through a lower compression nut 16, and then the 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 plate 25, the negative plate 24 and the glass fiber 26 are arranged between the top gasket 22 and the bottom gasket 29, and the glass fiber 26 is coated on the outer sides of the positive plate 25 and the negative plate 24; more specifically, the following description: inside the casing 18 are arranged from top to bottom a top gasket 22, a negative plate 24, a positive plate 25 and a bottom gasket 29.
In the process of this embodiment, it should be noted that: both the top shell 19 and the bottom shell 17 are boron nitride; the chain connecting rod 21 is made of aluminum; the case 18 of the battery body is a titanium zirconium alloy battery case; the upper compression nut 20 and the lower compression nut 16 are made of PEEK; top gasket 22 and 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 disposed between the top gasket 22 and the bottom gasket 29, respectively, and the housing 18, and an insulating sleeve 28 is disposed between the bottom gasket 19 and the housing 18, for clarity, at least two O-ring upper seals 23 are disposed between the top gasket 22 and the housing 18, and at least one O-ring lower seal 27 is disposed between the bottom gasket 29 and the housing 18. Further, the method comprises the following steps: the insulating sleeve 28 is step-shaped, adopts PEEK, and wraps up in the outside of bottom gasket 29, so, lower sealing washer 27 sets up between the step of insulating sleeve 28 and the step of shell 18, and sets up the recess that is used for embedding sealing washer 23 on the top gasket 22 side, and glass fiber 26 cladding is in the outside of negative pole piece 24 and positive pole piece 25 to isolated negative pole piece 24 and the contact of positive pole piece 25 and shell.
It will be appreciated that the top gasket 22, bottom gasket 29 and housing 18 together form a sealed chamber for providing sample environmental conditions for the vacuum requirements of the positive and negative plates 25 and 24, and that the joints between the top gasket 22, bottom gasket 29 and housing 18 provide a vacuum seal via the insulating sleeve 28, upper seal ring 23 and lower seal ring 27.
Therefore, before the assembly of the battery assembly 8 is completed, calibration work at the sample site is required, the position of the lower surface of the top part 22, namely the position of the upper surface of the negative plate 24, is firstly determined, the drawing operation is performed at the same position of the outer surface of the shell 18, the drawing operation is used as a reference for roughly adjusting the position of the battery assembly 8, and finally, fine adjustment is performed through signals received by the detector device 2 after neutron diffraction through the positive plate 25 and the negative plate 24 in the battery assembly 8.
It is easily understood by those skilled in the art that the top case (top boron nitride) 19 and the bottom case (bottom boron nitride) 17 together form a shielding body of the battery assembly 8, which is used for shielding neutron diffraction signals generated by materials other than the positive plate 25 and the negative plate 24 and avoiding the influence on the neutron diffraction background, the component materials of the battery assembly 8 close to the positive plate 25 and the negative plate 24 are titanium-zirconium alloy except the glass fiber 26, so that the neutron diffraction peak is almost zero, the glass fiber 26 generates a tiny disordered neutron diffraction background after neutron diffraction, and can generate regular neutron diffraction signals for the positive plate 25 and the negative plate 24, and the PEEK insulating sleeve 28, the lower sealing ring 27 and the upper sealing ring 23 have the influence on the neutron diffraction background, but the boron nitride 17, 19 outside the PEEK insulating sleeve 27, the lower sealing ring 27 and the upper sealing ring 23 can absorb neutrons and cannot generate neutron signals.
In addition, the insulation treatment between the top gasket 22 and the shell 18 is also adhered with Capton tape, the insulation between the shell 18 and the positive plate 25 and the negative plate 24 is realized by glass fiber 26, and the PEEK compression nuts 20 and 16 are adopted to compress the upper end and the lower end of the shell, so that the PEEK compression nuts have an insulation effect, and the risk caused by mistaken contact of testing personnel during experimental testing is prevented.
Referring to fig. 1 to 6, in 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 disposed on the top pad, the thermistor 33 is disposed on the bottom pad, the temperature controller is electrically connected to the heating rod 30 and the thermistor 33, respectively, and the temperature controller can be directly connected to a household appliance through a plug without an additional power supply.
Referring to fig. 5, in a non-limiting embodiment of the present invention, the top gasket 22 is formed with a first groove for mounting the heating rod 30 and a negative electrode connecting groove 31 for leading the negative electrode tab 24.
Accordingly, the link bar 21 is provided with a lead hole for electrically connecting with the lead wires of the heating rod 30 and the negative electrode wire connecting groove 31.
Referring to fig. 6, in a non-limiting embodiment of the present invention, the bottom spacer 29 is formed with a second recess for mounting a thermistor 33 and a positive terminal groove 32 for a lead wire of the positive electrode tab 25.
Referring to fig. 1 to 6, in a non-limiting embodiment of the present invention, the heating rod 30 heats the positive plate 25 and the negative plate 24 respectively by means of heat transfer to reach the temperature required by the reaction, and the temperature continues to be transferred, and feedback adjustment is implemented by the thermistor 33 to ensure the requirement of the environmental temperature of the sample.
Referring to fig. 1 to 6, the thermistor 33 is a platinum thermistor.
Referring to fig. 1 to 6, the temperature of the temperature controller ranges from 20 ℃ to 100 ℃.
Referring to fig. 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, and meanwhile, the battery testing system is electrically connected to the positive wiring groove 32 and the negative wiring groove 31, respectively, so as to set charging and discharging conditions and test contents.
Referring to fig. 1, a detector arrangement 2 is used to receive the signal scattered/diffracted by the battery from the light source 5.
Example 2
Based on the solid-state lithium ion battery test, the using method of the all-solid-state lithium ion in-situ test device mainly comprises the following steps,
s1: in the glove box, assembling a shell, a top gasket, a bottom gasket, a positive plate, a negative plate, glass fibers, an insulating sleeve, an upper compression nut, a lower compression nut, an upper sealing ring, a lower sealing ring and the like into a battery body, and taking the battery body out of the glove box;
s2: respectively installing a heating rod 30 and a thermistor 33 of the temperature control system 3 in a top gasket 22 and a bottom gasket 29, respectively connecting a positive wiring groove 32 in the top gasket 22 and a negative wiring groove 31 in the bottom gasket 29 with the charging and discharging system 6, and connecting a link rod 21 with the battery assembly 8 through threaded fit;
s3: b, hanging and installing a battery body at the lower end of a chain connecting rod 21 by using top boron nitride 19 and bottom boron nitride 17 through an upper compression nut 20 and a lower compression nut 16 respectively to obtain a battery assembly 8;
s4: the battery assembly 8 is in threaded fit connection with the lower end of the sample rod 15 through a link rod 21, and the upper end of the sample rod 15 is installed on the installation flange 10 of the connection assembly 7 through a guide part;
s5: the experimenter integrally and fixedly installs the testing device on a spectrometer sample environment six-dimensional adjusting table;
s6: the temperature controller is respectively and electrically connected with the heating rod 30 and the thermistor 33, and then the charging and discharging system 6 is respectively and electrically connected with the positive wiring groove 32 and the negative wiring groove 31 and is connected with the PC end 4 outside the spectrometer scattering chamber through a data line;
s7: starting a temperature controller to heat the positive plate 25 and the negative plate 24 to reach the environmental temperature required by the experiment, starting the charge and discharge system 6, and leaving the 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.
Referring to fig. 1 to 6, compared with the prior art, the use method of the all-solid-state lithium ion in-situ test device of the invention has the following beneficial effects:
1. the adopted temperature control system selects the material of the component contacted with the positive plate and the negative plate as the titanium-zirconium alloy has no diffraction peak for neutron diffraction, and simultaneously, the insulation treatment of the positive plate, the negative plate and the titanium-zirconium alloy battery shell adopts glass fiber, the glass fiber can generate tiny disordered neutron diffraction background after neutron diffraction, the glass fiber hardly has influence on the regular neutron diffraction signals generated on the positive plate and the negative plate, which is vital for obtaining the neutron diffraction peak of the positive plate and the negative plate and can not influence the signals of the positive plate and the negative plate, and in addition, the component which is not in direct contact has influence on the material, but a layer of shielding device-boron nitride is covered on the periphery, so that neutrons incident to the direction can be absorbed by the boron nitride and can not generate diffraction signals on related materials;
2. the adopted connecting device is suitable for a general powder diffraction spectrometer and a small-angle diffraction spectrometer of a Chinese spallation neutron source, is also suitable for other spectrometers, and avoids experimenters from repeatedly designing a matched connecting device;
3. when the sample is replaced, the battery body does not need to be completely removed, only the bottom PEEK compression nut, the bottom titanium-zirconium alloy gasket, the PEEK insulating sleeve and the large O-shaped sealing ring need to be removed, and other complicated operations are not needed;
4. when the position of an experimental sample is calibrated, the time for aligning the sample with a neutron beam is reduced, because the positions of a positive plate and a negative plate are calibrated in advance before the experiment begins, and lines are drawn outside a battery body so as to adjust the environmental displacement table of the spectrometer sample to be aligned, meanwhile, in order to replace the positive plate or the negative plate, the position of the sample is not changed, a small O-shaped sealing ring is arranged at the lower part of the top titanium-zirconium alloy, and the insulation between the top titanium-zirconium alloy and the battery shell adopts a form of sticking a Capton adhesive tape so as to prevent the position of the positive plate or the negative plate from being changed;
5 the invention adopts the all solid state lithium ion in-situ test device which comprises fewer parts and is convenient for production and processing, the battery device adopts a screw thread and hanging mode in the assembly form, which is convenient for operation and is beneficial to the use in the actual life and production, and the pressing mechanism which keeps close contact with the surface of the current collector in the charging and discharging process of the battery is changed into a screw thread prepressing structure from the original spring, thereby reducing the number of the parts of the battery device and leading the whole device to be more compact;
6. the all-solid-state lithium ion in-situ testing device adopts O-shaped sealing rings for sealing, two small O-shaped sealing rings are adopted at the upper part, 1 large O-shaped sealing ring is adopted at the lower part, and meanwhile, the charge and discharge of the positive plate and the negative plate and the heating lead are transferred from the electrode to the titanium-zirconium alloy gasket contacted with the electrode, so that the influence of pores on the sealing performance is eliminated;
7. the all-solid-state lithium ion in-situ testing device disclosed by the invention meets the testing environment of most batteries by matching a controllable temperature environment and an in-situ charging and discharging device, wherein the temperature range is 20-100 ℃;
8. the operation of replacing the positive plate/the negative plate and the positive plate/the negative plate is realized by matching the titanium zirconium alloy gaskets with different thicknesses.
In the description of the present invention, it is to be understood that terms such as "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used merely for convenience of description and simplicity of description, but do not indicate or imply that the devices or elements referred to must have specific orientations, be constructed and operated in specific orientations, and thus, are not to be construed as limiting the present invention.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The above embodiments are only specific embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications are possible without departing from the inventive concept, and such obvious alternatives fall within the scope of the 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211259407.7A CN115656235A (en) | 2022-10-14 | 2022-10-14 | Use method of all-solid-state lithium ion in-situ testing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211259407.7A CN115656235A (en) | 2022-10-14 | 2022-10-14 | Use method of all-solid-state lithium ion in-situ testing device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115656235A true CN115656235A (en) | 2023-01-31 |
Family
ID=84987605
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211259407.7A Pending CN115656235A (en) | 2022-10-14 | 2022-10-14 | Use method of all-solid-state lithium ion in-situ testing device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115656235A (en) |
-
2022
- 2022-10-14 CN CN202211259407.7A patent/CN115656235A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Herklotz et al. | A novel high-throughput setup for in situ powder diffraction on coin cell batteries | |
| US9022652B2 (en) | Transmission-geometry electrochemical cell for in-situ scattering and spectroscopy investigations | |
| CN210198962U (en) | High-temperature-resistant Raman/X-ray diffraction in-situ spectrum testing device for lithium battery | |
| CN102980903B (en) | A kind of synchrotron radiation X ray device for analyzing electrode material electrochemical performance and application thereof | |
| Sottmann et al. | Versatile electrochemical cell for Li/Na-ion batteries and high-throughput setup for combined operando X-ray diffraction and absorption spectroscopy | |
| CN109799527B (en) | Neutron energy spectrum measuring device and bunner sphere spectrometer system | |
| KR101359333B1 (en) | Multi-electrode cell test apparatus | |
| CN210198972U (en) | Lithium battery in-situ microscopic imaging device and in-situ high-temperature microscopic imaging device | |
| CN113758949B (en) | Double-tilting TIP (TIP) end applied to research of battery materials by in-situ sample rod under transmission electron microscope | |
| EP3037573A1 (en) | Plating apparatus and sensing device using same | |
| CN219302321U (en) | All-solid-state lithium ion in-situ testing device | |
| CN115656235A (en) | Use method of all-solid-state lithium ion in-situ testing device | |
| CN214252131U (en) | Electrochemical in-situ spectrum testing device with temperature adjustment function | |
| CN211654769U (en) | Sampling type fission ionization chamber | |
| CN112697850A (en) | Can observe electrochemistry testing arrangement of electrode cross section | |
| CN110987978B (en) | Device for in-situ observation of battery pole piece and electrolyte | |
| CN115656236A (en) | All-solid-state lithium ion in-situ testing device | |
| CN115575427A (en) | All-solid-state lithium ion in-situ testing device and using method thereof | |
| CN212301792U (en) | Be used for lithium cell thermal runaway frock | |
| JP2010230355A (en) | Analysis system, electrochemical cell for analysis, and analysis method | |
| CN117258691A (en) | Gas phase reaction tank capable of being used for in-situ high-temperature electrochemical Raman experiment and use method | |
| CN216525538U (en) | Controllable lithium cell normal position X ray diffraction spectrum testing arrangement of temperature | |
| KR20210112238A (en) | Chamber apparatus for xrd measurement of cell | |
| JP6507742B2 (en) | Sample switching device | |
| CN211856411U (en) | X-ray photoelectron spectroscopy electrochemical in-situ cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |