X-ray diffraction imaging and real-time gas analysis method and device

Abstract

The invention relates to an X-ray diffraction imaging and real-time gas analysis method and device, and the device comprises a detachable battery mold, an embedded gas circuit, a heating wire, a heating wire power supply line, an XY displacement platform pedestal, a mass spectrometer, a charging and discharging device, and a diaphragm. A first X-ray window is arranged on the battery mold positive electrode shell, a second X-ray window is arranged on the battery mold negative electrode shell, the XY displacement table base is supported at the bottom of the detachable battery mold, the charging and discharging device is electrically connected with a battery electrode, and the mass spectrometer is communicated with the embedded gas circuit through a pipeline. In the invention, through the cooperation of the detachable battery mold, the X-ray window I / II, the displacement mechanism, the embedded gas path, the gas inlet / outlet hole and the mass spectrometer (OEMS / GCMS), the structural evolution detection and large-area phase scanning imaging of the finished product soft package battery are realized, and the synchronous association of a crystal structure, gas production and the like is achieved.

Description

Technical Field

[0001] This invention relates to the field of electrochemical testing and battery safety diagnosis, specifically to an X-ray diffraction imaging and real-time gas analysis method and apparatus. Background Technology

[0002] With the rapid development of consumer electronics and new energy vehicles, the safety of lithium-ion batteries has become a key focus of the industry. Currently, pouch batteries employ a pad-type structure and can use liquid electrolytes, polymer semi-solid electrolytes, and, in the future, sulfide oxide solid electrolytes. The electrode design of pouch batteries, including current collector layout, electrode loading, uniformity of electrode material distribution, positive electrode particle size, charge / discharge temperature, charge / discharge current density, electrolyte wetting degree, and electrolyte formulation, all significantly impact the performance of pouch batteries. For example, during charge / discharge, uneven electrochemical reactions may occur in the electrode area, leading to localized material utilization imbalances, electrolyte decomposition and gas generation, and lithium plating at the negative electrode. These internal battery material design and manufacturing processes involve numerous important parameters; understanding which specific parameters significantly affect the battery's rate performance and cycle stability is crucial for optimizing battery materials and manufacturing processes.

[0003] Traditional in-situ battery X-ray diffraction devices primarily focus on the structural evolution of materials and lack the capability to detect the structural evolution of finished batteries, such as pouch cells (including liquid, solid, and semi-solid types). Furthermore, traditional in-situ battery X-ray diffraction devices are fixed to X-ray instruments, lacking the ability to scan and image the spatial distribution of phases. While in-situ mass spectrometry can detect gas-producing components, current technologies struggle to simultaneously observe crystal structure evolution, reaction homogeneity, and gas-producing kinetics. More importantly, it cannot be synchronously correlated with the spatial distribution and changes in electrode structures. Therefore, a new in-situ pouch cell testing platform capable of simultaneous multimodal monitoring is needed. Summary of the Invention

[0004] The purpose of this invention is to provide a method and apparatus for X-ray diffraction imaging and real-time gas analysis.

[0005] The objective of this invention is achieved through the following technical solution: an X-ray diffraction imaging and real-time gas analysis device, comprising a detachable battery mold, an embedded gas path, heating wires, a heating wire power supply line, an XY displacement stage base, a mass spectrometer, a charging and discharging device, and a separator. The detachable battery mold is formed by fastening together a positive electrode shell and a negative electrode shell. The positive electrode shell of the battery mold has an X-ray window one, and the negative electrode shell of the battery mold has an X-ray window two. The XY displacement stage base is supported at the bottom of the detachable battery mold. The charging and discharging device is electrically connected to the battery electrodes. The mass spectrometer is connected to the embedded gas path through a pipe. The heating wires are integrated inside the negative electrode shell of the battery mold and electrically connected to the heating wire power supply line. The separator is disposed inside the detachable battery mold and located between the positive and negative electrodes of the battery. This device enables multimodal synchronous measurement of large-area XRD scanning imaging and real-time gas analysis without damaging the battery packaging structure.

[0006] As a further description of the above technical solution:

[0007] A positive electrode tab is fixedly provided on the top left side of the positive electrode shell of the battery mold. A gas inlet hole is provided on the top of the positive electrode shell of the battery mold. A gas outlet hole is provided on the bottom of the positive electrode shell of the battery mold. An embedded gas passage is provided inside the positive electrode shell of the battery mold. The two ends of the embedded gas passage are connected to the gas inlet hole and the gas outlet hole, respectively. A screw hole is provided on the edge of the positive electrode shell of the battery mold. A sealing ring is provided around the edge of the positive electrode shell of the battery mold. An X-ray window is provided at a specific position of the positive electrode shell of the battery mold.

[0008] As a further description of the above technical solution:

[0009] The negative electrode shell of the battery mold is fixedly provided with a negative electrode tab on the top left side. The edge of the negative electrode shell of the battery mold is provided with a screw hole two. The edge of the negative electrode shell of the battery mold is surrounded by a sealing ring. The negative electrode shell of the battery mold is provided with an X-ray window two at a specific position. The heating wires are arranged in a specific distribution shape inside the negative electrode shell of the battery mold. One end of the heating wire power supply line is electrically connected to the heating wires, and the other end extends to the outside of the negative electrode shell of the battery mold.

[0010] As a further description of the above technical solution:

[0011] The XY displacement stage base is equipped with a Y-axis guide rail base plate, the Y-axis guide rail base plate is equipped with a Y-axis guide rail, the X-axis guide rail base plate is slidably connected to the Y-axis guide rail, the X-axis guide rail base plate is equipped with an X-axis guide rail, and the detachable battery mold is fixedly supported on the X-axis guide rail.

[0012] As a further description of the above technical solution:

[0013] Both X-ray window one and X-ray window two are composed of multiple windows spliced ​​together, and the splicing points are provided with PEEK or PTFE support structures;

[0014] As a further description of the above technical solution:

[0015] The embedded gas path, together with the gas inlet and gas outlet holes opened on the positive electrode shell of the battery mold, constitute a gas flow channel. The gas outlet holes are connected to the mass spectrometer through a pipe. The heating wire can achieve a temperature control environment from room temperature to 85°C.

[0016] As a further description of the above technical solution:

[0017] The XY displacement stage base, together with the Y-axis guide rail base plate, Y-axis guide rail, X-axis guide rail base plate and X-axis guide rail, constitutes a displacement mechanism with a movement range of centimeters and a positioning accuracy of micrometers. The materials of X-ray window one and X-ray window two are beryllium, mica, Kapton film, aluminum foil, silicon nitride, sapphire or diamond. The sapphire or diamond window is coated with an Al or Au conductive layer inside.

[0018] An X-ray diffraction imaging and real-time gas analysis method, applied to the aforementioned X-ray diffraction imaging and real-time gas analysis device, includes the following steps:

[0019] S1. Place the soft-pack battery between the positive electrode shell and the negative electrode shell of the battery mold, so that the separator is located between the positive and negative electrodes of the battery. Use screws in screw holes one and two to fasten and fix the positive electrode shell and the negative electrode shell of the battery mold. Use sealing rings to achieve sealing.

[0020] S2. Connect the gas source to the gas inlet through a pipe, and connect the mass spectrometer to the gas outlet through a pipe to complete the connection;

[0021] S3. Connect the charging and discharging device to the positive and negative electrode tabs, and connect the heating wire power supply line to the power supply circuit;

[0022] S4. Start the charging and discharging equipment, charge and discharge the soft-pack battery according to the set parameters, and adjust the internal temperature of the battery mold by heating wires according to the test requirements;

[0023] S5. Start the displacement mechanism corresponding to the XY displacement stage base. Through the coordinated movement of the Y-axis guide rail and the X-axis guide rail, drive the detachable battery mold to move along the X-axis and Y-axis directions, realize the large-area scanning of the X-ray focus at X-ray window one and X-ray window two, collect two-dimensional XRD patterns at each coordinate point, and obtain the XY position coordinates and XRD patterns corresponding to the test time (t).

[0024] S6. The gas discharged through the embedded gas path during the battery charging and discharging process is collected in real time by mass spectrometer. The gas composition is analyzed based on m / Z fragment information to obtain the gas composition corresponding to the test time (t).

[0025] S7. Define the XY coordinate sequence, extract the diffraction peak information in the XRD pattern, draw a two-dimensional diffraction mapping image, and synchronously associate the phase distribution image with the gas component data at the corresponding coordinate points to complete the collaborative analysis of battery structure evolution, phase distribution, gas production behavior, and spatial distribution of each gas component and concentration.

[0026] Compared with the prior art, the advantages of the present invention are as follows:

[0027] 1. In this invention, through the coordinated operation of a detachable battery mold, X-ray window one, X-ray window two and displacement mechanism, as well as embedded gas path, gas inlet hole, gas outlet hole and mass spectrometer (OEMS / GCMS), the detection of the structural evolution of finished soft-pack batteries (including liquid, solid and semi-solid) and large-area scanning imaging of phase spatial distribution are realized. At the same time, the synchronous correlation between crystal structure evolution, reaction uniformity, gas generation kinetics and electrode structure spatial changes is achieved.

[0028] 2. In this invention, the original packaging structure of the soft-pack battery is completely preserved by means of a detachable battery mold design that does not require opening holes or implanting reference electrodes, a temperature control function for heating wires, and a multi-structure adaptability design. This avoids leakage problems during testing, is compatible with batteries of different sizes and systems, and can simulate high-temperature abuse conditions.

[0029] 3. In this invention, the two-dimensional spatial distribution of the phases and the corresponding two-dimensional spatial distribution of the gas components of the soft-pack battery during the charging and discharging process are obtained, and accurate and comprehensive collaborative data are acquired, providing reliable support for optimizing battery materials and processes and improving battery performance. Attached Figure Description

[0030] Figure 1 This is an overall schematic diagram of an X-ray diffraction imaging and real-time gas analysis device according to the present invention;

[0031] Figure 2 This is a schematic diagram of the battery mold and diaphragm structure of an X-ray diffraction imaging and real-time gas analysis device according to the present invention.

[0032] Figure 3 This is a schematic diagram of the positive electrode shell structure of the battery mold of the X-ray diffraction imaging and real-time gas analysis device of the present invention;

[0033] Figure 4 This is a schematic diagram of the negative electrode shell structure of the battery mold of the X-ray diffraction imaging and real-time gas analysis device of the present invention;

[0034] Figure 5 This is a flowchart of the testing method for an X-ray diffraction imaging and real-time gas analysis method according to the present invention;

[0035] Figure 6 This is a flowchart of the gas analysis data processing method of an X-ray diffraction imaging and real-time gas analysis method according to the present invention.

[0036] Label Explanation:

[0037] 1. Positive electrode tab; 2. Gas inlet port; 3. Positive electrode shell of battery mold; 4. Screw hole one; 5. Sealing ring; 6. Gas passage; 7. X-ray window one; 8. Gas outlet port; 9. Negative electrode tab; 10. Heating wire power supply line; 11. Negative electrode shell of battery mold; 12. Screw hole two; 13. Sealing ring; 14. Heating wire; 15. X-ray window two; 16. Y-axis guide rail base plate; 17. Y-axis guide rail; 18. X-axis guide rail base plate; 19. X-axis guide rail; 20. XY displacement stage base; 21. Separator. Detailed Implementation

[0038] The present invention will now be described in detail with reference to the accompanying drawings and embodiments:

[0039] like Figures 1 to 4 The image shows an embodiment of an X-ray diffraction imaging and real-time gas analysis device provided by the present invention. It is suitable for in-situ testing of pouch, solid-state, and semi-solid-state batteries and can simultaneously realize large-area XRD scanning imaging and real-time gas analysis. Its overall structure includes a detachable battery mold, an embedded gas path 6, a heating wire 14, a heating wire power supply line 10, an XY displacement stage base 20, a mass spectrometer (OEMS / GCMS), a charging and discharging device, and a separator 21.

[0040] The detachable battery mold is formed by fastening together a positive electrode shell 3 and a negative electrode shell 11. A positive electrode tab 1 is fixedly provided on the top left side of the positive electrode shell 3. A gas inlet hole 2 is provided at the top, and a gas outlet hole 8 is provided at the bottom. An embedded gas passage 6 is provided inside, with both ends of the embedded gas passage 6 communicating with the gas inlet hole 2 and the gas outlet hole 8 respectively. Screw holes 4 are provided on the edge, and a sealing ring 5 is provided around it. An X-ray window 7 is provided at a specific position. A negative electrode tab 9 is fixedly provided on the top left side of the negative electrode shell 11. The outer edge has a screw hole 12 and a sealing ring 13. An X-ray window 15 is provided at a specific position. Heating wires 14 are arranged in a specific distribution shape inside. One end of the heating wire power supply line 10 is electrically connected to the heating wires 14, and the other end extends to the outside of the negative electrode shell 11 of the battery mold. The separator 21 is set inside the detachable battery mold and is located between the positive and negative electrodes of the battery. The screw hole 4 and the screw hole 12 can be used with screws to fasten and fix the positive electrode shell 3 and the negative electrode shell 11 of the battery mold. The sealing rings 5 ​​and 13 together ensure the sealing effect.

[0041] The XY displacement stage base 20 is supported on the bottom of the detachable battery mold, and a Y-axis guide rail base plate 16 is mounted on it. A Y-axis guide rail 17 is mounted on the Y-axis guide rail base plate 16. An X-axis guide rail base plate 18 is slidably connected to the Y-axis guide rail 17. An X-axis guide rail 19 is mounted on the X-axis guide rail base plate 18. The detachable battery mold is fixedly supported on the X-axis guide rail 19. The XY displacement stage base 20, together with the Y-axis guide rail base plate 16, Y-axis guide rail 17, X-axis guide rail base plate 18 and X-axis guide rail 19, constitutes a complete displacement mechanism. The movement range of this displacement mechanism is at the centimeter level, and the positioning accuracy is at the micrometer level.

[0042] Both X-ray window 7 and X-ray window 15 are composed of multiple windows spliced ​​together, with a PEEK or PTFE support structure at the splicing point. The material can be beryllium, mica, Kapton film, aluminum foil, silicon nitride, sapphire, or diamond. The sapphire or diamond window is coated with an Al or Au conductive layer. The embedded gas path 6, together with the gas inlet 2 and the gas outlet 8, forms a gas flow channel. The gas outlet 8 is connected to the mass spectrometer (OEMS / GCMS) through a pipe. The heating wire 14 can achieve a temperature control environment from room temperature to 85°C. The charging and discharging equipment is electrically connected to the positive electrode tab 1 and the negative electrode tab 9 through a circuit to provide charging and discharging conditions for the battery.

[0043] like Figures 5 to 6 The method for X-ray diffraction imaging and real-time gas analysis using the above-mentioned device includes the following steps:

[0044] S1. Place the soft-pack battery between the positive electrode shell 3 and the negative electrode shell 11 of the battery mold, so that the separator 21 is accurately positioned between the positive and negative electrodes of the battery. Use screw holes 1-4 and 2-12 to fasten and fix the positive electrode shell 3 and the negative electrode shell 11 of the battery mold. Use sealing rings 5 ​​and 13 to seal the device.

[0045] S2. Connect the gas source to the gas inlet port 2 through a pipe, and connect the mass spectrometer (OEMS / GCMS) to the gas outlet port 8 through a pipe to complete the assembly of the gas path system;

[0046] S3. Connect the charging and discharging device to the positive electrode tab 1 and the negative electrode tab 9, and connect the heating wire power supply line 10 to the power supply circuit to ensure stable circuit connection;

[0047] S4. Start the charging and discharging equipment, charge and discharge the soft-pack battery according to the set parameters, and adjust the internal temperature of the battery mold by heating wires according to the test requirements;

[0048] S5. Start the displacement mechanism corresponding to the XY displacement stage base. Through the coordinated movement of the Y-axis guide rail and the X-axis guide rail, drive the detachable battery mold to move along the X-axis and Y-axis directions, realize the large-area scanning of the X-ray focus at X-ray window one and X-ray window two, collect two-dimensional XRD patterns at each coordinate point, and obtain the XY position coordinates and XRD patterns corresponding to the test time (t).

[0049] S6. The gas discharged through the embedded gas path during the battery charging and discharging process is collected in real time by mass spectrometer. The gas composition is analyzed based on m / Z fragment information to obtain the gas composition corresponding to the test time (t).

[0050] S7. Based on the test time and the position of the XY displacement stage, define the XY coordinate sequence, extract the diffraction peak information in the XRD pattern, draw a two-dimensional diffraction imaging (mapping) image, and synchronously associate the phase distribution image with the gas component data at the corresponding coordinate points to complete the collaborative analysis of battery structure evolution, phase distribution, gas generation behavior and spatial distribution of each gas component / concentration.

[0051] Working Principle: The working principle of this invention addresses the shortcomings of traditional in-situ battery X-ray diffraction devices, which only focus on the evolution of material structure and cannot scan and image finished pouch batteries. Furthermore, existing technologies struggle to simultaneously observe crystal structure evolution and gas generation behavior. This invention achieves multi-modal synchronous monitoring through the coordinated operation of various structures. The pouch battery is placed within a detachable battery mold consisting of a positive electrode shell 3 and a negative electrode shell 11. A separator 21 is located between the positive and negative electrodes, ensuring proper separation of the internal electrochemical reactions without affecting the in-situ nature of the overall test. The mold is secured using screw holes 1-4 and 12, and sealing rings 5 ​​and 13 work together to form a reliable seal. This eliminates the need for opening holes or implanting reference electrodes in the pouch battery, preserving its original encapsulation structure and preventing gas or liquid leakage during testing, while maintaining a stable internal environment.

[0052] In the gas path system, the gas output from the gas source enters the embedded gas path 6 through the gas inlet 2. The embedded gas path 6 provides a preset path for gas flow, ensuring that the gas evenly covers the area around the battery. The gas is then discharged through the gas outlet 8. A mass spectrometer (OEMS / GCMS) connected to the gas outlet 8 captures the gas generated during the battery's charging and discharging process in real time. Based on the m / Z fragment information, the gas composition is accurately analyzed, overcoming the limitation of traditional in-situ mass spectrometry, which can only detect the gas-generated components but cannot correlate structural changes. In terms of circuit connection, the charging and discharging device achieves electrical connection with the battery through the positive electrode tab 1 and the negative electrode tab 9. It can simulate the charging and discharging conditions of the battery in actual use according to set parameters. The heating wire power supply line 10 provides stable power support for the heating wire 14. The heating wire 14 can achieve temperature control adjustment from room temperature to 85°C, meeting the simulation requirements of high-temperature abuse conditions and filling the gap in the lack of operating condition simulation capabilities of traditional devices.

[0053] The displacement mechanism consists of an XY displacement stage base 20, a Y-axis guide rail base plate 16, a Y-axis guide rail 17, an X-axis guide rail base plate 18, and an X-axis guide rail 19. It possesses a centimeter-level movement range and micrometer-level positioning accuracy. A detachable battery mold is supported on this displacement mechanism. During testing, the displacement mechanism drives the battery mold to move collaboratively, allowing X-rays to scan the battery over a large area through X-ray window 7 and X-ray window 15. Both X-ray window 7 and X-ray window 15 are made of X-ray-transmitting materials such as beryllium, mica, Kapton film, aluminum foil, silicon nitride, sapphire, or diamond, and are composed of multiple windows spliced ​​together. PEEK or PTFE support structures at the splicing points ensure the structural stability of the windows. The interior of the sapphire or diamond windows is also coated with an Al or Au conductive layer, further improving electrode conductivity and solving the problem of traditional devices fixed to X-ray instruments being unable to scan and image.

[0054] During charging and discharging, X-rays penetrate the window and acquire two-dimensional XRD patterns at each scanning coordinate point. Simultaneously, a mass spectrometer (OEMS / GCMS) continuously analyzes the gas composition. Subsequently, by defining a coordinate sequence, diffraction peak information (including peak intensity, peak ratio, peak area, etc.) is extracted from the XRD pattern to create a two-dimensional diffraction imaging image. The phase distribution image is synchronously correlated with the gas composition data at the corresponding coordinate points, ultimately achieving multimodal synchronous measurement of large-area XRD scanning imaging and real-time gas analysis. This clearly captures the causal relationship between battery electrode structure evolution, phase spatial distribution, and gas generation behavior. It also allows for observation of the spatial non-uniformity of electrode reactions through large-area imaging and is compatible with pouch cells of different sizes and systems, providing comprehensive and accurate data support for optimizing battery material design and manufacturing processes.

Claims

1. An X-ray diffraction imaging and real-time gas analysis apparatus, characterized by: The device includes a detachable battery mold, an embedded gas path (6), heating wires (14), a heating wire power supply line (10), an XY displacement stage base (20), a mass spectrometer, a charging and discharging device, and a separator (21). The detachable battery mold is formed by fastening together a positive electrode shell (3) and a negative electrode shell (11) of the battery mold. The positive electrode shell (3) of the battery mold is provided with an X-ray window one (7), and the negative electrode shell (11) of the battery mold is provided with an X-ray window two (15). The XY displacement stage base (20) is supported on the bottom of the detachable battery mold. The charging and discharging device is electrically connected to the battery electrodes. The mass spectrometer is connected to the embedded gas path (6) through a pipe. The heating wires (14) are integrated inside the negative electrode shell (11) of the battery mold and electrically connected to the heating wire power supply line (10). The separator (21) is set inside the detachable battery mold and located between the positive and negative electrodes of the battery. It can realize multi-modal synchronous measurement of large-area XRD scanning imaging and real-time gas analysis without damaging the battery packaging structure.

2. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: A positive electrode tab (1) is fixedly provided on the top left side of the positive electrode shell (3) of the battery mold. A gas inlet hole (2) is provided on the top of the positive electrode shell (3). A gas outlet hole (8) is provided on the bottom of the positive electrode shell (3). An embedded gas passage (6) is provided inside the positive electrode shell (3). The two ends of the embedded gas passage (6) are respectively connected to the gas inlet hole (2) and the gas outlet hole (8). A screw hole (4) is provided on the edge of the positive electrode shell (3). A sealing ring (5) is provided around the edge of the positive electrode shell (3). An X-ray window (7) is provided at a specific position of the positive electrode shell (3).

3. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: A negative electrode tab (9) is fixedly provided on the top left side of the negative electrode shell (11) of the battery mold. A screw hole (12) is provided on the edge of the negative electrode shell (11). A sealing ring (13) is provided around the edge of the negative electrode shell (11). An X-ray window (15) is provided at a specific position of the negative electrode shell (11). The heating wire (14) is arranged in a specific distribution shape inside the negative electrode shell (11) of the battery mold. One end of the heating wire power supply line (10) is electrically connected to the heating wire (14), and the other end extends to the outside of the negative electrode shell (11) of the battery mold.

4. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: The XY displacement stage base (20) is equipped with a Y-axis guide rail base plate (16), the Y-axis guide rail base plate (16) is equipped with a Y-axis guide rail (17), the Y-axis guide rail base plate (18) is slidably connected to the Y-axis guide rail (17), the X-axis guide rail base plate (18) is equipped with an X-axis guide rail (19), and the detachable battery mold is fixedly supported on the X-axis guide rail (19).

5. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: Both X-ray window one (7) and X-ray window two (15) are composed of multiple windows spliced ​​together, and the splicing points are provided with PEEK or PTFE support structures.

6. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: The embedded gas path (6) together with the gas inlet hole (2) and gas outlet hole (8) opened on the positive electrode shell (3) of the battery mold constitute a gas flow channel. The gas outlet hole (8) is connected to the mass spectrometer (OEMS / GCMS) through a pipe. The heating wire (14) can achieve a temperature control environment from room temperature to 85°C.

7. The X-ray diffraction imaging and real-time gas analysis device according to claim 1, characterized in that: The XY displacement stage base (20) is used in conjunction with the Y-axis guide rail base plate (16), Y-axis guide rail (17), X-axis guide rail base plate (18) and X-axis guide rail (19) to form a displacement mechanism with a movement range of centimeters and a positioning accuracy of micrometers. The materials of the X-ray window one (7) and X-ray window two (15) are beryllium, mica, Kapton film, aluminum foil, silicon nitride, sapphire or diamond. The sapphire or diamond window is coated with an Al or Au conductive layer.

8. An X-ray diffraction imaging and real-time gas analysis method, applied to the X-ray diffraction imaging and real-time gas analysis apparatus according to any one of claims 1-7, characterized in that: Includes the following steps: S1. Place the soft-pack battery between the positive electrode shell (3) and the negative electrode shell (11) of the battery mold, so that the separator (21) is located between the positive and negative electrodes of the battery. Use screw holes 1 (4) and 2 (12) to fasten and fix the positive electrode shell (3) and the negative electrode shell (11) of the battery mold, and use sealing rings (5) and (13) to achieve sealing. S2. Connect the gas source to the gas inlet (2) through a pipe, and connect the mass spectrometer to the gas outlet (8) through a pipe to complete the connection; S3. Connect the charging and discharging device to the positive electrode tab (1) and the negative electrode tab (9), and connect the heating wire power supply line (10) to the power supply circuit; S4. Start the charging and discharging equipment, charge and discharge the soft-pack battery according to the set parameters, and adjust the internal temperature of the battery mold by heating wires according to the test requirements; S5. Start the displacement mechanism corresponding to the XY displacement stage base. Through the coordinated movement of the Y-axis guide rail and the X-axis guide rail, drive the detachable battery mold to move along the X-axis and Y-axis directions to achieve large-area scanning of the X-ray focus at X-ray window one and X-ray window two. Collect two-dimensional XRD patterns at each coordinate point to obtain the XY position coordinates and XRD patterns corresponding to the test time (t). S6. The gas discharged through the embedded gas path during the battery charging and discharging process is collected in real time by mass spectrometer. The gas composition is analyzed based on m / Z fragment information to obtain the gas composition corresponding to the test time (t). S7. Based on the test time and the position of the XY displacement stage, define the XY coordinate sequence, extract the diffraction peak information in the XRD pattern, draw a two-dimensional diffraction imaging (mapping) image, and synchronously associate the phase distribution image with the gas component data at the corresponding coordinate points to complete the collaborative analysis of battery structure evolution, phase distribution, gas generation behavior and spatial distribution of each gas component / concentration.

Images