Electrical device sample holder for photoelectron spectrometer detection

Abstract

The utility model relates to an electrical device sample holder for detection of a photoelectron spectrometer, which comprises a base used for being mounted on a sample holder of the photoelectron spectrometer; the sample groove is formed in the base, the sample groove comprises a sample groove bottom plate and a plurality of sample groove side plates arranged on the sample groove bottom plate in a surrounding mode, the sample groove is provided with a sample inlet facing the side face and an upward pressure applying opening, and the battery collector is adjustably connected to the upper portion of the base through a pressing screw. The sample groove is arranged below the sample groove bottom plate; the temperature sensor is arranged on the peripheral side of the sample groove and is used for detecting the environment temperature of the sample groove; and the heater is fixed on the base and is used for heating the sample groove. A sample groove is arranged in a sample support, and a battery collector, a force sensor, a temperature sensor and a heater are implanted, so that an electrical device can be subjected to in-situ real-time test under the conditions of electrification, temperature change and pressurization.

Description

Technical Field

[0001] The utility model relates to the technical field of photoelectron energy spectrum detection, in particular to an electrical device sample holder used for photoelectron energy spectrometer detection. Background Art

[0002] Electrical devices such as diodes, capacitors, lithium-ion batteries, and solar cells have been widely used in our daily lives for nearly a hundred years and have developed rapidly with each passing day. However, these electrical devices still face the problem of unclear failure and performance improvement mechanisms during use or at extreme temperatures, which hinders their iteration and the sustainable development of society. Developing analytical methods that can characterize these devices in situ is the key to improving the understanding of device failure and performance improvement. Among the many surface analysis methods, X-ray photoelectron spectroscopy can provide information on the chemical composition, chemical state, and electronic structure of the material surface (depth less than 10nm), and is a powerful technology for studying the chemical state and electronic structure changes of material interfaces. The photoelectron spectrometer consists of an ultra-high vacuum system, an excitation light source, an electronic signal contact board, a detector, a data acquisition and processing system, and other accessories. The working process is as follows: (1) Place the sample to be tested on the sample holder and transfer it to the analysis chamber of the instrument by means of vacuum extraction or other means; (2) The narrow-band X-rays or ultraviolet light emitted by the excitation light source acts on the sample surface to excite electrons of different energy levels in the atoms on the sample surface, thereby generating characteristic signals such as photoelectrons and Auger electrons; (3) The electronic signal contact board, detector and data acquisition and processing system detect, collect and count the photoelectrons generated in step 2, and finally obtain the relationship curve between signal intensity and energy, that is, the photoelectron energy spectrum.

[0003] However, traditional photoelectron spectroscopy characterization methods usually separate the analysis object from its original system environment and move it into a photoelectron spectrometer for characterization. Usually, this requires disassembling the electrical device and placing its core components such as materials and electrodes on ordinary sample holders for offline testing. However, due to the difference between the working state of the offline environment and the electrical device in the actual electric field environment, this test method cannot accurately show the chemical and electronic structure changes of the core components of the device. At the same time, many devices often need to be measured at different temperatures and different external stacking pressures. Conventional sample holders can only collect signals at room temperature, and heatable sample holders are difficult to implement in-situ power-on experiments.

[0004] Therefore, it is urgent to develop a sample holder that can be powered, heated and pressurized and its use method to achieve in-situ photoelectron spectroscopy online real-time testing of electrical devices (such as solid-state lithium-ion batteries, solar cells, diodes, capacitors, etc.) at different temperatures and different external stacking pressures. Such research can explore the chemical and electronic structure changes of the core components of electrical devices (such as active layers, modified layers, electrodes, and device interfaces) during actual working processes. Utility Model Content

[0005] In order to solve the problem that the existing sample holder cannot study the performance of electrical devices online and at different temperatures / pressures, the utility model provides an electrical device sample holder for photoelectron spectrometer detection.

[0006] To achieve the above object, the inventor provides an electrical device sample holder for photoelectron spectrometer detection, comprising:

[0007] A base, which is used to be mounted on a sample holder of a photoelectron spectrometer;

[0008] A sample tank is arranged on the base, the sample tank comprises a sample tank bottom plate and a plurality of sample tank side plates arranged around the sample tank bottom plate, the sample tank is provided with a sample insertion port facing the side and a pressure port facing upward,

[0009] A battery collector, which is adjustably connected to the top of the base through a clamping screw and is used to apply pressure to the sample in the sample tank;

[0010] A force sensor is disposed below the bottom plate of the sample tank and is used to detect the pressure on the sample tank;

[0011] A temperature sensor is arranged on the periphery of the sample tank and is used to detect the ambient temperature of the sample tank;

[0012] The heater is fixed on the base and is used for heating the sample slot.

[0013] Furthermore, an analysis hole is provided on the battery collector, and the analysis hole corresponds to the position of the sample slot.

[0014] Furthermore, an insulating sheet is provided on the surface of the sample tank side plate facing the inner side of the sample tank.

[0015] Furthermore, the temperature sensor is arranged below the insulating sheet, and a sensing probe of the temperature sensor faces a side of the sample slot.

[0016] Furthermore, a sample slot placement groove is provided on the upper surface of the base, the sample slot and the force sensor are both arranged in the sample slot placement groove, and the battery collector cover is arranged at the notch of the sample slot placement groove.

[0017] Furthermore, the sample holder also includes a conductive contact assembly, which includes a plurality of conductive interfaces and signal springs that are electrically connected correspondingly, and each of the signal springs is correspondingly connected to the force sensor, the temperature sensor and the heater through a wire.

[0018] Furthermore, an electrode adapter sheet is provided at the bottom of the sample slot, the electrode adapter sheet is in contact with the bottom of the sample slot bottom plate, and the electrode connecting sheet is connected to the corresponding signal spring sheet through a wire.

[0019] Furthermore, the signal shrapnel is made of beryllium copper alloy.

[0020] Furthermore, a positioning hole and two electrode introduction holes are arranged on the side surface of the base, and the positioning hole and the two electrode introduction holes are arranged on two sides of the base opposite to each other.

[0021] Furthermore, the sample tank is made of beryllium copper alloy.

[0022] Different from the prior art, the above technical solution has the following advantages: by placing a sample slot in the sample holder and implanting a battery collector, a force sensor, a temperature sensor and a heater, the electrical device can be tested in situ in real time under the conditions of power supply, variable temperature and pressure. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a schematic structural diagram of a sample holder for an electrical device used for photoelectron spectrometer detection according to the utility model;

[0024] Figure 2 This is a schematic diagram of the exploded structure of a sample holder of an electrical device used for photoelectron spectrometer detection in the utility model;

[0025] Figure 3 This is a schematic diagram of the structure of a sample slot of a sample holder for an electrical device used for photoelectron spectrometer detection according to the utility model;

[0026] Figure 4 This is a schematic diagram of the structure of an electrical device sample holder for photoelectron spectrometer detection in the utility model. Figure 2 ;

[0027] Figure 5 This is a schematic structural diagram of a conductive contact assembly of a sample holder of an electrical device used for photoelectron spectrometer detection according to the utility model;

[0028] Figure 6 The utility model is a schematic diagram of the connection of wires in an analysis chamber of a sample holder of an electrical device used for detection by a photoelectron spectrometer.

[0029] Figure markings: 1. base, 11. positioning socket, 12-13. electrode introduction socket, 21. sample slot, 211. insulating ceramic sheet, 22. electrode transfer wire, 23. battery collector, 231. analysis hole, 24. force sensor, 25. temperature sensor, 26. heater, 3. conductive contact assembly, 31-37. signal spring, 38. main body mounting plate, 39. ceramic gasket, 310. mica gasket, 4. sample rack of photoelectron spectrometer, 41, 42. signal pins on the sample rack of photoelectron spectrometer, 5. signal contact plate, 51-57. signal contact, 6. analysis chamber, 7. original electrode of the sample rack of photoelectron spectrometer, 8. external temperature controller. DETAILED DESCRIPTION

[0030] In order to explain in detail the possible application scenarios, technical principles, specific schemes that can be implemented, and the purposes and effects that can be achieved, the following is a detailed description of the specific embodiments listed in conjunction with the accompanying drawings. The embodiments described herein are only used to more clearly illustrate the technical solutions of the present application, and are therefore only used as examples, and cannot be used to limit the scope of protection of the present application.

[0031] Reference to "embodiment" herein means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The term "embodiment" appearing in various places in the specification does not necessarily refer to the same embodiment, nor does it particularly limit its independence or association with other embodiments. In principle, in the present application, as long as there is no technical contradiction or conflict, the various technical features mentioned in the embodiments can be combined in any way to form a corresponding implementable technical solution.

[0032] Unless otherwise defined, the technical terms used in this document have the same meanings as those generally understood by those skilled in the art to which this application belongs; the use of relevant terms in this document is only for describing specific embodiments and is not intended to limit this application.

[0033] In the description of this application, the term "and / or" is an expression used to describe the logical relationship between objects, indicating that three relationships may exist, for example, A and / or B, which means: A exists, B exists, and A and B exist at the same time. In addition, the character " / " in this article generally indicates that the objects before and after are in an "or" logical relationship.

[0034] In the present application, terms such as “first” and “second” are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship of quantity, priority or sequence between these entities or operations.

[0035] Without further limitations, in this application, the words "include", "comprises", "has" or other similar expressions used in the sentences are intended to cover non-exclusive inclusion. These expressions do not exclude the presence of additional elements in the process, method or product including the elements, so that the process, method or product including a series of elements may include not only those limited elements, but also other elements not explicitly listed, or also include elements inherent to such process, method or product.

[0036] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than", "less than", "exceed" and the like are understood to exclude the number itself; expressions such as "above", "below", "within" and the like are understood to include the number itself. In addition, in the description of the embodiments of this application, "multiple" means more than two (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups", "multiple times", etc., unless otherwise clearly and specifically limited.

[0037] In the description of the embodiments of the present application, space-related expressions used, such as "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "vertical", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicate the orientation or position relationship based on the orientation or position relationship shown in the specific embodiments or drawings, and are only for the convenience of describing the specific embodiments of the present application or facilitating the reader's understanding, and do not indicate or imply that the referred device or component must have a specific position, a specific orientation, or be constructed or operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present application.

[0038] Unless otherwise expressly specified or limited, in the description of the embodiments of the present application, the terms such as "install", "connect", "connect", "fix", "set", etc. used should be understood in a broad sense. For example, the "connection" can be a fixed connection, a detachable connection, or an integrated setting; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium; it can be the internal connection of two elements or the interaction relationship between two elements. For technicians in the technical field to which the present application belongs, the specific meanings of the above terms in the embodiments of the present application can be understood according to the specific circumstances.

[0039] See also Figures 1 to 6 In this embodiment, an electrical device sample holder for photoelectron spectrometer detection includes:

[0040] A base, which is used to be mounted on a sample holder of a photoelectron spectrometer;

[0041] A sample tank is arranged on the base, the sample tank comprises a sample tank bottom plate and a plurality of sample tank side plates arranged around the sample tank bottom plate, the sample tank is provided with a sample insertion port facing the side and a pressure port facing upward,

[0042] A battery collector, which is adjustably connected to the top of the base through a clamping screw and is used to apply pressure to the sample in the sample tank;

[0043] A force sensor is disposed below the bottom plate of the sample tank and is used to detect the pressure on the sample tank;

[0044] A temperature sensor is arranged on the periphery of the sample tank and is used to detect the ambient temperature of the sample tank;

[0045] The heater is fixed on the base and is used for heating the sample slot.

[0046] The clamping screw specifically uses a stainless steel clamping screw.

[0047] The electrical device sample holder for photoelectron spectrometer detection is equipped with a sample slot, and a battery collector, a force sensor, a temperature sensor and a heater are implanted in the sample holder, so that the electrical device can be tested in situ in real time under the conditions of power on, temperature change and pressure application.

[0048] In some embodiments, an analysis hole is provided on the battery collector, and the analysis hole corresponds to the position of the sample slot. The function of the analysis hole is to conduct photoelectron spectroscopy testing from the analysis hole when the sample holder is placed horizontally. By using the rotation function of the sample holder of the photoelectron spectrometer, the information on the side of the electrical device can be analyzed by rotating the sample holder 90 degrees.

[0049] In some embodiments, the surface of the sample slot side plate facing the inner side of the sample slot is provided with an insulating sheet. The insulating sheet is preferably an insulating ceramic sheet. Preferably, both sides of the sample slot side are pasted with 0.2 mm thick insulating ceramic sheets to prevent short circuit between the upper and lower sample sheets.

[0050] In some embodiments, the temperature sensor is disposed below the insulating sheet, and a sensing probe of the temperature sensor faces a side of the sample slot.

[0051] In some embodiments, a sample slot placement groove is provided on the upper surface of the base, the sample slot and the force sensor are both provided in the sample slot placement groove, and the battery collector cover is provided at the notch of the sample slot placement groove. The sample slot placement groove can improve the compactness of the structure of the base and reduce the occupied space of the structure.

[0052] In some embodiments, the sample holder further includes a conductive contact assembly, which includes a plurality of conductive interfaces and signal springs that are electrically connected correspondingly, and each of the signal springs is correspondingly connected to the force sensor, the temperature sensor, and the heater via a wire.

[0053] In some embodiments, an electrode adapter sheet is further provided at the bottom of the sample slot, the electrode adapter sheet is in contact with the bottom of the sample slot bottom plate, and the electrode connecting sheet is connected to the corresponding signal spring sheet through a wire.

[0054] In some embodiments, the signal shrapnel is made of beryllium copper alloy.

[0055] In some embodiments, a positioning hole and two electrode introduction holes are provided on the side surface of the base, and the positioning hole and the two electrode introduction holes are arranged on two sides of the base opposite to each other.

[0056] In some embodiments, the sample tank is made of beryllium copper alloy.

[0057] The following is a detailed description of the above embodiment:

[0058] In order to explain the utility model more clearly, a photoelectron spectrometer and an analysis chamber are used for explanation. The photoelectron spectrometer includes an excitation light source, an electronic signal contact plate 5, a sample rack 4, a vacuum system and an analysis chamber 6. A vacuum system must be adopted in the photoelectron spectrometer, mainly for two reasons: First, photoelectron spectroscopy is a surface analysis technology. If the vacuum degree of the analysis chamber is very poor, the clean surface of the sample may be covered by residual gas molecules in the vacuum in a very short time, and the real information of the sample cannot be obtained. Second, because the signal and energy of the photoelectron are very weak, if the vacuum degree is poor, the photoelectrons can easily collide with the residual gas molecules in the analysis chamber and lose energy, and finally cannot reach the detector. In the X-ray photoelectron spectrometer, in order to make the vacuum degree of the analysis chamber reach 10-8Pa, a minimum two-stage vacuum pump system is generally used.

[0059] The utility model discloses an electrical device sample holder for photoelectron spectrometer detection, which is a vertical structure as a whole. The electrical devices that can be studied include solid-state lithium-ion batteries, solar cells, diodes, capacitors, etc. The sample holder includes:

[0060] Base 1, the base 1 is installed on the photoelectron spectrometer, specifically connected to the sample rack 4 of the photoelectron spectrometer, the base 1 is a beryllium copper alloy base, beryllium copper alloy has high conductivity, non-magnetic and good corrosion resistance. The base 1 contains a positioning hole 11, an electrode introduction hole 12 and an electrode introduction hole 13. The positioning hole 11 is located on the side of the base 1, and the electrode introduction hole 12 and the electrode introduction hole 13 are located on the side of the base 1 opposite to the positioning hole 11. A manipulator with a positioning pin can be used to grab the sample tray through the positioning hole 11 and place it on the sample rack 4 of the photoelectron spectrometer. The sample rack 4 of the photoelectron spectrometer has a signal pin 41 and a signal pin 42, the signal pin 41 is connected to the electrode introduction hole 12, and the signal pin 42 is connected to the electrode introduction hole 13.

[0061] The sample slot 21 is arranged on the base 1. The sample slot 21 is a movable slot structure, and the samples are placed horizontally in layers in the slot. The sample slot 21 is a beryllium copper alloy sample slot. The top of the sample slot 21 is in contact with the battery collector 23 through a stainless steel clamping screw. The battery collector 23 is connected to the base 1 through a stainless steel clamping screw, and outputs an electrical signal at one end through a 41 signal pin that contacts the base 1 through the sample rack 4 of the photoelectron spectrometer. The battery collector 23 is a stainless steel battery collector. The 41 signal pin is grounded together with the base 1 during the photoelectron spectrum test. There is an analysis hole 231 on the battery collector 23.

[0062] The bottom of the sample slot 21 is in direct contact with the electrode transfer wire 22 to achieve electrical conduction, and is connected to the signal pin 42 of the sample rack 4 of the photoelectron spectrometer through the signal shrapnel 34 made of beryllium copper alloy on the conductive contact assembly 3. The signal pin 41 and the signal pin 42 are connected to the analysis chamber 6 via the D- and A+ sockets of the CF16 electrode conversion port outside the vacuum. The D- socket is also directly connected to the ground. The analysis chamber can control the current and voltage values ​​of the conductive electrical device, that is, to charge and discharge the electrical device at different current densities, and realize the online operation and performance test of the electrical device. The performance test includes electrical performance and battery tests such as cyclic voltammetry test, constant current test, constant potential test, AC impedance test, volt-ampere characteristic measurement, stability test, etc. At the same time, the photoelectron energy spectrum data is collected during the above test process, thereby realizing the in-situ photoelectron energy spectrum real-time test of the electrical device.

[0063] The force sensor 24 is attached to the bottom of the sample slot 21, and is connected to the signal springs 32 and 33 made of beryllium copper alloy on the conductive contact assembly 3 through a wire, and stress measurement is achieved through an external stress sensor display device. The sample is compressed by tightening the M2 316 stainless steel compression screw on the battery collector 23 to achieve the fit and pressure of the battery collector and the upper electrode of the sample. The force sensor 24 collects pressure, which needs to be converted according to the contact area. The contact area is 61mm 2 , the maximum pressure can reach 120 N. The stress data stored in the force sensor 24 can be displayed and read through an external stress sensor display device and signal springs 32 and 33 .

[0064] The temperature sensor 25 is pressed under the side of the sample slot 21 by the insulating ceramic sheet 211, and is connected to the signal springs 31 and 37 made of beryllium copper alloy on the conductive contact assembly 3 through wires. The signal springs 31 and 37 are connected to the external temperature controller 8 through the 15+ and 16- sockets in the original electrodes 7 of the sample holder of the photoelectron spectrometer to achieve temperature measurement.

[0065] Heater 26, the heater 26 is placed in the hole between the base 1 and the conductive contact assembly 3. The heater 26 has a diameter of 3 mm and a length of 13 mm, and the operating voltage and power are 12 V and 12 W respectively. The heater 26 is connected to the signal shrapnel 35 and 36 made of beryllium copper alloy on the conductive contact assembly 3. The signal shrapnel 35 and 36 are connected to the external temperature controller 8 through the 17+ in the original electrode 7 of the sample holder of the photoelectron spectrometer and the D- socket of the CF16 electrode conversion port outside the vacuum to realize heating control.

[0066] Conductive contact assembly 3, the conductive contact assembly 3 is an assembly board for each conductive interface. Its main mounting plate 38 is made of beryllium copper alloy. Signal shrapnel 32 and 33, 34, 35 and 36, and 31 and 37 made of beryllium copper alloy are used to connect force sensor 24, electrode transfer wire 22, heater 26 and temperature sensor 25 respectively. The signal shrapnel is anchored with M1.6 316 stainless steel screws, and ceramic gaskets 39 and mica gaskets 310 are used to separate the electrical conduction between the signal shrapnel and the main mounting plate 38.

[0067] In addition, in order to reduce the length of the wire, a signal contact plate 5 is installed between the sample slot 21 and the conductive contact assembly 3. The signal contact plate 5 is provided with signal contacts 52, 53, 54, 55, 56, 51, 57 respectively connected to the signal springs 32 and 33, 34, 35 and 36, and 31 and 37. The signal contacts are anchored with M1.6 316 stainless steel screws, and ceramic washers are used to separate the electrical conduction between the signal contacts and the signal contact plate 5.

[0068] The utility model also discloses a method for using a sample holder of an electrical device for photoelectron spectrometer detection, comprising:

[0069] S1, placing the electrical device in the sample slot 21 of the electrical device sample holder for photoelectron spectrometer detection;

[0070] S2, connecting the stress sensor display device to the signal springs 32 and 33 to display the compressive stress;

[0071] S3, turning the stainless steel clamping screw on the battery collector 23 to clamp the electrical device. The degree to which the electrical device is clamped is ultimately determined by the required compressive stress value;

[0072] S4, placing the sample holder with the electrical device in step S3 in the analysis chamber 6 of the photoelectron spectrometer, connecting one end of the electrode contact of the sample holder 4 in the analysis chamber 6 to the electrode introduction jacks 12 and 13, and connecting the other end of the sample holder 4 in the analysis chamber 6 to the analysis chamber;

[0073] S5. Turn on the thermostat and set the temperature to the temperature required for the electrical device test, and wait for the temperature to rise to the set temperature and keep it warm for 20 minutes;

[0074] S6, by rotating the sample holder and measuring the photoelectron spectrum at the position to be measured through the analysis hole 231 to determine the best observation point;

[0075] S7. After setting the parameters on the analysis chamber, the photoelectron spectrum test can be performed.

[0076] Furthermore, the analysis chamber includes any one of an electrochemical workstation and an electrical performance tester.

[0077] At the same time, the base 1 of the sample holder is connected to the zero potential of the photoelectron spectrometer, and the test position must be in close contact with the base of the sample holder to ensure that the test position is near the zero potential, which can avoid causing the drift of the measured spectrum peak; the battery collector 23 is connected to the sample holder base 1, which can realize the non-polarity of the sample holder and can adjust the positive and negative poles of the electrical device as needed.

[0078] The definition of zero potential is generally as follows: a point A is selected in the circuit as a potential reference, and the potential is set to zero. The instrument has an independent ground wire and has good electrical contact with the earth. The zero potential of the instrument corresponds to the earth potential, and the earth potential is defined as zero potential.

[0079] In addition, the slotted structure design and rotatable operation of the sample holder facilitate in-situ research on the core components and interfaces of electrical devices.

[0080] The core components of electrical devices are electrolytes, electrodes, and the interface between electrolytes and electrodes.

[0081] Since the sample holder is a slot structure, a single electrode surface can be observed through the analysis hole 231 in the non-rotated state; after the sample holder is rotated 90 degrees, five positions such as the positive electrode, positive electrode / electrolyte interface, electrolyte, electrolyte / negative electrode interface, and negative electrode can be measured simultaneously.

[0082] Therefore, by changing the different positions of the electrical device in the detection area according to the research content, the chemical and electronic structure changes of the core components, modification layers, electrodes and device interfaces of the electrical device under different electric field conditions can be studied.

[0083] When performing electrochemical testing on solid-state lithium-ion batteries and collecting photoelectron spectra online in real time, the specific steps are as follows:

[0084] S1. Assemble a solid-state lithium-ion battery in a glove box connected to a photoelectron spectrometer, then place the solid-state lithium-ion battery between a battery collector 23 and a sample slot 21 to form a sandwich structure, and finally obtain a sample holder containing a solid-state lithium-ion battery under a predetermined pressure by locking the stainless steel clamping screws on the battery collector 23 and displaying the compressive stress of an external stress sensor display device;

[0085] S2, placing the sample holder in the analysis chamber 6 of the photoelectron spectrometer via a conveying device, the conveying device may be a manipulator with a pin, and the glove box is also a component of the photoelectron spectrometer. This can prevent the sample holder from being exposed to air during the transfer process, thereby affecting the performance of the solid-state lithium-ion battery;

[0086] S3, connecting the sample holder 4 of the photoelectron spectrometer to an external electrochemical workstation through the electrode contacts; connecting the temperature sensor 25 and the heater 26 to the external temperature controller 8 through the electrode leads in the built-in photoelectron spectrometer analysis chamber;

[0087] S3, heating the sample holder to the required temperature through the regulation of the external temperature controller 8; at the same time, through the program control of the electrochemical workstation, realizing electrochemical and battery tests such as charge and discharge at different rates, cyclic voltammetry test, constant current test, constant potential test, and AC impedance test of the solid-state lithium-ion battery;

[0088] S4. While the solid-state lithium-ion battery is undergoing the above-mentioned electrochemical and battery tests, the sample holder is rotated and the photoelectron spectrum measurement is performed on the position to be measured through the analysis hole 231 to determine the best observation point, so that the positive electrode, negative electrode, electrolyte, positive electrode / electrolyte interface, and negative electrode / electrolyte interface of the solid-state lithium-ion battery are irradiated with X-rays / ultraviolet light, and the excited photoelectrons are collected by the electronic signal contact plate to obtain a photoelectron spectrum diagram.

[0089] In addition, the materials used in the in-situ electric field sample holder of the photoelectron spectrometer for electrical devices of the utility model are all materials that can work under ultra-high vacuum and are non-magnetic materials, ensuring that the sample holder will not affect the normal operation of the instrument due to outgassing, magnetic conductivity, etc. The installation position of the electrical device is consistent with the elliptical direction of the X-ray / ultraviolet light source, and is located in the direction with the highest test efficiency, which is conducive to testing low-content elements.

[0090] Finally, it should be noted that although the above embodiments have been described in the specification and drawings of this application, this does not limit the scope of patent protection of this application. All technical solutions generated by replacing or modifying equivalent structures or equivalent processes based on the essential concept of this application using the contents recorded in the specification and drawings of this application, as well as directly or indirectly implementing the technical solutions of the above embodiments in other related technical fields, are included in the scope of patent protection of this application.

Claims

1. An electrical device sample holder for photoelectron spectrometer detection, characterized in that: include: A base, which is used to be mounted on a sample holder of a photoelectron spectrometer; A sample tank is arranged on the base, the sample tank comprises a sample tank bottom plate and a plurality of sample tank side plates arranged around the sample tank bottom plate, the sample tank is provided with a sample insertion port facing the side and a pressure port facing upward, A battery collector, which is adjustably connected to the top of the base through a clamping screw and is used to apply pressure to the sample in the sample tank; A force sensor is disposed below the bottom plate of the sample tank and is used to detect the pressure on the sample tank; A temperature sensor is arranged on the periphery of the sample tank and is used to detect the ambient temperature of the sample tank; The heater is fixed on the base and is used for heating the sample slot.

2. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: An analysis hole is provided on the battery collector, and the analysis hole corresponds to the position of the sample slot.

3. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: An insulating sheet is arranged on the surface of the sample tank side plate facing the inner side of the sample tank.

4. The electrical device sample holder for photoelectron spectrometer detection according to claim 3, characterized in that: The temperature sensor is arranged below the insulating sheet, and the sensing probe of the temperature sensor faces the side of the sample slot.

5. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: The upper surface of the base is provided with a sample slot placement groove, the sample slot and the force sensor are both arranged in the sample slot placement groove, and the battery collector cover is arranged at the notch of the sample slot placement groove.

6. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: The sample holder further comprises a conductive contact assembly, which comprises a plurality of conductive interfaces and signal springs that are electrically connected correspondingly, and each of the signal springs is correspondingly connected to the force sensor, the temperature sensor and the heater via a wire.

7. The electrical device sample holder for photoelectron spectrometer detection according to claim 6, characterized in that: An electrode adapter sheet is also provided at the bottom of the sample slot, and the electrode adapter sheet is in contact with the bottom of the sample slot bottom plate, and the electrode connecting sheet is connected to the corresponding signal spring sheet through a wire.

8. The electrical device sample holder for photoelectron spectrometer detection according to claim 6, characterized in that: The signal shrapnel is made of beryllium copper alloy.

9. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: A positioning socket and two electrode introduction sockets are arranged on the side surface of the base. The positioning socket and the two electrode introduction sockets are arranged on two sides of the base opposite to each other.

10. The electrical device sample holder for photoelectron spectrometer detection according to claim 1, characterized in that: The sample tank is made of beryllium copper alloy.

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