Sample cell for in situ x-ray diffraction and x-ray fluorescence coupled with an assembly method thereof

Abstract

The application discloses a sample cell combined with in-situ X-ray diffraction and X-ray fluorescence and an assembling method thereof, and relates to the technical field of electrochemistry.The sample cell comprises a positive electrode cover, an insulating cavity, a negative electrode cover and an elastic piece, the boss of the insulating cavity is matched with the groove of the positive electrode cover, the boss of the negative electrode cover is matched with the inner cavity of the insulating cavity, the number of parts is small, the assembling process is simple, the structure of the whole sample cell is more compact, and the sealing performance of the insulating cavity is better; the positive electrode cover and the insulating cavity, the negative electrode cover and the insulating cavity and the cushion block and the insulating cavity are all sealed, the excellent sealing performance in the insulating cavity is ensured, and the cycle performance of the battery is improved; in addition, in the assembling process, vacuumizing and adding foamed metal sheets are adopted, the contact compactness of the battery is improved, the internal resistance of the battery is reduced, the performance of the battery is optimized, and the test data is more real and effective.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of electrochemistry, and particularly relates to a sample cell for in-situ X-ray diffraction and X-ray fluorescence combined use and an assembling method thereof. BACKGROUND

[0002] With the continuous upgrading of people's requirements for new energy storage systems in terms of high power and high energy density, it has become a major challenge for researchers to find and develop energy storage materials with more excellent performance. Therefore, it is urgent to study the structure and performance evolution mechanism of energy storage materials during the charging and discharging process, explore the structure-performance relationship of composition-structure-performance, and use it to guide the synthesis of energy storage materials with more excellent performance, so as to optimize the current energy material supply structure. In-situ X-ray diffraction technology and X-ray fluorescence analysis technology can monitor the structure and composition changes of energy storage electrode materials in the charging and discharging process in real time, qualitatively analyze the crystal type, crystal parameter, crystal defect, and content of different structure phases of the material, so as to infer the intermediate generated in the electrochemical reaction process. Such in-situ detection technology provides a strong guarantee for accurately revealing the battery reaction mechanism and further optimizing the design and synthesis of electrode materials.

[0003] The design of the in-situ sample cell and its assembling method are important parts of the in-situ detection technology. In recent years, there have been some in-situ sample cells designed independently in China. For example, a patent document with the name of an in-situ test sample platform and the authorization announcement number of CN104458780B discloses a high-temperature in-situ test sample platform. The platform has many parts and is complex to assemble. A patent document with the name of an in-situ sample cell for in-situ test of lithium battery and the authorization announcement number of CN208688993U discloses an in-situ sample cell. Although the upper cover and the inner ring upper surface are sealed by a sealing ring, the sealing effect of the upper cover is not good in actual application. A patent application document with the name of an X-ray diffraction in-situ battery device and its assembling method and the application publication number of CN107910582A discloses an in-situ battery device and its assembling method. The assembling process is complex. As can be seen, most of the in-situ sample cells designed independently in China have the shortcomings of many parts, complex assembly, poor sealing (loose contact), etc. The assembled battery cannot be normally charged and discharged. Although the in-situ sample cells abroad have stable performance, they have poor structure design flexibility and cannot be directly matched with the detection equipment for X-ray diffraction and X-ray fluorescence analysis combined use. Moreover, they are expensive. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides an in-situ X-ray diffraction and X-ray fluorescence combined use sample cell and an assembling method thereof, so as to solve the problems of many parts and complex assembly of the existing sample cell.

[0005] The application solves the above technical problems by the following technical scheme: a sample cell for in-situ X-ray diffraction and X-ray fluorescence, comprising:

[0006] The positive cover is provided with a groove on the lower surface.

[0007] The insulating cavity is in T shape, the boss of the insulating cavity is inserted into the groove of the positive cover, and the upper surface of the platform of the insulating cavity is in contact with and connected to the lower surface of the positive cover; an electrode sheet, a diaphragm, a counter electrode and a pad are sequentially arranged in the inner cavity of the insulating cavity from top to bottom.

[0008] The negative cover is in T shape, the boss of the negative cover is inserted into the inner cavity of the insulating cavity, and the upper surface of the platform of the negative cover is in contact with and connected to the lower surface of the platform of the insulating cavity.

[0009] The elastic member is arranged on the boss of the negative cover at one end and is inserted into the inner cavity of the insulating cavity and presses the pad at the other end.

[0010] The sample cell comprises the positive cover, the insulating cavity, the negative cover and the elastic member, has fewer components, is easier to assemble, and the boss of the insulating cavity cooperates with the groove of the positive cover, and the boss of the negative cover cooperates with the inner cavity of the insulating cavity, so that the structure of the whole sample cell is more compact, and the sealing performance of the insulating cavity is better.

[0011] Further, the upper surface of the positive cover corresponding to the inner cavity of the insulating cavity is provided with a measurement window in inverted conical shape, the measurement window is in communication with the groove of the positive cover, and a window material is arranged at the communication position of the measurement window and the groove.

[0012] The measurement window in inverted conical shape serves as an incident window of X-ray, and facilitates the XRD diffraction measurement of X-ray through the window material.

[0013] Further, the upper surface of the boss of the insulating cavity is provided with a first sealing groove, and a positive sealing ring is arranged in the first sealing groove, so that the sealing performance between the insulating cavity and the positive cover is better on the basis of the cooperation of the boss of the insulating cavity and the groove of the positive cover.

[0014] Further, the top surface of the groove of the positive cover is provided with a first annular boss matched with the first sealing groove, the first annular boss is used to press the positive sealing ring, and the sealing performance between the insulating cavity and the positive cover is further improved.

[0015] Further, the lower surface of the platform of the insulating cavity is provided with a second sealing groove, and a negative sealing ring is arranged in the second sealing groove, so that the sealing performance between the insulating cavity and the negative cover is better.

[0016] Further, a second annular boss matched with the second sealing groove is arranged on the upper surface of the negative cover platform, and the second annular boss is used to press the negative sealing ring, thereby further improving the sealing performance between the insulating cavity and the negative cover.

[0017] Further, the cushion block is in a cylindrical shape, a third sealing groove is arranged on the side surface of the cushion block, and a sealing ring is arranged in the third sealing groove, so that the sealing performance between the cushion block and the insulating cavity is improved.

[0018] Further, a foam metal sheet is arranged between the counter electrode and the cushion block, so that the soft connection between the cushion block and the counter electrode is realized, and the internal resistance of the battery is reduced.

[0019] Further, an outer ring is arranged outside the insulating cavity, and the outer ring is made of a magnetized material. The outer ring made of the magnetized material can be directly adsorbed on a sample table of an X-ray diffraction and X-ray fluorescence instrument, so that the sample cell can be quickly assembled and disassembled.

[0020] Correspondingly, an assembling method of an in-situ X-ray diffraction and X-ray fluorescence combined sample cell comprises the following steps.

[0021] S1: the lower surface of the positive cover is upward, and a window material is arranged in the communication between the measuring window and the groove;

[0022] S2: the positive sealing ring is assembled, the boss of the insulating cavity is inserted into the groove of the positive cover with the downward direction, and the insulating cavity is fastened to the lower surface of the positive cover;

[0023] S3: in the glove box, the electrode sheet, the diaphragm, the electrolyte, the counter electrode and the foam metal sheet are sequentially arranged in the inner cavity of the insulating cavity;

[0024] S4: the cushion block is pressed on the foam metal sheet, vacuum is drawn, and the negative sealing ring is assembled;

[0025] S5: the negative cover with the assembled elastic member is arranged on the platform of the insulating cavity, so that the elastic member presses the cushion block, the insulating member is sleeved in the second through hole of the negative cover, and the negative cover is fastened to the lower surface of the platform of the insulating cavity;

[0026] S6: the outer ring is sleeved outside the insulating cavity, and the sample cell is installed on the sample table of the X-ray diffraction and X-ray fluorescence instrument, the positive cover and the negative cover are respectively connected with the positive electrode and the negative electrode of the electrochemical workstation, so that the in-situ test is realized.

[0027] Advantages

[0028] Compared with the prior art, the sample cell for in-situ X-ray diffraction and X-ray fluorescence combined with the application comprises a positive electrode cover, an insulating cavity, a negative electrode cover and an elastic member, the boss of the insulating cavity is matched with the groove of the positive electrode cover, the boss of the negative electrode cover is matched with the inner cavity of the insulating cavity, the number of parts is small, the assembly process is simple, the structure of the whole sample cell is more compact, and the sealing performance of the insulating cavity is better; the sealing design is performed between the positive electrode cover and the insulating cavity, between the negative electrode cover and the insulating cavity and between the cushion block and the insulating cavity, the excellent sealing performance in the insulating cavity is ensured, and the cycle performance of the battery is improved; in addition, in the assembly process, vacuum extraction and the addition of a foamed metal sheet are adopted, the contact tightness of the battery is improved, the internal resistance of the battery is reduced, the performance of the battery is optimized, and the test data is more real and effective.

[0029] The sample cell is suitable for an X-ray diffraction and X-ray fluorescence combined equipment, can simultaneously obtain X-ray diffraction spectrum and fluorescence spectrum information of a material in a charging and discharging process, provides guarantee for exploring the structure-activity relationship among composition-structure-performance of the material, and has a wide application prospect.

[0030] Since the sample cell has few parts and a simple and compact structure, the assembly method of the corresponding sample cell is simple to operate, the internal resistance of the battery is low, and the performance is more excellent. DETAILED DESCRIPTION

[0031] In order to more clearly illustrate the technical scheme of the application, the following will briefly introduce the drawings needed to be used in the embodiment description. Obviously, the drawings in the following description are only one embodiment of the application, and other drawings can be obtained by those skilled in the art without creative labor.

[0032] Figure 1 is the assembly drawing of the sample cell in the embodiment of the application;

[0033] Figure 2 is the top view of the positive electrode cover in the embodiment of the application;

[0034] Figure 3 is the sectional view of the positive electrode cover in the embodiment of the application;

[0035] Figure 4 is the top view of the insulating cavity in the embodiment of the application;

[0036] Figure 5 is the sectional view of the insulating cavity in the embodiment of the application;

[0037] Figure 6 is the structural schematic view of the battery to be tested 3 in the embodiment of the application;

[0038] Figure 7 is the top view of the negative electrode cover in the embodiment of the application;

[0039] Figure 8 is a cross-sectional view of the negative cover in the embodiment of the present application;

[0040] Figure 9 is a structural schematic view of the cushion block in the embodiment of the present application;

[0041] Figure 10 is a schematic view of the appearance of the sample cell in the embodiment of the present application;

[0042] Figure 11 is a charge-discharge cycle curve of the sample cell in the embodiment of the present application;

[0043] Figure 12 is an in-situ XRD spectrum of the sample cell in the embodiment of the present application;

[0044] Wherein, 1-positive cover, 101-groove of the positive cover, 102-measuring window, 103-first annular boss, 104-first threaded hole, 105-second threaded hole, 106-window material, 107-positive tab, 2-insulating cavity, 201-internal cavity, 202-platform of the insulating cavity, 203-boss of the insulating cavity, 204-second sealing groove, 205-first sealing groove, 206-platform hole, 207-first through hole, 208-positive sealing ring, 209-negative sealing ring, 3-battery to be measured, 301-electrode sheet, 302-separator, 303-counter electrode, 304-foamed metal sheet, 4-negative cover, 401-boss of the negative cover, 402-platform of the negative cover, 403-second annular boss, 404-third threaded hole, 405-second through hole, 406-negative tab, 407-mounting screw, 5-cushion block, 501-third sealing groove, 502-cylindrical boss, 6-elastic member, 7-outer ring. DETAILED DESCRIPTION

[0045] The technical solutions in the present application will be described clearly and completely below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0046] As shown in Figure 1 , the sample cell for in-situ X-ray diffraction and X-ray fluorescence provided by the present application comprises a positive cover, an insulating cavity, a negative cover 4 and an elastic member 6.

[0047] As shown in Figure 2 and 3As shown, the material of the positive electrode cover 1 is 304 stainless steel, the diameter is 58 mm, and the height is 6 mm. The upper surface of the positive electrode cover 1 is provided with a measuring window 102 in the shape of an inverted cone for facilitating X-ray incidence. The diameter of the upper surface of the measuring window 102 is 45 mm, the diameter of the lower surface of the measuring window 102 is 18 mm, and the depth of the measuring window 102 is 2 mm. The lower surface of the positive electrode cover 1 is provided with a circular groove 101. The inner diameter of the groove 101 is 34 mm, and the depth of the groove 101 is 4 mm. The measuring window 102 is in communication with the groove 101. The upper surface of the positive electrode cover 1 is provided with a first threaded hole 104 for mounting a positive electrode tab 107. The positive electrode tab 107 is connected to the positive electrode of an electrochemical workstation through a lead wire. The lower surface of the positive electrode cover 1 is provided with eight second threaded holes 105 for fastening connection with the insulating cavity 2 and the negative electrode cover 4. A window material 106 is arranged at the communication position of the measuring window 102 and the groove 101. The window material 106 can also be directly arranged on the top surface of the groove 101. In this embodiment, the window material 106 is a beryllium sheet.

[0048] As shown in Figure 4 and 5 The material of the insulating cavity 2 is polytetrafluoroethylene, which has good mechanical processing performance and insulation performance, and is designed in an integrated manner in the shape of a T. The inner cavity 201 of the insulating cavity 2 is a large through hole arranged at the center of the insulating cavity. The inner diameter of the large through hole is 19.5 mm, and the large through hole is used to assemble an electrode sheet 301, a diaphragm 302, a counter electrode 303, and a foam metal sheet 304 (as shown in Figure 4 In this embodiment, the foam metal sheet 304 is a foam nickel sheet, and the areal density of the foam nickel sheet is 480 g / m 2, thickness 1.7mm, the soft connection between the cushion 5 and the counter electrode 303 is realized by the foamed nickel sheet, and the internal resistance of the battery is reduced. The diameter of the platform 202 of the insulating cavity is 58mm, and the height is 12mm. The lower surface of the insulating cavity platform 202 is provided with a second sealing groove 204, the inner diameter of the second sealing groove 204 is 24.5mm, the outer diameter is 30.5mm, and the depth is 2mm. The negative electrode sealing ring 209 is arranged in the second sealing groove 204, and the negative electrode sealing ring 209 makes the sealing between the insulating cavity 2 and the negative electrode cover 4 better. The platform hole 206 matched with the second threaded hole 105 and the first through hole 207 are arranged on the platform 202 of the insulating cavity, the platform hole 206 and the first through hole 207 are arranged at intervals, and the platform hole 206 and the first through hole 207 are respectively 4. The platform hole 206 is used to tightly connect the positive electrode cover 1 and the insulating cavity 2, and the first through hole 207 matches the second through hole 405, which is used to tightly connect the negative electrode cover 4, the insulating cavity 2 and the positive electrode cover 1. The diameter of the boss 203 of the insulating cavity is 32mm, and the height is 4mm. The upper surface of the insulating cavity boss 203 is provided with a first sealing groove 205, the inner diameter of the first sealing groove 205 is 22mm, the outer diameter is 28mm, and the depth is 2mm. The positive electrode sealing ring 208 is arranged in the first sealing groove 205, and the positive electrode sealing ring 208 makes the sealing between the insulating cavity 2 and the positive electrode cover 1 better. The boss 203 of the insulating cavity is arranged in the groove 101 of the positive electrode cover, so that the structure is more compact, and the sealing is better.

[0049] As shown in Figure 7 and 8 , the material of the negative electrode cover 4 is 304 stainless steel, and the negative electrode cover 4 is designed in one piece and in T shape. The diameter of the platform 402 of the negative electrode cover is 55mm, and the height is 4mm. The third threaded hole 404 for mounting the negative electrode tab 406 is arranged on the lower surface of the platform 402 of the negative electrode cover. The second through hole 405 is arranged around the negative electrode cover 4, and the second through hole 405 is 4, which is used to pass through the first through hole 207 of the insulating cavity and the second threaded hole 105 of the positive electrode cover to be tightly connected. The second through hole 405 is provided with an insulating pad to separate the positive electrode and the negative electrode. The boss 401 of the negative electrode cover is in the shape of a cylinder, the diameter of the negative electrode cover boss 401 is 16.5mm, and the height is 5mm, which is used to mount the elastic member 6. One end of the elastic member 6 is mounted on the negative electrode cover boss 401, and the other end presses the cushion 5. The height of the elastic member 6 in the free state is 12mm. In this embodiment, the elastic member 6 is a spring.

[0050] To further improve sealing, a first annular boss 103 is provided on the top surface of the positive electrode cover groove 101 to cooperate with the first sealing groove 205. The first annular boss 103 is used to press the positive electrode sealing ring 208. The inner diameter of the first annular boss 103 is 23mm, the outer diameter is 26mm, and the height is 0.2mm. A second annular boss 403 is provided on the upper surface of the negative electrode cover platform 402 to cooperate with the second sealing groove 204. The second annular boss 403 is used to press the negative electrode sealing ring 209. The inner diameter of the second annular boss 403 is 26mm, the outer diameter is 29mm, and the height is 0.2mm.

[0051] like Figure 9 As shown, the pad 5 is made of 304 stainless steel, cylindrical in shape, with a diameter of 19mm and a height of 5mm. A third sealing groove 501 is provided on the side of the pad 5, and a sealing ring is installed within the third sealing groove 501. The sealing ring seals the pad 5 with the insulating cavity 2, further improving the sealing performance of the insulating cavity 2. A cylindrical boss 502 is also provided at the center of the upper surface of the pad 5. The diameter of the cylindrical boss 502 is 12~23mm, and the height is 2~16mm. The cylindrical boss 502 facilitates the compression of the foamed nickel sheet and the counter electrode 303.

[0052] An outer ring 7 is fitted on the outside of the insulating cavity 2. The inner diameter of the outer ring 7 is 58 mm and the outer diameter is 64 mm. The outer ring 7 is made of magnetized metal material, so that the outer ring 7 can be directly adsorbed on the sample stage of the X-ray diffraction and X-ray fluorescence instrument, which facilitates the quick loading and unloading of the sample cell.

[0053] Accordingly, a method for assembling a sample cell for in-situ X-ray diffraction and X-ray fluorescence coupling includes the following steps:

[0054] S1: With the lower surface of the positive electrode cover 1 facing upward, insert the window material 106 into the groove 101, so that the window material 106 is located at the connection between the measuring window 102 and the groove 101.

[0055] S2: Assemble the positive electrode sealing ring 208 in the first sealing groove 205, insert the boss 203 of the insulating cavity downward into the groove 101 of the positive electrode cover, and fasten the upper surface of the insulating cavity platform 202 to the lower surface of the positive electrode cover 1 through the second threaded hole 105 and the platform hole 206.

[0056] S3: In the glove box, the assembly of the electrode sheet 301, the diaphragm 302, the counter electrode 303 and the foam metal sheet 304 is completed in the inner cavity 201 of the insulating cavity; the sample to be tested composed of the electrode sheet 301, the diaphragm 302, the counter electrode 303 and the foam metal sheet 304 needs to be vacuum dried before assembly; when the sample to be tested is assembled, the powder layer of the electrode sheet 301 faces upwards, electrolyte is added on the surface of the electrode sheet 301, then the diaphragm 302 is assembled, electrolyte is added, and finally the counter electrode 303 and the foam metal sheet 304 are assembled;

[0057] S4: The cushion block 5 is pressed on the foam metal sheet 304, vacuum is drawn, and the negative electrode sealing ring 209 is assembled in the second sealing groove 204;

[0058] S5: One end of the elastic member 6 is assembled on the negative electrode cover boss 401, then the negative electrode cover 4 is placed on the lower surface of the insulating cavity platform 202, so that the elastic member 6 presses the cushion block 5, the insulating member is sleeved in the second through hole 405 of the lower surface of the negative electrode cover, and the upper surface of the negative electrode cover 4 is fastened to the lower surface of the insulating cavity platform 202 through the second threaded hole 105, the first through hole 207 and the second through hole 405;

[0059] S6: The outer ring 7 is sleeved on the outer side of the insulating cavity 2, and the sample cell is installed on the sample table of the X-ray diffraction and X-ray fluorescence instrument, the positive electrode tab 107 and the negative electrode tab 406 are respectively connected with the positive electrode and the negative electrode of the electrochemical workstation to realize in-situ testing, and the assembled sample cell is as shown in Figure 10 .

[0060] The in-situ testing of LiFePO4 is carried out by using the sample cell, Figure 11 The charge-discharge cycle curve of the LiFePO4 sample cell is as shown in Figure 11 It can be known that the capacity of the sample cell almost does not attenuate after 7 cycles, the platform voltage of the charge-discharge curve is stable, which indicates that the sample cell has good sealing performance, the structural members are in close contact, and the internal resistance is small. Figure 12 The in-situ XRD pattern of the LiFePO4 sample cell for the first time charge-discharge is as shown in Figure 12 It can be known that during charging, the diffraction peaks of the (020) and (311) crystal planes gradually weaken, and new phases are formed, and through analysis, it is concluded that new phases FePO4 are formed during the delithiation of the cathode LiFePO4, during discharging, the diffraction peaks of the (020) and (311) crystal planes return to the initial state, which indicates that FePO4 is converted into LiFePO4 during the lithium intercalation process, and thus it can be known that by using the sample cell for in-situ XRD testing, the change of the material structure during the charging and discharging process can be observed, which provides data support for mechanism research.

[0061] The above merely provides the specific embodiments of the present application, but the protection scope of the present application is not limited thereto, and any person skilled in the art can easily think of the changes or modifications within the technical range disclosed by the present application, which should be covered within the protection scope of the present application.

Claims

1. A sample cell for in situ X-ray diffraction and X-ray fluorescence, characterized by, The application relates to a positive electrode cover (1) provided with a groove (101) on the lower surface; an insulating cavity (2) in T shape, a boss (203) of the insulating cavity being inserted into the groove (101) of the positive electrode cover, and the upper surface of a platform (202) of the insulating cavity being in contact with and connected to the lower surface of the positive electrode cover (1); an electrode sheet (301), a diaphragm (302), a counter electrode (303) and a cushion block (5) being sequentially arranged in the inner cavity (201) of the insulating cavity from top to bottom; a foamed metal sheet (304) being arranged between the counter electrode (303) and the cushion block (5); a negative electrode cover (4) in T shape, a boss (401) of the negative electrode cover being inserted into the inner cavity (201) of the insulating cavity, and the upper surface of a platform (402) of the negative electrode cover being in contact with and connected to the lower surface of the platform (202) of the insulating cavity; an elastic member (6) being arranged on one end of the boss (401) of the negative electrode cover and being inserted into the inner cavity (201) of the insulating cavity and pressing the cushion block (5); a first sealing groove (205) being arranged on the upper surface of the boss (203) of the insulating cavity, and a positive electrode sealing ring (208) being arranged in the first sealing groove (205); a first annular boss (103) being arranged on the top surface of the groove (101) of the positive electrode cover and matched with the first sealing groove (205); a second sealing groove (204) being arranged on the lower surface of the platform (202) of the insulating cavity, and a negative electrode sealing ring (209) being arranged in the second sealing groove (204); a second annular boss (403) being arranged on the upper surface of the platform (402) of the negative electrode cover and matched with the second sealing groove (204); the cushion block (5) being in the shape of a cylinder, a third sealing groove (501) being arranged on the side surface of the cushion block (5), and a sealing ring being arranged in the third sealing groove (501); a measuring window (102) in the shape of an inverted cone being arranged on the upper surface of the positive electrode cover (1) corresponding to the inner cavity (201) of the insulating cavity, the measuring window (102) being communicated with the groove (101) of the positive electrode cover, and a window material (106) being arranged at the communication position of the measuring window (102) and the groove (101); an outer ring (7) being arranged on the outer side of the insulating cavity (2), and the outer ring (7) being made of magnetized material; and the following steps: S1, arranging the window material (106) at the communication position of the measuring window (102) and the groove (101) with the lower surface of the positive electrode cover (1) upward; S2, assembling the positive electrode sealing ring (208), inserting the boss (203) of the insulating cavity into the groove (101) of the positive electrode cover downward, and fastening the insulating cavity (2) to the lower surface of the positive electrode cover (1); S3, sequentially arranging the electrode sheet (301), the diaphragm (302), dropping the electrolyte, arranging the counter electrode (303) and the foamed metal sheet (304) in the inner cavity (201) of the insulating cavity in a glove box; S4, pressing the cushion block (5) on the foamed metal sheet (304), vacuumizing, and assembling the negative electrode sealing ring (209). ​ ​ ​ ​ ​ ​ ​ 2. The cell according to claim 1, wherein: ​ 3. The cell according to claim 1, wherein: ​ 4. A method of assembling a sample cell for in situ X-ray diffraction and X-ray fluorescence according to any one of claims 1 to 3, characterized in that ​ ​ ​ ​ ​ S5: the negative cover (4) with the assembled elastic member (6) is placed on the platform (202) of the insulating cavity, so that the elastic member (6) presses the cushion block (5), the insulating member is sleeved in the second through hole (405) of the negative cover (4), and the negative cover (4) is fastened to the lower surface of the platform (202) of the insulating cavity; S6: the outer ring (7) is sleeved on the outer side of the insulating cavity (2), the sample pool is installed on the sample table of the X-ray diffraction and X-ray fluorescence instrument, and the positive cover (1) and the negative cover (4) are respectively connected with the positive and negative electrodes of the electrochemical workstation, so that in-situ testing is realized.

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