An in-situ device for high-temperature hydrogen cell reactions using synchrotron radiation

Abstract

The present invention provides an in-situ device for high-temperature hydrogen battery reaction of synchrotron radiation, comprising a base, a ceramic support and a main body, wherein the main body comprises an in-situ box, a battery mounting plate installed in the cavity of the in-situ box and isolating the cavity into two air chambers, and a top cover installed on the top of the in-situ box; the high-temperature hydrogen battery is a thin-film battery, a through hole for accommodating the thin-film battery is provided at the center of the battery mounting plate, a temperature measuring couple and a heating electrode are respectively installed on the back and front of the battery mounting plate, and the centers of the temperature measuring couple and the heating electrode respectively have light holes; the in-situ box is provided with an incident light window, a laser heating window, a fluorescence window, and a diffraction window provided on the front side of the battery mounting plate and on the side wall of the in-situ box. The in-situ device of the present invention simultaneously meets the reaction requirements of the high-temperature hydrogen battery and the synchrotron radiation test requirements, so that synchrotron radiation characterization can be performed while the fuel cell reaction is in progress.

Description

Technical Field

[0001] The present invention relates to a synchrotron radiation in-situ device, in particular to an in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation. Background Art

[0002] As a representative of clean energy, hydrogen energy has many advantages such as high energy efficiency density, clean and pollution-free. How to safely use hydrogen energy is the key research direction for future scientific and technological development. Hydrogen fuel cells, as a new technology for green use of hydrogen energy, are widely studied by the scientific community. In the research process of hydrogen fuel cells, half of the battery's anode and cathode are plated on the surface of the film. When the fuel cell is working, the film will be heated to a high temperature of more than 600 or 700 degrees, and the anode and cathode will react in different atmospheres.

[0003] As a non-destructive characterization technology, synchrotron radiation can characterize the microstructure and chemical valence changes of materials. It is of great help in studying the reaction mechanism of fuel cells and finding and designing suitable catalysts, and is a reliable means of studying fuel cells. However, due to limited conditions, traditional synchrotron radiation methods can only characterize the first and last stages of the battery reaction, that is, pre-reaction characterization and post-reaction characterization, and know nothing about the changes during the reaction process.

[0004] Specifically, in the existing fuel cell devices, the hydrogen fuel cell devices that meet the high-temperature reaction conditions are only developed for battery energy reactions, and the requirements for the use of synchrotron radiation are not considered. Therefore, the fuel cell devices that meet the high-temperature reaction conditions cannot be used in synchrotron radiation devices. Existing synchrotron radiation tests require corresponding X-ray feed windows and signal output windows. This will destroy the original fuel cell device and make it impossible to achieve conditions such as high temperature. Therefore, the existing fuel cell devices that can be used in synchrotron radiation cannot meet the high-temperature reaction conditions and cannot perform high-temperature reactions. Therefore, the traditional synchrotron radiation method can only perform hydrogen reactions offline, and then the reaction products are tested by synchrotron radiation. Only the pre-reaction characterization and post-reaction characterization are known, and the changes during the reaction process are unknown. Summary of the invention

[0005] The present invention aims to provide an in-situ device for high-temperature hydrogen battery reaction under synchrotron radiation, so as to simultaneously meet the reaction requirements of high-temperature hydrogen battery and the synchrotron radiation testing needs, thereby enabling synchrotron radiation characterization to be performed simultaneously with the fuel cell reaction.

[0006] In order to achieve the above-mentioned object, the present invention provides an in-situ device for high-temperature hydrogen battery reaction under synchrotron radiation, comprising a base, a ceramic support and a main body which are fixedly connected in sequence from bottom to top, wherein the main body comprises an in-situ box with a sealed bottom and an open top, a battery mounting plate which is installed in the cavity of the in-situ box and isolates the cavity into two air chambers, and a top cover installed on the top of the in-situ box;

[0007] The high-temperature hydrogen battery is a thin-film battery. A through hole for accommodating the thin-film battery is provided at the center of the battery mounting plate. A temperature measuring couple and a heating electrode are respectively installed on the back and front of the battery mounting plate. The heating electrode and the temperature measuring couple clamp the thin-film battery therebetween. The centers of the temperature measuring couple and the heating electrode respectively have a first light through hole and a second light through hole.

[0008] The in-situ box is provided with a plurality of observation windows, including an incident light window located on the back side of the battery mounting plate and arranged on the side wall of the in-situ box, a laser heating window, a fluorescence window, and a diffraction window located on the front side of the battery mounting plate and arranged on the side wall of the in-situ box.

[0009] The top cover is mounted on the in-situ box by screws, a first battery positioning groove is provided at the center of the lower surface of the top cover, and a vacuum pad is provided between the first battery positioning groove and the battery mounting plate.

[0010] The top cover is provided with a first air outlet and a second air outlet on both sides of the first battery positioning groove, respectively. The first air outlet valve is installed on the first air outlet, and the second air outlet valve is installed on the second air outlet.

[0011] Two groups of oppositely arranged clamps are provided on the side walls of the in-situ box, each group of clamps includes two adjacent clamps, and the sides of the two adjacent clamps close to each other are affixed with clamp sealing strips, thereby, the clamps form a slot for inserting the battery mounting plate on the side wall of the in-situ box; and a second battery positioning groove is provided on the bottom wall of the in-situ box.

[0012] The bottom wall of the in-situ box is provided with a first air inlet hole for installing the first air inlet valve and a second air inlet hole for installing the second air inlet valve, which are located on both sides of the second battery positioning groove; the bottom wall of the in-situ box is also provided with a first vacuum plug and a second vacuum plug, which are located on both sides of the second battery positioning groove, and the first vacuum plug and the second vacuum plug are used to lead out the circuit of the temperature measuring couple, the circuit of the heating electrode and the circuit of the thin film battery.

[0013] The through hole of the battery mounting plate is surrounded by a plurality of threaded holes that penetrate the battery mounting plate, the temperature measuring thermocouple is fixed to the back side of the battery mounting plate through the first surface screws and the threaded holes, the battery mounting plate is fixed to the front side of the battery mounting plate through the second surface screws, and the sum of the lengths of the first surface screws and the second surface screws is less than the thickness of the battery mounting plate;

[0014] The first surface screws and the second surface screws are coated with vacuum glue, the temperature measuring couple is in close contact with the thin film battery, the temperature measuring couple is in close contact with the battery mounting plate, and the temperature measuring couple and the battery mounting plate are sealed with vacuum glue.

[0015] The temperature measuring thermocouple comprises a first cylinder and a first cylindrical boss which is arranged on the back of the first cylinder and has a smaller diameter than the first cylinder; the first light hole passes through the center of the first cylinder and the first cylindrical boss; the first light hole is composed of a temperature measuring wedge with an inclination angle of 45° and an incident wedge with an inclination angle of 50°; the angles between the surfaces of the incident light window and the fluorescent window and the surface of the thin film battery are both 40° and are respectively located on both sides of the laser heating window; a thermocouple wire is installed on the back of the temperature measuring wedge;

[0016] The heating electrode includes a second cylinder and a second cylindrical boss disposed on the back of the second cylinder and having a smaller diameter than the second cylinder. The second light hole passes through the centers of the second cylinder and the second cylindrical boss. The second light hole is wedge-shaped with an inclination angle of 45°.

[0017] The outer diameter of the first cylinder is 12mm and the thickness is 1.5mm; the diameter of the first cylindrical boss is 6mm and the height is 1.5mm; the diameter of the first light-through hole on the back of the temperature measuring couple is 2mm; the outer diameter of the second cylinder is 12mm and the thickness is 1.5mm; the diameter of the second cylindrical boss is 6mm and the height is 1mm; and the diameter of the second light-through hole on the back of the heating electrode is 2mm and the diameter on the front of the heating electrode is 7mm.

[0018] An incident light hole, a laser heating hole and a fluorescent hole are provided on the side wall of the in-situ box; the incident light window is pressed and fixed to the incident light hole of the in-situ box by an incident light window pressure ring; the laser heating window is pressed and fixed to the laser heating hole of the in-situ box by a laser heating window pressure ring; the fluorescent window is pressed and fixed to the fluorescent hole of the in-situ box by a fluorescent window pressure ring; the diameter of the light-through hole is 10 mm; the aperture of the laser heating hole is 15 mm; the diameter of the fluorescent hole is 6 mm; and a diffraction light hole is provided on the side wall of the in-situ box, and the diffraction window is pressed and fixed to the diffraction light hole of the in-situ box by a diffraction window pressure ring; the cross-section of the diffraction window is a rectangle of 40 mm×16 mm.

[0019] The battery mounting plate is made of refractory ceramics, and the top cover and the in-situ box are made of stainless steel.

[0020] The in-situ device for the high-temperature hydrogen battery reaction of synchrotron radiation of the present invention adopts laser heating to meet the atmosphere requirements and reaction requirements of the high-temperature hydrogen fuel cell, and the heat insulation design of the device can effectively protect the synchrotron radiation experimental platform, so that the reaction requirements of the high-temperature hydrogen battery and the synchrotron radiation test requirements can be met at the same time, so that synchrotron radiation in-situ characterization can be performed during the reaction process of the fuel cell. In addition, the in-situ device for the high-temperature hydrogen battery reaction of synchrotron radiation of the present invention adopts multiple observation windows, and can comprehensively utilize various methods in the synchrotron radiation method, such as synchrotron radiation fluorescence, absorption spectrum and diffraction method, to characterize the reaction process of the in-situ battery, especially during the battery reaction process, The state of the cathode, anode and catalyst can be characterized. The device is relatively small and can be used on a synchrotron radiation experimental platform. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 This is an overall structural diagram of an in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to an embodiment of the present invention.

[0022] Figure 2 For Figure 1 An exploded view of the main body of the in-situ device for the synchrotron radiation high-temperature hydrogen cell reaction is shown.

[0023] Figure 3 Yes Figure 1 A schematic structural diagram of the top cover of the in-situ device for high-temperature hydrogen cell reaction using synchrotron radiation and the components installed thereon is shown.

[0024] Figure 4 Yes Figure 1 A schematic structural diagram of a battery mounting plate and components mounted thereon of an in-situ device for a high-temperature hydrogen battery reaction under synchrotron radiation is shown.

[0025] Figure 5A-5C They are Figure 1 The front surface view, rear surface view and cross-sectional view of the thermocouple of the in-situ device of the synchrotron radiation high-temperature hydrogen cell reaction are shown.

[0026] Figure 6A-6C They are Figure 1 The front surface view, rear surface view and cross-sectional view of the heating electrode of the in-situ device for high-temperature hydrogen cell reaction under synchrotron radiation are shown.

[0027] Figure 7 Yes Figure 1 The structure diagram of the in-situ box of the in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation and the components installed thereon is shown.

[0028] Figure 8 Yes Figure 1A top view of the in-situ box of the in-situ device for the high-temperature hydrogen cell reaction using synchrotron radiation is shown.

[0029] Fig. 9 Yes Figure 1 The distribution diagram of the window of the in-situ box of the in-situ device of the high-temperature hydrogen battery reaction of synchrotron radiation is shown, where Fig. 9 The overall structure of the in-situ box is shown on the back side of the battery mounting plate. Fig.10 An exploded view showing the back side of the in-situ box located on the battery mounting plate, Fig.11 An exploded view of the in-situ box is shown on the front side of the battery mounting plate. DETAILED DESCRIPTION

[0030] The present invention is further described below in conjunction with specific examples. It should be understood that the following examples are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0031] like Figure 1 The figure shows an in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to an embodiment of the present invention, which includes a base 101, a ceramic support 102 and a main body 103 which are fixedly connected in sequence from bottom to top.

[0032] The in-situ device for the high-temperature hydrogen battery reaction of synchrotron radiation is installed on the synchrotron radiation experimental platform through the base 101. Since one synchrotron radiation platform can perform a variety of synchrotron radiation methods, the base 101 only needs to be installed on one synchrotron radiation experimental platform to enable the in-situ device for the high-temperature hydrogen battery reaction of synchrotron radiation of the present invention to perform a variety of synchrotron radiation methods. The base 101 is the interface for installing the in-situ device on the synchrotron radiation experimental platform. There are various types of synchrotron radiation experimental platforms, and they are all different. Therefore, the shape of the base 101 can be changed accordingly according to the type of platform. The material of the base 101 is aluminum alloy or stainless steel, without special requirements.

[0033] The ceramic pillar 102 is insulated by its ceramic material to prevent the high temperature of the in-situ device from being transmitted to the synchrotron radiation experimental platform, thereby protecting the synchrotron radiation experimental platform and stabilizing the temperature of the in-situ device; in addition, the upper and lower ends of the ceramic pillar 102 are respectively connected to the base 101 and the main body 103, thereby supporting the main body 103 from the base 101. In this embodiment, the ceramic pillar 102 is made of refractory ceramic (zirconia ceramic) and is cylindrical in shape. The diameter of the cylinder is 6 mm and the height is 40 mm. Among them, the height of the exposed part of the ceramic pillar 102 other than the connection part with the base 101 and the main body 103 is not less than 15 mm.

[0034] like Figure 2As shown, the main body 103 includes an in-situ box 201 with a sealed bottom and an open top, a battery mounting plate 202 installed in the cavity of the in-situ box 201 and isolating the cavity into two air chambers, and a top cover 203 installed on the top of the in-situ box 201 .

[0035] The top cover 203 is installed on the in-situ box 201 by screws, and is used to seal the two air chambers of the cavity of the in-situ box 201. A vacuum pad is provided between the top cover 203 and the in-situ box 201, and the vacuum pad is used to separate the two air chambers to prevent gas leakage. The material of the top cover 203 is stainless steel. Figure 3 As shown, the top cover 203 is provided with a first air outlet valve 302 and a second air outlet valve 303 which are independent of each other. After the top cover 203 is installed, the first air outlet valve 302 and the second air outlet valve 303 are respectively located on both sides of the battery mounting plate 202, thereby connecting the two air chambers mentioned above.

[0036] The top cover 203 has a first battery positioning groove 305 at the center of the lower surface thereof. The first battery positioning groove 305 is used to fix the battery mounting plate 202 and seal the battery mounting plate 202. Preferably, the vacuum pad is disposed between the first battery positioning groove 305 and the battery mounting plate 202. The top cover 203 has a first air outlet 306 and a second air outlet 304 on both sides of the first battery positioning groove 305, respectively. The first air outlet valve 302 is mounted on the first air outlet 306, and the second air outlet valve 303 is mounted on the second air outlet 304.

[0037] like Figure 4 As shown, the battery mounting plate 202 is a ceramic substrate, and an upper sealing strip 403 and a lower sealing strip 401 are respectively provided at the upper end and the lower end of the battery mounting plate 202.

[0038] The high-temperature hydrogen battery used in the present invention is a thin-film battery 406 with a sandwich structure. The middle of the thin-film battery 406 is a support material (the support material is similar to a plastic film). The two sides of the support material are a cathode and an anode respectively. The cathode and anode materials are not fixed, and different components are used according to experimental requirements. Therefore, the thin-film battery 406 is a multi-layer film with an overall thickness of about 0.15-0.5 mm. Therefore, the thin-film battery 406 can be sealed on the through hole in a form similar to a layer of plastic film, so that the X-ray can shine on the thin-film battery 406 in the process of passing through the through hole, and the detection signal after the X-ray passes through the thin-film battery 406 can also be transmitted through this through hole to the detector outside the in-situ device of the present invention.

[0039] The battery mounting plate 202 is used to install the thin film battery 406, and its material is refractory ceramic (i.e., zirconia ceramic), and its thickness is 2.4mm. The refractory ceramic has good thermal insulation, which not only ensures that the battery can be heated to the required temperature, but also effectively prevents the battery temperature from diffusing to the outer shell through heat conduction. In particular, the elements contained in the material are non-polluting to the thin film battery 406 and will not bring interference signals during testing. The upper sealing strip 403 and the lower sealing strip 401 are used to isolate the cavity of the in-situ box 201 into two different air chambers, and the material is preferably fluororubber. During the reaction process of the thin film battery 406, the positive and negative electrodes of the high-temperature hydrogen battery need to be under different atmospheric conditions, so two different air chambers need to be separated. There are no special requirements for the air pressure of the two air chambers, which are generally between 0-1.5 atmospheres and may change according to experimental requirements.

[0040] A through hole for accommodating a thin-film battery 406 is provided at the center of the battery mounting plate 202, and a plurality of threaded holes are provided around the through hole and penetrate the battery mounting plate 202. A thermocouple 405 fixed to the battery mounting plate 202 through a first face screw 404 and the threaded hole is installed on the back of the battery mounting plate 202, and a heating electrode 407 fixed to the battery mounting plate 202 through a second face screw 408 is installed on the front of the battery mounting plate 202. That is, a first face screw 404 is installed at one end of each threaded hole, and a second face screw 408 is installed at the other end, and the sum of the lengths of the first face screw 404 and the second face screw 408 must be less than the thickness of the battery mounting plate 202. The number of the threaded holes is preferably 4. Vacuum glue is applied to the first face screw 404 and the second face screw 408 to ensure that the threaded holes will not leak after assembly.

[0041] It is particularly noted that the battery mounting plate 406 needs to isolate the in-situ device into two independent air chambers, so there must be no gaps (leakage) on the battery mounting plate. The thermocouple 405 is close to the thin-film battery 406 to ensure the accuracy of temperature measurement during the experiment. In addition, the thermocouple 405 is close to the battery mounting plate 20 and the thermocouple 405 and the battery mounting plate 202 are sealed with vacuum glue, and after the installation is completed, the heating electrode 407 and the thermocouple 405 tightly clamp the thin-film battery 406 between the two, so that there is no gap between the thin-film battery 406 and the thermocouple 405, and the light hole on the thermocouple 405 is sealed by the thin-film battery 406, so as to ensure the independence of the two air chambers and prevent air leakage. The thin-film battery 406 plays the role of a sealing film here, and a light hole is provided in the center of the thermocouple 405, so after the thin-film battery 406 and the thermocouple 405 are close, it is ensured that the gas will not diffuse to the other side from the gap between them. There is no need to seal between the heating electrode 407 and the battery mounting plate 202. In order to ensure the tightness of the heating electrode 407 and the temperature measuring couple 405 clamping the thin film battery 406, there can be a slight gap between the heating electrode 407 and the battery mounting plate 202 after installation.

[0042] The installation process of the thin film battery 406, the thermocouple 405 and the heating electrode 407 is as follows: first, install the thermocouple closely attached to the thin film battery 406, so that the thermocouple 405 is closely attached to the battery mounting plate 202, and after the first screw 404 is tightened, spray vacuum glue to ensure sealing, so as to ensure that there is no gap between the thermocouple 405 and the battery mounting plate 202. Then install the heating electrode 407, so that the heating electrode 407 and the thermocouple 405 together tightly clamp the thin film battery 406, so as to ensure that there is no gap between the thin film battery 406 and the thermocouple 405.

[0043] Figure 5A-5C They are respectively the front surface view, the rear surface view and the cross-sectional view of the temperature measuring couple 405. Figure 5A-5C As shown, the thermocouple 405 includes a first cylinder 451, a first cylindrical boss 452 disposed on the back of the first cylinder 451 and having a smaller diameter than the first cylinder 451, and a first light hole 453 that passes through the center of the first cylinder 451 and the first cylindrical boss 452. A plurality of first screw through holes 454 for mounting the first face screws 404 are evenly distributed around the first cylinder 451. In this embodiment, the number of the first screw through holes 454 is 4.

[0044] In this embodiment, the outer diameter of the first cylinder 451 is 12 mm and the thickness is 1.5 mm. The diameter of the first cylindrical boss 452 is 6 mm and the height is 1.5 mm. The diameter of the first light hole 453 on the back of the temperature measuring couple is 2 mm.

[0045] A temperature measuring groove 455 is provided on the back of the temperature measuring thermocouple 405 for accommodating a thermocouple wire (not shown) for temperature measurement. The thermocouple wire is an existing one, and pt100 can be used.

[0046] At least a portion of the first light hole 453 is wedge-shaped. In this embodiment, the first light hole 453 is composed of a temperature measuring wedge 4531 with an inclination angle of 45° and an incident wedge 4532 with an inclination angle of 50°, wherein the temperature measuring wedge occupies half of the hole and the incident wedge 4532 occupies the other half. The incident wedge 4532 is used to meet the requirement that the X-rays in the fluorescence experiment have an incident angle of 45° with the battery surface, so that the incident light will not interfere with the temperature measuring thermocouple 405. A thermocouple wire is installed on the back of the temperature measuring wedge 4531. Specifically, the temperature measuring groove 455 is arranged on the back side of the first cylinder 451 and the first cylindrical boss 452 corresponding to the temperature measuring wedge 4531, so that the temperature measuring groove 455 is a blind hole and its end can be as close to the first light-transmitting hole 453 as possible, so that the temperature measurement is more accurate. Considering the metal strength and processing difficulty, the distance between the end of the temperature measuring groove 455 and the surface of the temperature measuring wedge 4531 is generally more than 0.5 mm. The galvanic wire is used to test the temperature of the thin-film battery, so it needs to be as close to the thin-film battery as possible, but if it is too close to the first light-transmitting hole 453, it will also interfere with the test. Here, the temperature measuring groove 455 adopts a blind hole, and its end does not penetrate the surface of the temperature measuring wedge 4531, to ensure that the galvanic wire will not accidentally extend into the optical path and interfere with the test results, and the complete wedge surface is beneficial for suppressing stray light in the experiment.

[0047] Figure 6A-6C They are respectively a front surface view, a rear surface view and a cross-sectional view of the heating electrode 407. Figure 6A-6C As shown, the heating electrode 407 includes a second cylinder 471, a second cylindrical boss 472 disposed on the back of the second cylinder 471 and having a smaller diameter than the second cylinder 471, and a second light hole 473 that passes through the center of the second cylinder 471 and the second cylindrical boss 472. The second cylindrical boss 472 is used to insert into the through hole in the center of the battery mounting plate 202 and clamp the thin film battery 406, so that the heating effect is better. A plurality of second screw through holes 474 for mounting the second face screws 408 are evenly distributed around the second cylinder 471. In this embodiment, a power pin 475 is provided on one side of the second cylinder 471, and the number of the second screw through holes 474 is 3, and the second screw through holes 474 are distributed on the other three sides of the second cylinder 471 except the power pin. The heating electrode 407 is electrically connected to the power supply through the power pin 475, so that heating is achieved by power supply. The power source is disposed outside the main body 103 and is connected to the power pin 475 via wires and vacuum plugs 805 , 806 .

[0048] In this embodiment, the outer diameter of the second cylinder 471 is 12 mm and the thickness is 1.5 mm. The diameter of the second cylindrical boss 472 is 6 mm and the height is 1 mm. The second light hole 473 is a wedge with an inclination angle of 45°. The diameter of the second light hole 473 on the back side of the heating electrode 407 is 2 mm, and the diameter on the front side of the heating electrode 407 is 7 mm.

[0049] Figure 7 2 is an appearance diagram of the in-situ box 201 and the components installed thereon. Figure 7 As shown, the in-situ box 201 is a cylindrical box body, which has a bottom wall and a side wall, a first air inlet valve 701 and a second air inlet valve 702 are provided at the bottom, and an in-situ box sealing ring 704 is provided at the upper edge of the side wall. The first air inlet valve 701 and the second air inlet valve 702 are used to supply air to the two air chambers in the cavity of the in-situ box 201 respectively, and the in-situ box sealing ring 704 is used to seal between the in-situ box 201 and the top cover 203. The in-situ box 201 is made of stainless steel, and an observation window, a test interface and an air supply interface are provided on the side wall.

[0050] The first air inlet valve 701 and the second air inlet valve 702 are structurally the same as the first air outlet valve 302 and the second air outlet valve 303 described above, but have different functions and are not interchangeable. The in-situ device in this case is a reaction device for a hydrogen fuel cell at high temperature. It is necessary to heat the surface of the thin-film battery to a high temperature (above 700°) so that the anode and cathode of the thin-film battery react in different atmospheres. The atmosphere can act as a catalyst or be used as a reaction raw material in a chemical reaction, so fresh gas must be supplied all the time. The present invention arranges the first air outlet valve 302 and the second air outlet valve 303 at the bottom of the main body and the first air inlet valve 701 and the second air inlet valve 702 at the top of the main body, and adopts a bottom-in and top-out method, which helps to effectively discharge the hot exhaust gas after the reaction.

[0051] In this embodiment, the diameter of the original box 201 is 60 mm, the height is 50 mm, and the material is stainless steel. The bottom wall and the side wall of the original box 201 are used as the bottom wall and the side wall of the original box 201, and the wall thickness of the bottom wall and the side wall of the original box 201 are both 5 mm.

[0052] Figure 8 FIG. 2 is a top view of the in-situ box 201, which shows the internal structure of the in-situ box 201. Figure 8As shown, the bottom wall of the in-situ box 201 is provided with a first air inlet hole 801 for installing the first air inlet valve 701 and a second air inlet hole 802 for installing the second air inlet valve 702. Two groups of oppositely arranged clamping plates 803 are provided on the side wall of the in-situ box 201, each group of clamping plates 803 includes two adjacent clamping plates 803, and the sides of the two adjacent clamping plates 803 close to each other are affixed with clamping plate sealing strips (not shown in the figure), thereby, the clamping plates 803 form a slot for inserting the battery mounting plate 202 provided on the side wall of the in-situ box 201, and the bottom wall of the in-situ box 201 is provided with a second battery positioning groove 804, and the second air inlet hole 802 of the second air inlet valve 702 is located on both sides of the second battery positioning groove 804, and the slot and the second battery positioning groove 804 are used to limit the battery mounting plate 202 and maintain sealing. The bottom wall of the in-situ box 201 is also provided with a first vacuum plug 805 and a second vacuum plug 806 located on both sides of the second battery positioning groove 804, which are used to lead out the circuit of the temperature measuring couple 405, the circuit of the heating electrode 407, and the circuit of the thin film battery 406, so that the experiment can use two methods of laser heating or electrode heating, or use these two methods at the same time. In addition, the first vacuum plug 805 and the second vacuum plug 806 can also reserve some circuit interfaces for expanding functions, such as adding gas flow sensors, component analysis sensors, etc. in the in-situ box 201, and the circuits of these sensors also need to lead out devices from the first vacuum plug 805 and the second vacuum plug 806.

[0053] Figure 9-11 2 is a distribution diagram of the windows of the in-situ box 201. The in-situ box 201 is provided with a plurality of observation windows, including an incident light window 901 located on the back side of the battery mounting plate 202 and provided on the side wall of the in-situ box 201, a laser heating window 902, a fluorescent window 903, and a diffraction window 904 provided on the front side of the battery mounting plate 202 and provided on the side wall of the in-situ box 201.

[0054] The angles between the surfaces of the incident light window 901 and the fluorescent window 903 and the surface of the thin film battery 406 are both 45° and they are located on both sides of the laser heating window 902, so that the fluorescent yield is the highest. In addition, the incident light window 901 is aligned with the incident wedge 4532 of the first light hole 453. The surface of the laser heating window 902 is parallel to the surface of the thin film battery 406 and faces the thin film battery 406, so that the efficiency of laser heating is the highest.

[0055] The side wall of the in-situ box 201 is provided with an incident light hole, a laser heating hole and a fluorescent hole. The incident light window 901 is pressed and fixed on the incident light hole of the in-situ box 201 by an incident light window pressing ring 1003, the laser heating window 902 is pressed and fixed on the laser heating hole of the in-situ box 201 by a laser heating window pressing ring 1006, and the fluorescent window 903 is pressed and fixed on the fluorescent hole of the in-situ box 201 by a fluorescent window pressing ring 1009, so as to ensure the passage of X-rays, heating lasers and fluorescent light respectively while taking into account the sealing of gas. In this embodiment, the incident light window 901 and the fluorescent window 903 are made of 0.2mm thick polyamide film. In other embodiments, the materials of the incident light window 901 and the fluorescent window 903 can be replaced by other materials that can transmit X-rays and will not interfere with the test of thin film batteries, and the thickness of the incident light window 901 can be 50um-500um. The laser heating window 902 is made of a quartz window with a thickness of 1 mm. The quartz window has good transparency and the best absorption of the visible light band. As a laser feed window, it has the highest efficiency.

[0056] The diameter of the light-through hole is 10mm. The aperture of the laser heating hole is 15mm. The diameter of the fluorescence hole is 6mm. The aperture of the fluorescence hole matches the fluorescence detector, which can ensure the fluorescence acceptance angle while reducing stray light signals. The larger the fluorescence acceptance angle, the better, but due to the thermal insulation requirements of the device, the fluorescence window must maintain a certain distance from the thin-film battery. The farther the thermal insulation needs to be, the better, and the closer the fluorescence experiment requires, the better. In this embodiment, the distance between the fluorescence window and the thin-film battery is selected to be 26.5mm, so that the heat of the thin-film battery will not destroy the fluorescence window, and the thin-film battery will not dissipate heat too quickly. At this distance, the fluorescence detector should be as close to the fluorescence window as possible. The effective diameter of the fluorescence detector probe is generally around 5mm, and the fluorescence window should be slightly larger than the effective diameter of the fluorescence probe. If a fluorescence probe with a larger detection area is selected, the fluorescence window also needs to be enlarged accordingly.

[0057] A diffraction light hole is provided on the side wall of the in-situ box 201, and the diffraction window 901 is pressed and fixed on the diffraction light hole of the in-situ box 201 by a diffraction window pressing ring 1103, so as to ensure the transmission of the X-ray and the diffraction X-ray while taking into account the sealing of the air chamber. In this embodiment, the diffraction window 901 adopts a 0.5 mm thick polyamide film. In other embodiments, due to the large size of the diffraction window 901, only a 0.5-1 mm polyamide film can be used, but the thinner the film, the better the X-ray penetration.

[0058] The cross-section of the diffraction window 901 is a 40mm×16mm rectangle, and this size can strike a balance between the diffraction solid angle and the thermal insulation effect of the cavity. Specifically, the diffraction window 904 needs to be as large as possible. The larger the diffraction window 904 is, the more diffraction signals can be received (high-angle diffraction signals). However, the diffraction window 904 cannot be too large. The window on the outer shell has an impact on the thermal insulation and temperature stability of the thin-film battery 406. A window that is too large is not conducive to the heating of the thin-film battery 406, nor is it conducive to maintaining a stable temperature during the reaction. In other embodiments, the size of the diffraction window 901 can be reduced, but cannot be less than 38.44X16mm, otherwise the transmitted light cannot pass through the device. The window cannot be enlarged either. The larger it is, the more serious the impact on the temperature stability of the thin-film battery. At the size of 40mm×16mm, the diffraction angle range is 0-92.11°.

[0059] In addition, the synchrotron radiation platform is provided with an X-ray source located outside the in-situ box 201 and facing the incident light window 901, a laser facing the laser heating window 902, a fluorescence detector facing the fluorescence window 903, and an X-ray detector facing the diffraction window 901. Thus, the incident X-ray enters the device from the incident light window 901, irradiates the thin film battery 406, and stimulates a fluorescence signal. The fluorescence signal will radiate 360° in all directions, wherein part of the signal passes through the in-situ box 201 from the fluorescence window 903 and is received by the fluorescence detector outside the in-situ box 201. Among the fluorescence signals transmitted from the fluorescence window 903, the elastic scattering signal of the thin film battery 406 is the least (the stray interference signal is the least), so the fluorescence signal quality is the highest. The laser heating window faces the thin film battery 406, the window material absorbs the least visible light, the laser power can act on the surface of the thin film battery 406 to the maximum extent, and the heating effect is the best.

[0060] The above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. The above embodiments of the present invention can also be modified in various ways. All simple, equivalent changes and modifications made according to the claims and the description of the present invention fall within the scope of protection of the claims of the present invention. The contents not described in detail in the present invention are all conventional technical contents.

Claims

1. An in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation, characterized in that: It comprises a base, a ceramic support and a main body which are fixedly connected in sequence from bottom to top, wherein the main body comprises an in-situ box with a sealed bottom and an open top, a battery mounting plate which is installed in the cavity of the in-situ box and isolates the cavity into two air chambers, and a top cover which is installed on the top of the in-situ box; The high-temperature hydrogen battery is a thin-film battery. A through hole for accommodating the thin-film battery is provided at the center of the battery mounting plate. A temperature measuring couple and a heating electrode are respectively installed on the back and front of the battery mounting plate. The heating electrode and the temperature measuring couple clamp the thin-film battery therebetween. The centers of the temperature measuring couple and the heating electrode respectively have a first light through hole and a second light through hole. The in-situ box is provided with a plurality of observation windows, including an incident light window located on the back side of the battery mounting plate and arranged on the side wall of the in-situ box, a laser heating window, a fluorescence window, and a diffraction window located on the front side of the battery mounting plate and arranged on the side wall of the in-situ box.

2. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: The top cover is mounted on the in-situ box by screws, a first battery positioning groove is provided at the center of the lower surface of the top cover, and a vacuum pad is provided between the first battery positioning groove and the battery mounting plate.

3. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 2, characterized in that: The top cover is provided with a first air outlet and a second air outlet on both sides of the first battery positioning groove, respectively. The first air outlet valve is installed on the first air outlet, and the second air outlet valve is installed on the second air outlet.

4. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: Two groups of oppositely arranged clamps are provided on the side walls of the in-situ box, each group of clamps includes two adjacent clamps, and the sides of the two adjacent clamps close to each other are affixed with clamp sealing strips, thereby, the clamps form a slot for inserting the battery mounting plate on the side wall of the in-situ box; and a second battery positioning groove is provided on the bottom wall of the in-situ box.

5. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 4, characterized in that: The bottom wall of the in-situ box is provided with a first air inlet hole for installing the first air inlet valve and a second air inlet hole for installing the second air inlet valve, which are located on both sides of the second battery positioning groove; the bottom wall of the in-situ box is also provided with a first vacuum plug and a second vacuum plug, which are located on both sides of the second battery positioning groove, and the first vacuum plug and the second vacuum plug are used to lead out the circuit of the temperature measuring couple, the circuit of the heating electrode and the circuit of the thin film battery.

6. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: The through hole of the battery mounting plate is surrounded by a plurality of threaded holes that penetrate the battery mounting plate, the temperature measuring thermocouple is fixed to the back side of the battery mounting plate through the first surface screws and the threaded holes, the battery mounting plate is fixed to the front side of the battery mounting plate through the second surface screws, and the sum of the lengths of the first surface screws and the second surface screws is less than the thickness of the battery mounting plate; The first surface screws and the second surface screws are coated with vacuum glue, the temperature measuring couple is in close contact with the thin film battery, the temperature measuring couple is in close contact with the battery mounting plate, and the temperature measuring couple and the battery mounting plate are sealed with vacuum glue.

7. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: The temperature measuring thermocouple comprises a first cylinder and a first cylindrical boss which is arranged on the back of the first cylinder and has a smaller diameter than the first cylinder; the first light hole passes through the center of the first cylinder and the first cylindrical boss; the first light hole is composed of a temperature measuring wedge with an inclination angle of 45° and an incident wedge with an inclination angle of 50°; the angles between the surfaces of the incident light window and the fluorescent window and the surface of the thin film battery are both 40° and are respectively located on both sides of the laser heating window; a thermocouple wire is installed on the back of the temperature measuring wedge; The heating electrode includes a second cylinder and a second cylindrical boss disposed on the back of the second cylinder and having a smaller diameter than the second cylinder. The second light hole passes through the centers of the second cylinder and the second cylindrical boss. The second light hole is wedge-shaped with an inclination angle of 45°.

8. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 7, characterized in that: The outer diameter of the first cylinder is 12mm and the thickness is 1.5mm; the diameter of the first cylindrical boss is 6mm and the height is 1.5mm; the diameter of the first light-through hole on the back of the temperature measuring couple is 2mm; the outer diameter of the second cylinder is 12mm and the thickness is 1.5mm; the diameter of the second cylindrical boss is 6mm and the height is 1mm; and the diameter of the second light-through hole on the back of the heating electrode is 2mm and the diameter on the front of the heating electrode is 7mm.

9. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: An incident light hole, a laser heating hole and a fluorescent hole are provided on the side wall of the in-situ box; the incident light window is pressed and fixed to the incident light hole of the in-situ box by an incident light window pressure ring; the laser heating window is pressed and fixed to the laser heating hole of the in-situ box by a laser heating window pressure ring; the fluorescent window is pressed and fixed to the fluorescent hole of the in-situ box by a fluorescent window pressure ring; the diameter of the light-through hole is 10 mm; the aperture of the laser heating hole is 15 mm; the diameter of the fluorescent hole is 6 mm; and a diffraction light hole is provided on the side wall of the in-situ box, and the diffraction window is pressed and fixed to the diffraction light hole of the in-situ box by a diffraction window pressure ring; the cross-section of the diffraction window is a rectangle of 40 mm×16 mm.

10. The in-situ device for high-temperature hydrogen battery reaction using synchrotron radiation according to claim 1, characterized in that: The battery mounting plate is made of refractory ceramics, and the top cover and the in-situ box are made of stainless steel.

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