Device for high and low temperature synchrotron radiation in-situ characterization of zinc ion battery

Abstract

The invention discloses a device for high and low temperature synchrotron radiation in-situ characterization of a zinc ion battery. The device comprises an electrode carrier, a first electrode shell, a second electrode shell and a temperature adjusting assembly, the electrode carrier is provided with an electrode chamber for loading a to-be-detected electrode material of the zinc ion battery; the first electrode shell is assembled on the first end surface of the electrode carrier, and is provided with a first wiring structure and a first incident structure communicated with the electrode chamber; the second electrode shell is assembled on the second end surface of the electrode carrier, and is provided with a second wiring structure and an emergent structure communicated with the electrode chamber; the first incident structure and the emergent structure are collinear, and the first electrode shell and the second electrode shell can also be conducted with a to-be-detected electrode material in the electrode chamber; the temperature adjusting assembly is used for adjusting the temperature of the electrode chamber so that the electrode chamber can be at a high temperature or a low temperature, in-situ characterization can be conveniently conducted on the zinc ion battery in a low-temperature or high-temperature environment, and therefore research on the zinc ion battery under the low-temperature or high-temperature working condition can be conveniently achieved.

Description

Technical Field

[0001] The invention relates to the technical field of aqueous zinc ion batteries, and in particular to a device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries. Background Art

[0002] Aqueous zinc-ion batteries have become an important candidate for lithium-ion batteries due to their better safety, lower cost, higher ionic conductivity, simpler preparation process and higher ecological benefits. However, the poor performance of aqueous zinc-ion batteries under low and high temperature conditions has become one of the important factors hindering their large-scale commercial use. Therefore, the in-situ characterization of aqueous zinc-ion batteries under high and low temperature conditions is of great significance for the research of zinc-ion batteries, and can also provide an important means for electrochemical temperature-variable in-situ testing.

[0003] In-situ characterization refers to the characterization of batteries in direct operation, which can observe the structural changes of the battery during operation. It plays an important role in the in-depth understanding of the structural transformation and transformation mechanism of each component of the battery during the charge and discharge process and the electrochemical reaction mechanism of the battery, and is conducive to revealing the mechanism of performance degradation during the cycle of zinc-ion batteries. Among them, synchrotron radiation technology can be used to perform in-situ characterization of zinc-ion battery materials. However, the existing technology is still unable to perform in-situ characterization of zinc-ion battery materials under low or high temperature environments, which is not conducive to the study of zinc-ion batteries under such conditions. Summary of the invention

[0004] In view of this, the present invention provides a device for in-situ characterization of zinc ion batteries using high and low temperature synchrotron radiation, which can perform in-situ characterization of electrode materials to be tested of zinc ion batteries under low or high temperature environments, which can facilitate the study of zinc ion batteries under low or high temperature conditions.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries, comprising: an electrode carrier, a first electrode shell, a second electrode shell and a temperature regulating component;

[0007] The electrode carrier has an electrode chamber and is used to load the electrode material to be tested of the zinc ion battery;

[0008] The first electrode shell is mounted on the first end surface of the electrode carrier and is provided with a first wiring structure and a first incident structure connected to the electrode chamber;

[0009] The second electrode shell is mounted on the second end surface of the electrode carrier, and is provided with a second wiring structure, and an exit structure connected to the electrode chamber; wherein the first incident structure and the exit structure are collinear, and the first electrode shell and the second electrode shell can also be connected to the electrode material to be tested in the electrode chamber;

[0010] The temperature regulating component is used to regulate the temperature of the electrode chamber so that the electrode chamber is at a high temperature or a low temperature.

[0011] Preferably, the temperature regulating component comprises:

[0012] A heating component disposed in the electrode chamber;

[0013] A cooling liquid circulation channel is provided in the electrode carrier and is used to cool the electrode chamber; wherein the electrode carrier is capable of heat conduction, and the cooling liquid in the cooling liquid circulation channel is provided by an external cooling liquid circulation system;

[0014] A temperature sensor is disposed in the electrode chamber.

[0015] Preferably, the coolant circulation channel is an annular structure and is distributed around the electrode chamber;

[0016] The outer side wall of the electrode carrier is respectively provided with a coolant inlet and a coolant outlet;

[0017] The coolant inlet is used to be connected to the liquid inlet pipe of the coolant circulation system and is connected to the coolant circulation channel; the coolant outlet is used to be connected to the liquid return pipe of the coolant circulation system and is connected to the coolant circulation channel.

[0018] Preferably, the temperature increasing component comprises a heating probe.

[0019] Preferably, the electrode chamber passes through the first end surface and the second end surface of the electrode carrier;

[0020] The second electrode shell is capable of contacting and conducting with the electrode material to be tested in the electrode chamber; the first electrode shell is contacting and conducting with the electrode material to be tested in the electrode chamber through a conducting component; wherein the conducting component is provided with a through second incident structure, and the first incident structure, the second incident structure and the emission structure are collinear in sequence.

[0021] Preferably, the conductive component is an elastic conductive component, which can provide elastic pressure for the electrode material to be tested in the electrode chamber, so that the electrode material to be tested is fixed between the elastic conductive component and the second electrode shell.

[0022] Preferably, the elastic conduction component comprises: a spring and a gasket;

[0023] The first end surface of the gasket is provided with a positioning column, and the second end surface is used for contacting and cooperating with the electrode material to be tested;

[0024] The spring is sleeved on the positioning column of the gasket, and the first end of the spring is in abutment with the first electrode shell, and the second end of the spring is in abutment with the first end surface of the gasket;

[0025] The second incident structure passes through the positioning post and the gasket.

[0026] Preferably, the electrode chamber is a cylindrical electrode chamber;

[0027] The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries also includes an insulating ferrule;

[0028] The insulating ferrule is sleeved on the inner circumferential wall of the cylindrical electrode chamber, and the conductive component and the electrode material to be tested are both located in the insulating ferrule;

[0029] The first electrode shell is insulated from a first end surface of the electrode carrier, and the second electrode shell is insulated from a second end surface of the electrode carrier.

[0030] Preferably, the first incident structure comprises a first incident hole and is used for incident synchrotron radiation X-rays;

[0031] The second incident structure includes a second incident hole;

[0032] The emission structure includes an emission hole.

[0033] Preferably, it also includes: a first sealing ring and a second sealing ring;

[0034] The first end surface of the electrode carrier is provided with a first sealing ring groove, and the second end surface is provided with a second sealing ring groove, and both are distributed around the electrode chamber;

[0035] The first sealing ring is installed in the first sealing ring groove and abuts against the first electrode shell; the second sealing ring is installed in the second sealing ring groove and abuts against the second electrode shell.

[0036] It can be seen from the above technical solutions that the device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided by the present invention can facilitate the charge and discharge cycle of the electrode material to be tested of the zinc ion battery by connecting the first wiring structure of the first electrode shell and the second wiring structure of the second electrode shell to the external circuit respectively, and the first electrode shell and the second electrode shell are connected to the electrode material to be tested in the electrode chamber, and can facilitate the in-situ characterization of the electrode material to be tested of the zinc ion battery by synchrotron radiation technology through the collinear arrangement of the first incident structure of the first electrode shell and the second incident structure of the second electrode shell, and adjust the temperature of the electrode chamber by the temperature adjustment component so that the electrode material to be tested in the electrode chamber is in a high temperature or low temperature environment, so that the electrode material to be tested of the zinc ion battery can be conveniently characterized in-situ under low temperature or high temperature environment, so as to facilitate the research of zinc ion batteries under low temperature or high temperature conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0038] Figure 1 A schematic diagram of the structure of a device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided in an embodiment of the present invention;

[0039] Figure 2 A structural front view of a device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided in an embodiment of the present invention;

[0040] Figure 3 for Figure 2 AA section view;

[0041] Figure 4 A structural segmentation diagram of a device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided in an embodiment of the present invention;

[0042] Figure 5 A structural exploded view of a device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided in an embodiment of the present invention;

[0043] Figure 6 A schematic diagram of the front structure of a second electrode shell provided by an embodiment of the present invention;

[0044] Figure 7 A schematic diagram of the back structure of the second electrode shell provided in an embodiment of the present invention.

[0045] Wherein, 1 is a first electrode shell, 101 is a first incident hole, 102 is a thermocouple hole, 103 is a heating probe hole, and 104 is a first terminal hole;

[0046] 2 is a second electrode shell, 201 is an exit hole, 202 is a polyetheretherketone threaded washer, 203 is a second terminal hole, 204 is a washer groove, and 205 is a groove;

[0047] 3 is an electrode carrier, 301 is a coolant inlet, 302 is a coolant outlet, 303 is a first sealing ring groove, 304 is a second sealing ring groove, 305 is a coolant circulation channel, 306 is an upper end surface, and 307 is a lower end convex surface;

[0048] 4 is a spring;

[0049] 5 is a gasket, 501 is a second incident hole;

[0050] 6 is an insulating ferrule;

[0051] 7 is an electrode chamber;

[0052] 8 is a positioning column. DETAILED DESCRIPTION

[0053] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0054] The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided in the embodiment of the present invention is as follows: Figure 1 As shown, it includes: a first electrode shell 1, a second electrode shell 2, an electrode carrier 3 and a temperature regulating component;

[0055] like Figure 4 As shown, the electrode carrier 3 has an electrode chamber 7 and is used to load the electrode material to be tested of the zinc ion battery;

[0056] The first electrode shell 1 is mounted on the first end surface of the electrode carrier 3 and is provided with a first wiring structure and a first incident structure connected to the electrode chamber 7;

[0057] The second electrode shell 2 is mounted on the second end surface of the electrode carrier 3, and is provided with a second wiring structure, and an exit structure connected to the electrode chamber 7; wherein the first incident structure and the exit structure are collinear, and the first electrode shell 1 and the second electrode shell 2 can also be connected to the electrode material to be tested in the electrode chamber 7;

[0058] The temperature regulating assembly is used to regulate the temperature of the electrode chamber 7 so that the electrode chamber 7 is at a high temperature or a low temperature.

[0059] It should be noted that the electrode chamber 7 of the electrode carrier 3 is used to load or place the electrode material to be tested of the zinc ion battery; wherein the electrode material to be tested of the zinc ion battery may include battery components such as a positive electrode material, a negative electrode material, a separator and an electrolyte;

[0060] The first electrode shell 1 can be used as a positive electrode shell, and can be assembled to the first end surface of the electrode carrier 3 by screws, and the first electrode shell 1 is insulated from the first end surface of the electrode carrier 3; wherein, Figure 2 and Figure 3 As shown, the first end surface of the electrode carrier 3 may be the upper end surface 306 of the electrode carrier 3; Figure 1 As shown, the first wiring structure may be a first terminal hole 104, which is used to install the first terminal, and then connected to the external circuit (battery cycle test equipment) through the first terminal; the first incident structure may be a first incident hole 101, which is used to incident synchrotron radiation X-rays, and then facilitates in-situ characterization of zinc ion battery materials through synchrotron radiation technology;

[0061] The second electrode shell 2 can be used as a negative electrode shell, and can be assembled to the second end surface of the electrode carrier 3 by screws, and the second electrode shell 2 is insulated from the second end surface of the electrode carrier 3; wherein, Figure 2 and Figure 3 As shown, the second end surface of the electrode carrier 3 may be the lower end surface of the electrode carrier 3, and the first end surface and the second end surface of the electrode carrier 3 are actually distributed relatively; Figure 1 As shown, the second wiring structure may be a second terminal hole 203, which is used to install the second terminal, and then connected to the external circuit (battery cycle test equipment) through the second terminal; Figure 4 As shown, the exit structure may be an exit hole 201, and may be distributed relative to the first entrance hole 101, so as to facilitate the injection and emission of synchrotron radiation X-rays; the first electrode shell 1 and the second electrode shell 2 may also be conductive with the electrode material to be tested loaded in the electrode chamber 7, so that the electrode material to be tested is conductive between the first electrode shell 1 and the second electrode shell 2, so that the first wiring structure and the second wiring structure are connected to an external circuit, so as to facilitate the charge and discharge cycle of the electrode material to be tested; in addition, the first electrode shell 1, the second electrode shell 2, and the electrode carrier 3 may all be made of titanium metal material;

[0062] The temperature regulating component is used to regulate the temperature of the electrode chamber 7 so that the electrode chamber 7 is at a high temperature or a low temperature; of course, the temperature regulating component has the function of heating and cooling; that is, the temperature of the electrode chamber 7 is heated or cooled by the temperature regulating component so that the electrode chamber 7 is in a high temperature or a low temperature environment, thereby facilitating the in-situ characterization of zinc ion battery materials under a low temperature or a high temperature environment, thereby facilitating the research of zinc ion batteries under low temperature or high temperature conditions.

[0063] In other words, this device can allow the electrode materials of the zinc-ion battery to be charged and discharged in a high-temperature or low-temperature environment, and can also perform real-time synchrotron radiation X-ray in-situ characterization of the positive and negative electrodes, diaphragms, electrolytes and other components of the zinc-ion battery.

[0064] In summary, the present solution actually provides an in-situ cell for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries. By connecting the first wiring structure of the first electrode shell 1 and the second wiring structure of the second electrode shell 2 to the external circuit respectively, and the first electrode shell 1 and the second electrode shell 2 are connected to the electrode material to be tested in the electrode chamber 7, it is convenient to realize the charge and discharge cycle of the electrode material to be tested of the zinc ion battery. By setting the first incident structure of the first electrode shell 1 and the second incident structure of the second electrode shell 2 in a colinear manner, it is convenient to perform in-situ characterization of the electrode material to be tested of the zinc ion battery by synchrotron radiation technology. The temperature of the electrode chamber 7 is adjusted by the temperature adjustment component so that the electrode material to be tested in the electrode chamber 7 is in a high temperature or low temperature environment, so that the electrode material to be tested of the zinc ion battery can be conveniently characterized in situ under low temperature or high temperature environment, which can facilitate the research of zinc ion batteries under low temperature or high temperature conditions.

[0065] In this scheme, if Figure 3 and Figure 4 As shown, the temperature regulation assembly includes:

[0066] A heating component disposed in the electrode chamber 7;

[0067] A cooling liquid circulation channel 305 is provided in the electrode carrier 3 and is used to cool the electrode chamber 7; wherein the electrode carrier 3 is capable of heat conduction, and the cooling liquid in the cooling liquid circulation channel 305 is provided by an external cooling liquid circulation system;

[0068] A temperature sensor is provided in the electrode chamber 7 .

[0069] It should be noted that the temperature-raising component can be a heating component, and is used to heat the electrode chamber 7 so that the electrode chamber 7 is at a high temperature; as described above, the titanium metal material used in the electrode carrier 3 is capable of heat conduction, and the coolant circulation channel 305 is arranged in the electrode carrier 3, and can be distributed around the electrode chamber 7, or can be distributed in a spiral shape around the electrode chamber 7, so as to cool the electrode chamber 7 to the greatest extent, and the coolant can be provided to the coolant circulation channel 305 through an external coolant circulation system; wherein, the liquid inlet of the coolant circulation channel 305 can be used to communicate with the coolant The liquid inlet of the cooling liquid circulation system is connected, and the liquid outlet can be used to be connected to the liquid return port of the cooling liquid circulation system, so that the cooling liquid forms a circulation loop in the electrode carrier 3, which is used to realize water cooling of the electrode chamber 7; of course, the cooling liquid circulation system can provide cooling liquids of different temperatures to cool the electrode chamber 7 to different temperatures; the temperature sensor arranged in the electrode chamber 7 is used to monitor the temperature of the electrode chamber 7 in real time, and can also realize feedback after temperature adjustment; of course, in order to avoid conflicts, when the temperature of the electrode chamber 7 is increased, the cooling should be turned off, and when the temperature is reduced, the heating should be turned off.

[0070] That is to say, the temperature regulating component includes: a heating part (heating component), a cooling part (cooling liquid circulation channel 305) and a feedback part (temperature sensor). This has obvious functions and is convenient for the electrode chamber 7 to achieve high and low temperature regulation. Moreover, the heating part and the feedback part are directly arranged in the electrode chamber 7, and the cooling part adopts the liquid cooling circulation channel built into the electrode carrier 3, so as to avoid the temperature regulating component occupying too much space of the electrode carrier 3, that is, the device can be compact in structure and reasonably laid out.

[0071] Specifically, Figure 4 As shown, the coolant circulation channel 305 is a ring-shaped structure and is distributed around the electrode chamber 7;

[0072] The outer side wall of the electrode carrier 3 is respectively provided with a coolant inlet 301 and a coolant outlet 302;

[0073] The coolant inlet 301 is used to be connected to the liquid inlet pipe of the coolant circulation system and communicated with the coolant circulation channel 305 ; the coolant outlet 302 is used to be connected to the liquid return pipe of the coolant circulation system and communicated with the coolant circulation channel 305 .

[0074] It should be noted that if Figure 5 As shown, the electrode chamber 7 may be a cylindrical electrode chamber, and the coolant circulation channel 305 may be an annular channel and distributed around the cylindrical electrode chamber. Of course, it also needs to be close to the cylindrical electrode chamber to form an annular coolant circulation channel around the electrode chamber 7, so that the electrode chamber 7 can obtain a better cooling effect; wherein, the coolant circulation channel 305 may be an integrated coolant circulation channel, and the electrode carrier 3 may be manufactured by 3D printing technology; as shown Figure 4As shown, the coolant inlet 301 can be arranged along the radial direction of the cylindrical electrode chamber, and its outer end is used to connect with the inlet pipe of the coolant circulation system, and the inner end is communicated with the coolant circulation channel 305; the coolant outlet 302 can be arranged along the radial direction of the cylindrical electrode chamber, and its outer end is used to connect with the return pipe of the coolant circulation system, and the inner end is communicated with the coolant circulation channel 305; of course, as Figure 4 As shown, the coolant inlet 301 and the coolant outlet 302 can be symmetrically distributed about the cylindrical electrode chamber. In this way, the coolant of the coolant circulation system flows from the coolant inlet 301 into the coolant circulation channel 305, and then flows back to the coolant circulation system from the coolant outlet 302. In this way, the electrode chamber 7 can be continuously cooled by surrounding water, so that the electrode chamber 7 can obtain a better cooling effect. In addition, Figure 4 As shown, the outer port of the coolant inlet 301 may be provided with an internal thread for screwing with the first heat-conducting copper tube, and then connected to the liquid inlet pipe of the coolant circulation system through the first heat-conducting copper tube; similarly, the outer port of the coolant outlet 302 may be provided with an internal thread for screwing with the second heat-conducting copper tube, and then connected to the liquid return pipe of the coolant circulation system through the second heat-conducting copper tube.

[0075] That is to say, the coolant circulation channel 305 of the electrode carrier 3 can form a circulation loop around the electrode chamber 7 in the electrode carrier 3 by connecting with the external coolant circulation system, and based on the thermal conductivity of the electrode carrier 3, the electrode chamber 7 can obtain a better cooling effect, and the temperature of the electrode chamber 7 can be reduced to a preset low temperature by changing the temperature of the coolant in the coolant circulation system; in addition, the coolant is not limited in composition, and dry ice gas or liquid nitrogen, etc. can be used.

[0076] Furthermore, the heating component includes a heating probe, which can make the electrode chamber 7 convenient to heat, and will not occupy too much space in the electrode chamber 7. Of course, this solution can also use other heating components, such as heating wires. Figure 1As shown, the first electrode shell 1 may be provided with a heating probe hole 103 connected to the electrode chamber 7, and the heating probe is installed in the electrode chamber 7 through the heating probe hole 103 of the first electrode shell 1; in addition, the temperature sensor includes a thermocouple; the first electrode shell 1 may also be provided with a thermocouple hole 102 connected to the electrode chamber 7, and the thermocouple is installed in the electrode chamber 7 through the thermocouple hole 102 of the first electrode shell 1; of course, after the heating probe and the thermocouple are installed in the electrode chamber 7 through their respective holes, polyimide film tape should be used to seal the heating probe hole 103 and the thermocouple hole 102 respectively to prevent the thermocouple and the heating probe from shifting during use, thereby avoiding battery short circuit, inability to control temperature, or blocking of synchrotron radiation signals, etc. Among them, through the action of the heating probe and the coolant circulation loop, a closed environment of -70°C to 100°C can be formed in the electrode chamber 7, and the temperature of the electrode chamber 7 can be adjusted to -70°C~100°C, so that the zinc ion battery can be monitored in situ within the temperature range of -70°C to 100°C, thus solving the problem that the prior art cannot adjust the temperature (control the temperature) and the temperature adjustment range is too narrow when using synchrotron radiation technology to perform in situ characterization of zinc ion battery materials.

[0077] Furthermore, if Figure 3 As shown, the electrode chamber 7 penetrates the first end surface and the second end surface of the electrode carrier 3;

[0078] The second electrode shell 2 can be in contact with and conduct with the electrode material to be tested in the electrode chamber 7; the first electrode shell 1 is in contact with and conducts with the electrode material to be tested in the electrode chamber 7 through a conducting component; wherein the conducting component is provided with a through second incident structure, and the first incident structure, the second incident structure and the ejection structure are collinear in sequence.

[0079] It should be noted that, as described above, the first end surface of the electrode carrier 3 may be the upper end surface 306, and the second end surface may be the lower end surface. Figure 4 As shown, the electrode chamber 7 also passes through the upper and lower end surfaces of the electrode carrier 3, and the electrode chamber 7 is also the hollow chamber of the electrode carrier 3. In this way, the electrode material to be tested loaded in the electrode chamber 7 can be distributed at the lower end of the electrode chamber 7, which is convenient for contacting and conducting with the upper end surface of the second electrode shell 2, and the first electrode shell 1 is then contacted and conducted with the electrode material to be tested distributed at the lower end of the electrode chamber 7 through the conducting component, thereby ensuring that the electrode material to be tested is conducted between the first electrode shell 1 and the second electrode shell 2;

[0080] In addition, in order to avoid interference with the incident synchrotron radiation X-rays, the conductive component is provided with a through second incident structure, and the first incident structure, the second incident structure and the emission structure are arranged in a colinear manner, that is, the first incident structure, the second incident structure and the emission structure are arranged relatively in sequence; wherein, the second incident structure can be an incident hole; and the through-type design of the electrode chamber 7 also facilitates the first incident structure and other structures of the first electrode shell 1 to be connected to the electrode chamber 7, and the second incident structure and other structures of the second electrode shell 2 to be connected to the electrode chamber 7; of course, when the first electrode shell 1 is assembled on the upper end face 306 of the electrode carrier 3, the upper port of the electrode chamber 7 can be sealed, and when the second electrode shell 2 is assembled on the lower end face of the electrode carrier 3, the lower port of the electrode chamber 7 can be sealed.

[0081] In this solution, the conductive component is an elastic conductive component, which can provide elastic pressure for the electrode material to be tested in the electrode chamber 7, so that the electrode material to be tested is fixed between the elastic conductive component and the second electrode shell 2. That is to say, the conductive component can not only play a conductive role, but also play a role in elastically pressing the electrode material to be tested, thereby fixing the electrode material to be tested loaded in the electrode chamber 7, avoiding shaking of the electrode material to be tested during in-situ characterization, thereby ensuring the stability of the test of the electrode material to be tested.

[0082] Specifically, Figure 4 and Figure 5 As shown, the elastic conduction component includes: a spring 4 and a gasket 5;

[0083] The first end surface of the gasket 5 is provided with a positioning column 8, and the second end surface is used for contacting and matching with the electrode material to be tested;

[0084] The spring 4 is sleeved on the positioning column 8 of the gasket 5, and the first end of the spring 4 is in abutment with the first electrode shell 1, and the second end of the spring 4 is in abutment with the first end surface of the gasket 5;

[0085] The second incident structure passes through the positioning column 8 and the gasket 5 .

[0086] It should be noted that if Figure 4 As shown, the first end surface of the gasket 5 can be the upper end surface, and the second end surface can be the lower end surface. Figure 5As shown, the upper end surface of the gasket 5 may be provided with a positioning column 8, that is, the gasket 5 is a two-stage stepped gasket, and the lower end surface of the gasket 5 is used to contact and conduct with the electrode material to be tested; the spring 4 is sleeved on the positioning column 8 of the gasket 5, and abuts between the first electrode shell 1 and the first end surface of the gasket 5, and is used to provide elastic pressure for the gasket 5, so that the gasket 5 elastically presses the electrode material to be tested, that is, the electrode material to be tested is fixed between the gasket 5 and the second electrode shell 2; of course, the spring 4 is in a compressed state at this time; wherein, the outer diameter of the positioning column 8 and the inner diameter of the spring 4 can be adapted (matched), so that the spring 4 is just sleeved on the positioning column 8 without shaking, ensuring the stability of the spring 4 sleeved or sleeved; in addition, the second incident structure can be an incident hole, and passes through the positioning column 8 and the gasket 5 in sequence, and can be distributed in the center of the positioning column 8 and the gasket 5. In addition, the spring 4, the gasket 5 and the positioning column 8 can all be made of titanium metal material. Of course, the elastic conductive component is designed in this way, which has a simple structure, is convenient to press and easy to assemble.

[0087] Furthermore, if Figure 4 As shown, the electrode chamber 7 is a cylindrical electrode chamber;

[0088] like Figure 5 As shown, the device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries also includes an insulating ferrule 6;

[0089] like Figure 4 As shown, the insulating ferrule 6 is sleeved on the inner circumferential wall of the cylindrical electrode chamber, and the conductive component and the electrode material to be tested are both located inside the insulating ferrule 6;

[0090] The first electrode shell 1 is insulated from a first end surface of the electrode carrier 3 , and the second electrode shell 2 is insulated from a second end surface of the electrode carrier 3 .

[0091] It should be noted that the electrode chamber 7 can be a cylindrical electrode chamber that penetrates the upper and lower end surfaces of the electrode carrier 3; Figure 1As shown, the electrode carrier 3 can adopt a cylindrical structure, and the cylindrical electrode chamber is concentric with the electrode carrier 3, so that the electrode carrier 3 forms a circular ring structure; the insulating ring 6 is sleeved on the inner circumferential wall of the cylindrical electrode chamber, and the conductive component and the electrode material to be tested are both arranged in the insulating ring 6, so that the electrode carrier 3 and the conductive component are separated from the electrode material to be tested, so that the conductive component and the electrode material to be tested are isolated from the electrode carrier 3, which can not only avoid the electrode carrier 3 from affecting the test result of the electrode material to be tested, but also prevent the external circuit from being short-circuited due to accidentally touching the electrode carrier 3 when an external circuit is connected. Condition; wherein, the insulating ferrule 6 can be made of polyetheretherketone, and its corrosion resistance is better than that of the electrode carrier 3, and its outer diameter is adapted to the inner diameter of the electrode chamber 7, so that the outer peripheral wall of the insulating ferrule 6 contacts the inner peripheral wall of the electrode chamber 7, and the insulating ferrule 6 can be fixed in the electrode chamber 7; of course, the setting of the insulating ferrule 6 can also play a positioning role for the battery material to be tested, further improving the airtightness inside the device, while also slowing down the external influence on the temperature of the battery material to be tested, improving the stability of the internal temperature of the device, and optimizing the test effect of the device; of course, the electrode chamber 7 can also be a square columnar electrode chamber;

[0092] In addition, after the first electrode shell 1 is assembled on the first end surface of the electrode carrier 3, it is also insulated from the first end surface of the electrode carrier 3; wherein the first electrode shell 1 can be fastened and insulated with the first end surface of the electrode carrier 3 by a plurality of insulating screws, and an insulating tape can be laid between the first electrode shell 1 and the first end surface of the electrode carrier 3, and the insulating screws can be made of polyetheretherketone;

[0093] In addition, after the second electrode shell 2 is assembled on the second end surface of the electrode carrier 3, it is also insulated from the second end surface of the electrode carrier 3; Figure 7 As shown, the lower end surface (bottom surface) of the second electrode shell 2 may be provided with a plurality of gasket grooves 204, and the gasket grooves 204 may be evenly distributed around the center of the second electrode shell 2, as shown in FIG. Figure 3As shown, multiple polyetheretherketone threaded washers 202 can be installed one by one in multiple washer grooves 204 on the lower end face of the second electrode shell 2. After the second electrode shell 2 is installed on the second end face of the electrode carrier 3, multiple titanium metal conductive screws are installed one by one in multiple polyetheretherketone threaded washers 202, and the second electrode shell 2 and the second end face of the electrode carrier 3 are fastened, that is, the second electrode shell 2 can be fastened to the second end face of the electrode carrier 3 by multiple titanium metal conductive screws, and polyetheretherketone threaded washers 202 are provided between the titanium metal conductive screws and the second electrode shell 2 to separate the second electrode shell 2 and the titanium metal conductive screws to prevent metal-to-metal wear and metal penetration molding during high and low temperature changes; of course, insulating tape can be laid between the second electrode shell 2 and the second end face of the electrode carrier 3. In other words, the first end face of the first electrode shell 1 and the electrode carrier 3, and the second end face of the second electrode shell 2 and the electrode carrier 3 are insulated and not in direct contact, so as to avoid a short circuit between the first electrode shell 1 and the second electrode shell 2.

[0094] Furthermore, if Figure 4 As shown, the first incident structure includes a first incident hole 101, and is used to incident synchrotron radiation X-rays; of course, if other technologies are used to perform in-situ characterization of the electrode material of the zinc ion battery, the first incident hole 101 of the first electrode shell 1 can also be used to incident the medium used for in-situ characterization of the electrode material in the technology;

[0095] The second incident structure includes a second incident hole 501;

[0096] The emission structure includes an emission hole 201 .

[0097] Among them, Figure 4 As shown, the first incident hole 101, the second incident hole 501 and the exit hole 201 are distributed from top to bottom in sequence, and as shown in FIG. Figure 3 As shown, the first incident hole 101 can be located at the center of the first electrode shell 1, the second incident hole 501 can be located at the center of the positioning column 8 and the gasket 5, and the exit hole 201 can be located at the center of the second electrode shell 2, and the first incident hole 101, the second incident hole 501 and the exit hole 201 can all be cylindrical through holes; in addition, to ensure the sealing of the device, the first incident hole 101 can be sealed flatly with a polyimide film tape, and the exit hole 201 can be sealed flatly with a polyimide film tape. In other words, the first incident structure, the second incident structure and the exit structure all adopt a through hole structure, so the structure is simple and easy to process.

[0098] In addition, if Figure 1As shown, the first wiring structure of the first electrode shell 1 can be the first terminal hole 104, and the second wiring structure of the second electrode shell 1 can be the second terminal hole 203; wherein, a banana head (which can be used as a terminal) can be installed in the first terminal hole 104 and the second terminal hole 203. When in use, the first electrode shell 1 and the second electrode shell 2 can be connected to an external circuit (battery cycle test equipment) respectively through the banana head to realize charge and discharge cycles for the electrode material to be tested.

[0099] In this solution, the device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries provided by the embodiment of the present invention further includes: a first sealing ring and a second sealing ring;

[0100] like Figure 3 As shown, a first sealing ring groove 303 is formed on the first end surface of the electrode carrier 3, and a second sealing ring groove 304 is formed on the second end surface, and both of them are distributed around the electrode chamber 7;

[0101] The first sealing ring is installed in the first sealing ring groove 303 and abuts against the first electrode shell 1 ; the second sealing ring is installed in the second sealing ring groove 304 and abuts against the second electrode shell 2 .

[0102] It should be noted that the first sealing ring groove 303 can be a first annular groove and can be distributed around the electrode chamber 7. The first sealing ring can be a first annular sealing ring. The first annular sealing ring can be adapted to be installed in the first annular groove and protrude from the first end face of the electrode carrier 3. When the first electrode shell 1 is assembled on the first end face of the electrode carrier 3, it abuts against the bottom surface of the first electrode shell 1, so that the outer ring between the first electrode shell 1 and the upper end of the electrode chamber 7 forms a seal, ensuring the sealing of the first electrode shell 1 and the upper end of the electrode chamber 7. Similarly, the second sealing ring groove 304 can be a second annular groove and can be distributed around the electrode chamber 7. The second sealing ring can be a second annular sealing ring, which can be adapted to be installed in the second annular groove and protrude from the second end face of the electrode carrier 3, and abut against the top surface of the second electrode shell 2 when the second electrode shell 2 is assembled on the second end face of the electrode carrier 3, so that the outer ring between the second electrode shell 2 and the lower port of the electrode chamber 7 forms a seal, thereby ensuring the sealing of the second electrode shell 2 and the lower port of the electrode chamber 7.

[0103] In addition, in order to realize the rapid positioning and assembly of the second electrode shell 2 and the lower end surface (second end surface) of the electrode carrier 3, as shown in FIG. Figure 4 As shown, the lower end surface of the electrode carrier 3 may be provided with a boss, such as Figure 6 As shown, the upper end surface of the second electrode shell 2 may be provided with a groove 205 for positioning and matching with the boss on the lower end surface of the electrode carrier 3. Figure 3As shown, the second sealing ring groove 304 may be provided on the lower end convex surface 307 of the electrode carrier 3 (the lower end surface of the boss of the electrode carrier 3 ).

[0104] In addition, the process of in-situ characterization of the electrode material to be tested of the zinc ion battery in the in-situ cell (i.e., the device) using synchrotron radiation technology is described as follows:

[0105] The electrode materials to be tested of the zinc ion battery are placed in the electrode chamber 7 of the in-situ cell in order, and then the in-situ cell is assembled, and then the in-situ cell is connected to an external cooling circuit (i.e., a coolant circulation system), and the in-situ cell is connected to a test circuit (i.e., a battery cycle test device), and then the in-situ cell is irradiated with synchrotron radiation light of different energies, so that the synchrotron radiation light enters from a first incident port of the in-situ cell and leaves from an exit port of the in-situ cell. At the same time, the signal generated by the interaction of the synchrotron radiation light with the electrode material to be tested is received by a detector located near the exit port. According to the difference in the energy of the light band and the type of the detected signal, it can be divided into XAFS, in-situ XRD, etc.

[0106] The present invention is further described below in conjunction with specific embodiments:

[0107] The present invention provides an in-situ cell suitable for controllable high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries, wherein the in-situ cell comprises a first electrode shell 1, a second electrode shell 2 and a temperature control ring (i.e., an electrode carrier 3, the same below).

[0108] Among them, the first electrode shell 1 is made of titanium metal material, and is provided with a first incident hole 101, a thermocouple hole 102, a heating probe hole 103 and a first terminal hole 104; wherein, the first incident hole 101, the thermocouple hole 102 and the heating probe hole 103 are through holes, and the first terminal hole 104 is a blind hole; when in use, the thermocouple hole 102 and the heating probe hole 103 should be sealed with polyimide film tape after the thermocouple and the heating probe are inserted respectively, so as to prevent the thermocouple and the heating probe from shifting during use, so as to avoid causing battery short circuit, failure to control temperature or blocking synchrotron radiation signals, etc.; at the same time, the first incident hole 101 is sealed flatly with polyimide film tape.

[0109] The second electrode shell 2 is made of titanium metal material, and is provided with an outlet hole 201, a second terminal hole 203 and a gasket groove 204; a groove 205 is provided on the side of the second electrode shell 2 away from the gasket groove 204, and the groove 205 is adapted to the lower convex surface 307 on the temperature control ring; when in use, the outlet hole 201 is sealed by flattening with a polyimide film tape.

[0110] The banana plug (as a terminal) is installed in the first terminal hole 104 and the second terminal hole 203. When in use, the first electrode shell 1 and the second electrode shell 2 are connected to an external circuit through the terminal to realize the charge and discharge cycle of the battery.

[0111] The first electrode shell 1 and the second electrode shell 2 form a closed electrode chamber 7 in the cavity of the temperature control ring.

[0112] Among them, the fastening spring (i.e., spring 4), gasket 5, and insulating ring 6 are arranged in the electrode chamber 7. The gasket 5 is provided with a second incident hole 501 and a step-shaped structure (i.e., positioning column 8), which is adapted to the fastening spring and is used to position the fastening spring; when in use, one end of the gasket 5 is connected to one pole of the battery material to be tested, and the other end is connected to the first electrode shell 1 through the fastening spring, and the other pole of the battery material to be tested is directly in contact with the second electrode shell 2, so that the battery material to be tested is conductive between the first electrode shell 1 and the second electrode shell 2.

[0113] The first electrode shell 1 is provided with a first incident hole 101, the second electrode shell 2 is provided with an exit hole 201, and the gasket 5 is provided with a second incident hole 501. The first incident hole 101, the second incident hole 501 and the exit hole 201 are distributed in sequence.

[0114] Among them, the temperature control ring is made of titanium metal and has a hollow "U"-shaped structure. A lower end convex surface 307 is provided on the opposite side of its upper end surface 306, which is compatible with the groove 205 of the second electrode shell 2; the upper end surface 306 of the temperature control ring is a flat surface, and a first sealing ring groove 303 is provided, and a second sealing ring groove 304 is provided on the lower end convex surface 307, and a coolant inlet 301 and a coolant outlet 302 are provided on the temperature control ring.

[0115] When in use, the first heat-conducting copper tube and the second heat-conducting copper tube are connected to the coolant inlet 301 and the coolant outlet 302 one by one, and are connected to the external coolant circulation system, so that the coolant enters the integrated coolant loop in the cavity (i.e., the coolant circulation channel 305, the same below) from the coolant inlet 301, and is discharged from the coolant outlet 302, forming a complete coolant circulation loop.

[0116] The first electrode shell 1 is insulated and fastened to the upper end surface of the temperature control ring by a polyetheretherketone insulating screw, and the second electrode shell 2 is conductively fastened to the temperature control ring by a polyetheretherketone threaded washer 202 and a titanium metal conductive screw. The first electrode shell 1 and the second electrode shell 2 are in contact with the opposite side surfaces of the temperature control ring respectively, and the first electrode shell 1 and the second electrode shell 2 are not in direct contact to avoid a short circuit.

[0117] During assembly, the fastening spring, the gasket 5 , the insulating ferrule 6 , the positive electrode material, the negative electrode material, the diaphragm and the electrolyte to be tested are placed in the electrode chamber 7 .

[0118] It should be noted that the integrated cooling liquid loop in the cavity of the present device is used to conduct heat to the entire device. The integrated cooling liquid loop in the cavity can be connected to the external circulating cooling liquid to form a closed loop, and the thermal conductivity of titanium metal is used to cool the entire device, thereby realizing in-situ monitoring of zinc ion batteries in the temperature range of -70°C to 100°C; the integrated cooling liquid loop in the cavity is not limited to shape, and can be converted into a heat-conducting copper tube as needed; the coolant is not limited to the composition, and dry ice gas, liquid nitrogen, etc. can be used, and the temperature of the entire zinc ion battery controllable high and low temperature synchrotron radiation in-situ characterization device can be changed by changing the temperature of the external circulating cooling liquid, and can also be heated and accurately monitored in real time by thermocouples and heating probes placed in the electrode chamber 7.

[0119] In one embodiment, if Figure 3 As shown, an insulating collar 6 is provided in the electrode chamber 7, and the outer wall of the insulating collar 6 is in close contact with the inner wall of the temperature control ring and is fixed in the electrode chamber 7, so as to position the battery to be tested and further improve the airtightness inside the in-situ pool, while reducing the influence of the outside world on the temperature of the battery to be tested, improving the stability of the temperature inside the in-situ pool, and optimizing the in-situ pool test effect.

[0120] The in-situ cell of the present invention has a simple structure, readily available materials, and is easy to assemble. It can be used to assemble into a full cell or a half cell for synchrotron radiation X-ray in-situ testing, thereby reducing the difficulty of the test and avoiding possible damage and loss during assembly, disassembly or transfer of electrode materials, thereby improving test efficiency and the accuracy of characterization results.

[0121] Finally, it should be noted that the technical solutions not described in detail in this application may adopt publicly known technologies.

[0122] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0123] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries, characterized in that: include: An electrode carrier (3), a first electrode shell (1), a second electrode shell (2) and a temperature regulating component; The electrode carrier (3) has an electrode chamber (7) and is used to load the electrode material to be tested of the zinc ion battery; The first electrode shell (1) is mounted on a first end surface of the electrode carrier (3), and is provided with a first wiring structure, and a first incident structure connected to the electrode chamber (7); The second electrode shell (2) is mounted on the second end surface of the electrode carrier (3), and is provided with a second wiring structure, and is provided with an exit structure connected to the electrode chamber (7); wherein the first incident structure and the exit structure are collinear, and the first electrode shell (1) and the second electrode shell (2) are also capable of conducting with the electrode material to be tested in the electrode chamber (7); The temperature regulating component is used to regulate the temperature of the electrode chamber (7) so that the electrode chamber (7) is at a high temperature or a low temperature.

2. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 1, characterized in that: The temperature regulating component comprises: A temperature increasing component disposed in the electrode chamber (7); a cooling liquid circulation channel (305) provided in the electrode carrier (3) and used for cooling the electrode chamber (7); wherein the electrode carrier (3) is capable of heat conduction, and the cooling liquid in the cooling liquid circulation channel (305) is provided by an external cooling liquid circulation system; A temperature sensor is arranged in the electrode chamber (7).

3. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 2, characterized in that: The coolant circulation channel (305) is an annular structure and is distributed around the electrode chamber (7); The outer side wall of the electrode carrier (3) is respectively provided with a cooling liquid inlet (301) and a cooling liquid outlet (302); The coolant inlet (301) is used to be connected to a liquid inlet pipe of the coolant circulation system and is communicated with the coolant circulation channel (305); the coolant outlet (302) is used to be connected to a liquid return pipe of the coolant circulation system and is communicated with the coolant circulation channel (305).

4. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 2, characterized in that: The temperature raising component includes a heating probe.

5. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 1, characterized in that: The electrode chamber (7) penetrates the first end surface and the second end surface of the electrode carrier (3); The second electrode shell (2) is capable of contacting and conducting with the electrode material to be tested in the electrode chamber (7); the first electrode shell (1) is in contact and conducting with the electrode material to be tested in the electrode chamber (7) via a conducting component; wherein the conducting component is provided with a through second incident structure, and the first incident structure, the second incident structure and the emission structure are collinear in sequence.

6. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 5, characterized in that: The conductive component is an elastic conductive component, which can provide elastic pressure for the electrode material to be tested in the electrode chamber (7), so that the electrode material to be tested is fixed between the elastic conductive component and the second electrode shell (2).

7. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 6, characterized in that: The elastic conduction component comprises: a spring (4) and a gasket (5); The first end surface of the gasket (5) is provided with a positioning column (8), and the second end surface is used for contacting and cooperating with the electrode material to be tested; The spring (4) is sleeved on the positioning column (8) of the gasket (5), and the first end thereof is in abutment with the first electrode shell (1), and the second end thereof is in abutment with the first end surface of the gasket (5); The second incident structure passes through the positioning column (8) and the gasket (5).

8. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 5, characterized in that: The electrode chamber (7) is a cylindrical electrode chamber; The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries also includes an insulating ferrule (6); The insulating ferrule (6) is sleeved on the inner circumferential wall of the cylindrical electrode chamber, and the conductive component and the electrode material to be tested are both located inside the insulating ferrule (6); The first electrode shell (1) is insulated from a first end surface of the electrode carrier (3), and the second electrode shell (2) is insulated from a second end surface of the electrode carrier (3).

9. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 5, characterized in that: The first incident structure comprises a first incident hole (101) and is used for incident synchrotron radiation X-rays; The second incident structure comprises a second incident hole (501); The emission structure comprises an emission hole (201).

10. The device for high and low temperature synchrotron radiation in-situ characterization of zinc ion batteries according to claim 5, characterized in that: Also includes: a first sealing ring and a second sealing ring; The first end surface of the electrode carrier (3) is provided with a first sealing ring groove (303), and the second end surface is provided with a second sealing ring groove (304), and both are distributed around the electrode chamber (7); The first sealing ring is installed in the first sealing ring groove (303) and is in abutment with the first electrode shell (1); the second sealing ring is installed in the second sealing ring groove (304) and is in abutment with the second electrode shell (2).

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