Temperature-controllable objective table suite for in-situ XRD (X-Ray Diffraction) test

Abstract

The utility model relates to a temperature-controllable objective table kit for an in-situ XRD (X-Ray Diffraction) test, and relates to the technical field of instrument analysis. Comprising a lower adjusting frame and a soaking table, the shape and the size of the adjusting frame are determined according to a target X-ray diffractometer type objective table to be applied, and high-matching-degree installation with an original type is achieved. Temperature control of the integrated soaking table is achieved through a low-temperature liquid cooling channel and a high-temperature electric heating channel, in the low-temperature channel, cooling liquid flows into an outlet channel from an inlet channel and flows out, and cooling temperature control of-40 DEG C to 25 DEG C is achieved on the soaking table through a circulation loop; the high-temperature passage is realized by a temperature control heating assembly, the assembly comprises a precise thermocouple and a matched electric heating disc, and the high-temperature control of 25-380 DEG C is realized on the soaking table. The device is simple in structure and convenient to mount, is compatible with various XRD test instruments, can realize ex-situ / in-situ XRD detection of various samples in a wide temperature range of-40 DEG C to 380 DEG C by matching with various sample tables, and can realize high and low temperature control and XRD online analysis of battery charging and discharging behaviors by matching with an in-situ electrochemical XRD battery assembly.

Description

Technical Field

[0001] This invention relates to the field of instrumental analysis technology, and specifically to a temperature-controlled stage kit for in-situ XRD. Background Technology

[0002] X-ray diffraction (XRD) is a crucial characterization technique in materials science for studying the composition and structure of materials. It effectively analyzes the crystal structure and relative content of different structures, and is widely used in battery energy storage and other materials fields. Common in-situ XRD techniques include in-situ variable-temperature XRD and in-situ electrochemical XRD. In-situ variable-temperature XRD typically characterizes the compositional and crystalline changes of solid materials from room temperature to high temperatures. In-situ electrochemical XRD, on the other hand, provides crystallographic information about electrodes during charge and discharge at ambient temperatures, such as the real-time changes in the crystal structure of positive and negative electrode materials. The combination of these two in-situ techniques allows for a deeper understanding of the reactions occurring in electrode materials during charge and discharge at different temperatures, which is crucial for elucidating important topics such as the failure mechanisms of high and low temperature batteries.

[0003] The invention patent CN 115144419 A from Harbin Institute of Technology relates to a temperature-controlled battery in-situ XRD testing device and its battery components and testing method. The testing temperature is between -20℃ and 60℃, but it is difficult to achieve a testing temperature higher than 60℃. Moreover, the device is too complex and can only be applied to a few XRD testing devices.

[0004] Traditional in-situ XRD electrochemical testing limits the battery testing temperature to the temperature inside the XRD apparatus's detection chamber, making it impossible to meet the requirements of specific environmental temperatures. Furthermore, the in-situ testing process is time-consuming, and continuous X-ray irradiation causes significant heat buildup on the sample stage, resulting in test results that differ considerably from the actual battery condition under real-world operating conditions. Summary of the Invention

[0005] The present invention aims to provide a highly compatible integrated temperature-controlled stage kit for in-situ XRD testing. When used with a conventional sample stage, it can realize crystallographic data of samples at low to high temperatures. When used with an electrochemical sample stage, it can realize electrochemical in-situ XRD testing under controlled temperature conditions.

[0006] The technical solution adopted in this invention is:

[0007] A temperature-controlled stage kit for in-situ XRD testing includes: an adjustment frame, a heat exchanger, a heating wire, and a thermocouple. The heat exchanger includes a connecting part and a loading part. A groove is provided on the upper surface of the loading part for placing the experimental object. A heating wire and a thermocouple are located at the bottom of the groove on the upper surface of the loading part, with their connection ports located on the side wall of the loading part. A coolant channel is provided inside the loading part near the upper surface, and an inlet and outlet for the coolant channel are provided on the side wall of the loading part. The cylindrical connecting part is located on the lower surface of the loading part. The connecting part is threadedly connected to the adjustment frame, allowing the heat exchanger to be adjusted relative to the adjustment frame by rotation. The thermocouple is used to collect temperature data from the loading part.

[0008] Furthermore, the connecting part is a cylinder with external threads, and the adjusting bracket is an annular ring with internal threads, with the external threads and internal threads meshing with each other.

[0009] Furthermore, the heat exchange platform is made of metal and has internal fluid flow channels formed by friction welding.

[0010] Furthermore, the connectors at the inlet and outlet of the coolant flow channel are externally insulated.

[0011] Furthermore, the cooling channel has a controlled temperature range of -40°C to room temperature, and the heating wire has a controlled temperature range of room temperature to 380°C.

[0012] This invention achieves the telescopic adjustment of the heat exchange platform through the threaded connection between the adjustment frame and the heat exchange platform. By setting a coolant flow channel and an electric heating wire on the heat exchange platform, the temperature range can be controlled from -40℃ to 380℃, which greatly increases the temperature adjustment range. Attached Figure Description

[0013] Figure 1 This is a simplified structural diagram of the integrated temperature-controlled stage kit for in-situ XRD testing in this invention.

[0014] Figure 2 The in-situ XRD test charge-discharge curves and in-situ XRD patterns of carbon cathode in zinc-air battery at -10℃ are shown.

[0015] Figure 3 The in-situ XRD test charge-discharge curves and in-situ XRD patterns of carbon cathode in zinc-air batteries at 50°C are shown.

[0016] 1. Adjustment frame; 2. Connecting part of the heat exchanger; 3. Loading part of the heat exchanger; 4. Heating resistance wire; 5. Thermocouple; 6. Heating wire connector; 7. Coolant connection port. Detailed Implementation

[0017] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments;

[0018] This invention specifically relates to a temperature-controlled stage for in-situ XRD, the core components of which include a ring-shaped lower adjustment frame and an integrated cylindrical heat exchange stage. The integrated cylindrical heat exchange stage is equipped with a liquid cooling path and a temperature-controlled electric heating component, making it easy to install and enabling uniform and precise temperature control of the reaction environment of the battery assembly.

[0019] A temperature-controlled stage kit for in-situ XRD testing includes a battery reaction stage and a matching temperature control kit. The battery reaction stage can be nested within the original X-ray diffractometer stage and is an integrated heat exchanger including an adjustment bracket, a liquid cooling path, and a temperature-controlled electric heating path. The lower adjustment bracket has threads on its inner wall and is rotatably connected to the heat exchanger; the height of the kit can be controlled by rotation to meet X-ray path requirements. The integrated cylindrical heat exchanger has a sample stage recess on its upper part for placing a conventional sample stage or an electric heating stage to be tested. A chemical testing sample stage; the integrated cylindrical heat exchanger stage has a liquid cooling passage, with a coolant inlet and outlet channel on the side wall, which are respectively connected to a compressor / refrigeration unit via pipelines; in the liquid cooling passage of the cylindrical heat exchanger stage, coolant flows in through the inlet channel and flows out through the outlet channel, forming a circulation loop to cool and control the temperature of the cylindrical heat exchanger stage, controlling the sample stage testing temperature between -40℃ and 25℃; the integrated cylindrical heat exchanger stage has a temperature-controlled electric heating component containing a heating wire connected to a thermoelectric generator. The thermocouple assembly forms a passageway; in the temperature control heating assembly of the cylindrical heat spreader, the working state of the heating wire is adjusted based on the temperature information measured by the thermocouple, thereby achieving precise temperature control of the heat spreader, which can be controlled between 25℃ and 380℃; the outer diameter of the lower adjustment bracket is consistent with the outer diameter of the sample stage of the in-situ XRD diffractometer, and it can be embedded in the X-ray diffractometer. The inner wall thread can be rotatably connected to the cylindrical heat spreader, and the height of the assembly is controlled by rotation; the integrated cylindrical heat spreader has a groove inside and a bolt joint on the outer wall. It is connected to the liquid cooling connector to achieve a sealed liquid cooling passage; the outer wall of the liquid cooling passage is fitted with thermal insulation material to prevent condensate from dripping into the XRD host cavity and causing equipment damage; the temperature control and heating assembly of the heat spreader includes a heating resistance wire and a thermocouple; the outer diameter of the integrated heat spreader is larger than the outer diameter of the lower adjustment bracket, and the shape and size of the groove on the upper surface are consistent with those of ordinary sample stages and electrochemical sample stages; except for the metal heat spreader assembly and the heating and temperature control assembly, the remaining structural components of the adjustment bracket and sample stage are made of insulating material.

[0020] See Figure 1The lower adjustment bracket has threads on its inner wall and is rotatably connected to the cylindrical heat exchanger platform. The height of the kit can be controlled by rotation. The integrated cylindrical heat exchanger platform has a circular groove on its upper part for placing the battery assembly to be tested. The integrated cylindrical heat exchanger platform has a liquid cooling passage with a coolant inlet channel and an outlet channel, which are respectively connected to a compressor refrigeration unit. The integrated cylindrical heat exchanger platform has a temperature-controlled electric heating assembly with an internal heating wire that connects to a thermocouple assembly to form a passage.

[0021] See Figure 1 The cylindrical heat spreader is connected to a liquid cooling channel. Coolant flows in through the inlet channel and flows out through the outlet channel, forming a circulation loop to cool and control the temperature of the cylindrical heat spreader, controlling the battery test temperature between -40℃ and 25℃. The temperature control heating component of the cylindrical heat spreader can adjust the working state of the heating wire according to the temperature information measured by the thermocouple, thereby achieving precise temperature control of the heat spreader, which can be controlled between 25℃ and 380℃.

[0022] The outer diameter of the lower adjustment bracket is consistent with the outer diameter of the sample stage of the in-situ XRD diffractometer, and can be embedded in the X-ray diffractometer. The inner wall has threads and can be rotatably connected to the cylindrical heat exchange stage. The height of the kit can be controlled by rotation.

[0023] An integrated heat exchange platform is located on the annular lower adjustment frame, with an outer diameter larger than that of the lower adjustment frame. It has an internal groove for embedding the battery assembly. It also includes two liquid cooling connectors located on the outer wall, with a heating resistance wire and a thermocouple in the groove on the upper surface.

[0024] In practical use, firstly, the annular lower adjustment frame is rotatably connected to the integrated heat exchanger. Next, the annular lower adjustment frame is placed on the XRD diffractometer, and the heat exchanger is adjusted to a suitable height by rotation. Then, the liquid cooling path and the temperature-controlled electric heating component are connected sequentially, and the required reaction temperature and heating rate are set to achieve temperature control of the cylindrical heat exchanger. Finally, the battery assembly is placed in the upper groove of the cylindrical heat exchanger to achieve temperature control during in-situ XRD testing.

[0025] Example 1;

[0026] In-situ XRD testing of a zinc-air battery using a carbon cathode at -35°C;

[0027] Carbon positive electrode and zinc sheet are used as working electrode and counter electrode, respectively, composite zinc salt is used as electrolyte, and commercial diaphragm is used.

[0028] First, rotate and connect the ring-shaped lower adjustment frame to the integrated heat exchange stage, and then place the ring-shaped lower adjustment frame on the XRD diffractometer.

[0029] Open the liquid cooling circuit of the compressor refrigeration unit and set the temperature parameter to -35℃ and the refrigerant flow rate;

[0030] Embed the battery assembly into the upper groove of the heat exchange platform;

[0031] When the compressor reading reaches the specified temperature, the charge / discharge procedure and XRD diffractometer are started to perform low-temperature in-situ XRD testing. The data results are shown below. Figure 2 .

[0032] Example 2;

[0033] In-situ XRD testing of pyrite-potassium copper ore during the heating process;

[0034] The powdered sample to be tested is placed into the sample cell and the surface is flattened.

[0035] First, rotate and connect the ring-shaped lower adjustment frame to the integrated heat exchange stage, and then place the ring-shaped lower adjustment frame on the XRD diffractometer.

[0036] Turn on the electric heating circuit and set the target temperature to 300℃ on the controller for 10 hours;

[0037] Embed the powder sample holder into the upper groove of the homogenization stage;

[0038] Set the scanning angle 2θ = 5–40°, scan continuously for 10 hours, and simultaneously start the heating circuit switch and scanning program. Data results are shown below. Figure 3 .

Claims

1. A temperature-controlled stage kit for in-situ XRD testing, characterized in that, The stage kit includes: an adjustment frame, a heat spreader, a heating wire, and a thermocouple. The heat spreader includes a connecting part and a loading part. The upper surface of the loading part has a groove for placing experimental objects. The bottom of the groove on the upper surface of the loading part is provided with a heating wire and a thermocouple, and the connection ports of the heating wire and the thermocouple are located on the side wall of the loading part. A coolant channel is provided inside the loading part near the upper surface, and the side wall of the loading part has an inlet and an outlet for the coolant channel. The connecting part is cylindrical and located on the lower surface of the loading part. The connecting part is connected to the adjustment frame by threads, and the heat spreader can be extended or retracted relative to the adjustment frame by rotation. The thermocouple is used to collect temperature data of the loading part.

2. The temperature-controlled stage kit for in-situ XRD testing as described in claim 1, characterized in that, The connecting part is a cylinder with external threads, and the adjusting bracket is an annular ring with internal threads, with the external and internal threads meshing with each other.

3. The temperature-controlled stage kit for in-situ XRD testing as described in claim 1, characterized in that, The heat exchange platform is made of metal, and the internal coolant flow channels are constructed through friction welding.

4. The temperature-controlled stage kit for in-situ XRD testing as described in claim 1, characterized in that, The connectors at the inlet and outlet of the coolant flow channel are externally insulated.

5. A temperature-controlled stage kit for in-situ XRD testing as described in claim 1, characterized in that, The temperature range of the coolant flow channel is -40℃ to room temperature, and the temperature range of the heating wire is room temperature to 380℃.

Images