High-temperature reaction tank and experimental device

Abstract

The invention relates to the technical field of experiments, and provides a high-temperature reaction tank and an experimental device, the high-temperature reaction tank comprises a base table, a supporting table which is arranged on the base table and is provided with a placing sheet for placing a sample, a laser heating unit which is positioned below the supporting table and is used for heating laser to face the sample, and a temperature measuring unit (the temperature measuring end faces or contacts with the sample). And the placing sheet is made of a transparent material which is resistant to high temperature and inert to the sample and does not react with the sample. Through organic combination of the high-temperature-resistant transparent placing piece, underneath laser rapid local heating and near-field accurate temperature measurement, non-contact and high-energy-density rapid heating and small-scale hot areas can be achieved, meanwhile, the thermal background and interference of a sample table and a heating body are reduced, the time resolution, the bulk phase characterization capacity and the data reliability of high-temperature in-situ XRD are remarkably improved, and the high-temperature in-situ XRD temperature measurement accuracy is improved. The method is suitable for in-situ research on high-temperature phase change, reaction kinetics, thermal stability and the like.

Description

Technical Field

[0001] This invention relates to the field of experimental technology, and in particular to a high-temperature reaction tank and experimental apparatus. Background Technology

[0002] High-temperature in-situ XRD (X-ray diffraction) experiments are of great significance for studying thermal stability, phase transformation mechanisms, sintering processes, and high-temperature chemical reactions.

[0003] Current mainstream high-temperature in-situ XRD platforms typically employ a monolithic heating chamber or sample stage based on radiation or resistance, achieving temperature control by heating the sample and its surrounding environment as a whole. However, their heating rate and response are relatively slow, making it difficult to capture rapid dynamic processes. Furthermore, monolithic heating causes the sample volume, sample stage, and environment to heat up together, potentially triggering unnecessary side reactions or interfacial interactions. Summary of the Invention

[0004] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a high-temperature reaction tank and experimental apparatus to improve experimental accuracy.

[0005] To achieve the above and other related objectives, the present invention provides a high-temperature reaction tank, comprising:

[0006] abutment; A support platform is disposed on the base, the support platform including a placement plate for placing a sample; A laser heating unit is disposed below the support platform, and the heating laser of the laser heating unit is directed toward the sample; A temperature measuring unit, wherein the temperature measuring end of the temperature measuring unit faces the sample or is used to contact the sample; The placement sheet is made of a high-temperature resistant transparent material and is configured not to react with the sample.

[0007] In a specific embodiment of the present invention, the placement piece is provided with a protrusion for placing the sample, and the upper end surface of the protrusion is the highest point of the support.

[0008] In a specific embodiment of the present invention, the support platform includes a placement platform and a sample tray. The placement platform is used to connect with the base. The placement platform is provided with a slot for inserting the sample tray. The placement piece is disposed on the sample tray. The placement platform and the sample tray have a hollow structure corresponding to the position of the placement piece.

[0009] In one specific embodiment of the present invention, the laser heating unit includes an optical fiber and a laser head, the laser head being connected to one end of a plurality of optical fibers, and the laser head being used to focus the light within the optical fibers.

[0010] In one specific embodiment of the present invention, the laser head passes through the base from bottom to top, and a cooling channel is provided inside the base.

[0011] In one specific embodiment of the present invention, a heat insulation pad is provided between the support platform and the base.

[0012] In a specific embodiment of the present invention, the temperature measuring unit includes a ceramic thermocouple, the ceramic thermocouple is arranged vertically along its length, and the ceramic thermocouple is configured such that its temperature measuring end can contact the sample in a molten state.

[0013] In one specific embodiment of the present invention, a support frame is connected to the base, a cantilever is connected to the support frame, and a ceramic thermocouple is disposed at the end of the cantilever away from the support frame. The ceramic thermocouple is assembled to be able to slide and lock in the vertical direction on the cantilever.

[0014] In a specific embodiment of the present invention, the ceramic thermocouple includes a ceramic tube and a thermocouple wire passing through the ceramic tube. A ceramic block is provided at the upper end of the support frame, and the ceramic block is used to fix the thermocouple wire led out from the upper end of the ceramic thermocouple.

[0015] The present invention also provides an experimental apparatus for X-ray diffraction experiments, comprising: Base; A sample stage is disposed on the base. The sample stage includes a high-temperature reaction tank and a support as described above. The high-temperature reaction tank is disposed on the support. An X-ray source, wherein the X-ray source is used to irradiate the sample; A detector used to detect the sample.

[0016] In one specific embodiment of the present invention, the support is configured to be able to translate and adjust the position of the high-temperature reaction tank in a first direction and a second direction, wherein the first direction is a vertical direction and the second direction is perpendicular to the first direction and the emission direction of the X-ray source.

[0017] In one specific embodiment of the present invention, the detector is disposed on the side of the sample stage away from the X-ray source, and the detector avoids the emission direction of the X-ray source.

[0018] The technical advantages of this invention are as follows: by organically combining a high-temperature resistant, transparent, and non-reactive placement plate located on the substrate, a laser heating unit positioned below the placement plate and facing the sample, and a temperature measuring unit facing or in contact with the sample, rapid, controllable, and localized heating and precise temperature monitoring are achieved, thereby significantly improving the temporal resolution and data reliability of high-temperature in-situ XRD. The under-mounted laser heating provides non-contact, high-energy-density rapid heating and a small-scale hot zone, reducing thermal background and sample stage interference caused by overall heating. Attached Figure Description

[0019] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0020] Figure 1 This is a three-dimensional structural diagram of a high-temperature reaction tank according to one embodiment of the present invention; Figure 2 This is a schematic diagram of the high-temperature reaction tank in one embodiment of the present invention from another perspective. Figure 3 This is a schematic diagram of the high-temperature reaction tank in one embodiment of the present invention from another perspective; Figure 4 This is a schematic diagram of the experimental apparatus according to one embodiment of the present invention; Figure 5 This is a schematic diagram of the sample stage of the experimental apparatus in one embodiment of the present invention; Explanation of reference numerals in the attached figures: 1. Sample; 2. Base; 3. Sample stage; 4. X-ray source; 5. Detector; 10. Base; 11. Cooling channel; 12. Stand; 13. Cantilever; 14. Ceramic block; 20. Support; 21. Placement plate; 22. Parking stage; 23. Sample holder; 30. Laser heating unit; 31. Optical fiber; 32. Laser head; 40. Temperature measuring unit. Detailed Implementation

[0021] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that, unless otherwise specified, the following embodiments and features described therein can be combined with each other.

[0022] It should be noted that the illustrations provided in the following embodiments are only schematic representations of the basic concept of the present invention. Therefore, the illustrations only show the components related to the present invention and are not drawn according to the actual number, shape and size of the components in the actual implementation. In the actual implementation, the form, quantity and proportion of each component can be arbitrarily changed, and its component layout may also be more complex.

[0023] X-ray diffraction (XRD) is a non-destructive structural analysis technique based on Bragg's law (2d sinθ = nλ). It is widely used to characterize the crystal structure, phase composition, lattice parameters, crystallinity, and microstrain of materials. By recording the angle and intensity distribution of the diffraction of incident X-rays with crystal planes, the ordered arrangement of atoms and phase evolution within the sample can be deduced. It is one of the fundamental methods in materials science, physics, and chemistry research.

[0024] To study the structural evolution of materials under non-equilibrium environments such as high temperature, low temperature, and high pressure, in-situ XRD technology has emerged. High-temperature in-situ XRD, in particular, is of great significance for studying thermal stability, phase transition mechanisms, sintering processes, and high-temperature chemical reactions. Current mainstream high-temperature in-situ XRD platforms typically employ a monolithic heating chamber or sample stage based on radiation or resistance, achieving temperature control by heating the sample and its surrounding environment as a whole. However, this traditional heating method has several inherent limitations: first, the heating rate and response are slow, making it difficult to capture rapid dynamic processes; second, monolithic heating causes the sample volume, sample stage, and environment to heat up together, potentially triggering unnecessary side reactions or interfacial interactions; and third, the heating element and chamber generate significant thermal radiation and background noise, increasing diffraction noise, reducing the signal-to-noise ratio, and affecting data quality and analytical accuracy.

[0025] In X-ray incident geometry design, grazing incidence geometry is widely used to enhance diffraction signals and suppress the background of the substrate or sample stage. Grazing incidence limits the X-ray penetration depth by using a very small incident angle, making it highly sensitive to thin film or surface structures, and therefore very effective in surface and thin film analysis. However, this method also has significant drawbacks: first, the detection depth is limited, making it difficult to reflect the bulk structure of the material; second, it requires extremely high surface smoothness and uniformity of the sample, as surface roughness or morphological undulations will significantly weaken the diffraction signal; and third, precisely controlling a small incident angle increases experimental complexity and limits the adaptability of sample morphology and mounting methods.

[0026] Laser heating, as a non-contact, high-energy-density heating method, provides rapid and localized temperature control, achieving heating rates of hundreds to thousands of degrees Celsius per second. It precisely confines the heat-affected zone to the micrometer to millimeter scale, thus avoiding side reactions and interactions with the support caused by overall heating. Laser heating also reduces cavity thermal noise and improves the temporal resolution and spatial selectivity of in-situ measurements. However, current research and applications combining laser heating with high-temperature in-situ XRD are still limited, and most existing methods involve grazing incidence geometry coupling, making them still biased towards surface / thin film analysis and unable to meet the needs for rapid and quantitative characterization of bulk materials under high-temperature conditions.

[0027] Therefore, in order to achieve high-speed and high-precision in-situ characterization of the bulk structure of materials, there is an urgent need for a new in-situ measurement scheme that combines the advantages of high energy density and rapid local heating of laser with horizontal / conventional incident XRD (to improve bulk penetration and representativeness) to simultaneously meet the requirements of time resolution, signal-to-noise ratio and bulk representativeness.

[0028] To solve the above technical problems, such as Figure 1-3 As shown, the present invention proposes a high-temperature reaction cell (not necessarily a pool-shaped structure, but specifically a flat plate, groove, or cavity that can hold sample 1), including a base 10, a support 20, a laser heating unit 30, and a temperature measuring unit 40.

[0029] The placement plate 21 on the stage 20 is made of a high-temperature resistant transparent material (such as a quartz plate), with a polished surface and chemical inertness to the sample 1. This provides mechanical support for the sample 1 while minimizing X-ray obstruction and scattering. The laser heating unit 30 emits a heating laser from below, which can directly act on the sample 1 through the quartz placement plate 21, achieving non-contact, localized heating. The temperature measuring end of the temperature measuring unit 40 faces or is in contact with the sample 1, allowing real-time acquisition of the sample 1's temperature information for accurate correlation between temperature and structural evolution. The overall structure isolates the laser heating from the sample 1 outside the high-temperature resistant transparent placement plate 21, protecting the sample 1 from direct contact with the heater while ensuring compatibility and ease of operation of the heating optical path and XRD detection geometry.

[0030] Bottom-mounted laser heating reduces the thermal background of the cavity and sample stage 3 caused by overall heating, shrinks the heat-affected zone, and lowers the probability of side reactions with the support. The high-temperature resistant, transparent, and polished placement plate 21 can withstand high temperatures while minimizing interference with the diffraction signal, improving the signal-to-noise ratio. The temperature measurement unit 40 provides real-time temperature feedback, which helps to precisely control the heating program and accurately determine the temperature-structure relationship. In summary, this reaction cell is beneficial for capturing rapid phase transitions, clarifying reaction kinetics, and obtaining more representative high-temperature XRD characterization results of the bulk phase.

[0031] In one specific embodiment of the present invention, such as Figure 1-3 As shown, the placement plate 21 is provided with a protrusion for placing the sample 1, and the upper end face of the protrusion is the highest point of the support 20. The sample 1 is dispersed in powder form in a volatile solvent (such as alcohol) and dropped onto the top of the protrusion. After the solvent evaporates, the sample 1 powder remains at the highest point of the protrusion. The X-ray source 4 emits X-rays in a direction parallel to the placement plate 21, so that the X-rays irradiate the highest point of the sample 1 along a path parallel to the plate surface, avoiding obstruction by the edge of the placement plate 21 or the structure of the support 20 or causing unnecessary scattering, thereby ensuring the geometric and thermal coordination of heating, temperature measurement and XRD detection.

[0032] In one specific embodiment of the present invention, such as Figure 1-3 As shown, the support platform 20 consists of a placement platform 22 and a pluggable sample holder 23. The placement platform 22 is fixed to the base 10 and has a slot for inserting the sample holder 23. The sample holder 23 can slide into the slot and be positioned and fixed. The placement piece 21 is installed on the sample holder 23. To avoid the base structure from obstructing or affecting the heat conduction of the laser heating unit 30, both the placement platform 22 and the sample holder 23 are designed with a hollow structure at the corresponding positions of the placement piece 21, that is, an opening or through hole is left below the placement piece 21 so that the laser emitted by the lower laser heating unit 30 can reach the sample 1 area without obstruction. This structure realizes a modular and repositionable sample 1 installation method. The sample holder 23 can be quickly inserted and removed for easy replacement and cleaning. The slot positioning ensures the consistency and mechanical stability of the sample 1 in terms of horizontal plane and height, improving experimental repeatability.

[0033] In one specific embodiment of the present invention, such as Figure 1-3As shown, the laser heating unit 30 consists of multiple optical fibers 31 and a laser head 32 connected to them. One end of each optical fiber 31 converges to the laser head 32. The laser head 32 has a built-in optical focusing mechanism (lens group or microlens array) to combine and focus the beams from each optical fiber 31 into the desired heating spot. The laser source is spatially isolated from the temperature measurement / sample 1 area through the transmission of light through the optical fibers 31, allowing for flexible wiring. The emitting end of the laser head 32 is equipped with a sapphire plate as a protective window. The sapphire plate is transparent, heat-resistant, wear-resistant, and chemically corrosion-resistant. It can be placed at the light outlet to isolate the internal optical components of the laser head 32 from the high-temperature molten splashes or particles in the sample 1 area. The sapphire window can be designed to be replaceable or used with a cooling structure and a reflection / sealing structure to maintain optical alignment and atmosphere isolation. The configuration of optical fiber 31 + focusing laser head 32 ensures both high power transmission and flexible arrangement, while also enabling localized heating of a small size with high energy density, which is beneficial for rapid and controllable heating of sample 1 and in-situ observation with high temporal resolution. The sapphire protective window effectively prevents damage to the internal optical components of the laser head 32 from high-temperature molten material or particle impact, reduces contamination and facilitates maintenance, extends the service life of the laser head 32, reduces the frequency of downtime maintenance, and its excellent optical transmittance and thermal stability can maintain the quality of the emitted beam and heating stability. At the same time, it is easy to seal and cool in a controlled atmosphere or vacuum environment, which improves the overall reliability, repeatability and experimental safety of the laser heating unit 30, and is conducive to the long-term stable conduct of high-temperature in-situ XRD experiments.

[0034] In one specific embodiment of the present invention, such as Figure 2 As shown, the laser head 32 passes through the base 10 from bottom to top. A cooling channel 11 is arranged inside the base 10, and inlet and outlet ports for coolant are provided on the base 10. Quick-release water pipe connectors are used for quick connection or disconnection with a water chiller or cooling circuit. The cooling channel 11 is positioned around or near the laser head 32 cylinder and the optical window at the light-emitting end located on the base 10, to efficiently remove the heat generated by the laser head 32 passing through the base 10, as well as the heat accumulated in the base 10 body due to laser irradiation or environmental heat load. The design of the inlet / outlet ports and quick-release connectors facilitates the assembly, maintenance, and replacement of the cooling circuit, and can be combined with sealing components and leakage detection measures to improve the maintainability and safety of the system. The water-cooling cycle of the stage 10 can effectively control the temperature of the laser head 32 and the stage 10, reduce the thermal expansion and contraction and thermal drift of optical components and mechanical supports, maintain the stability of the optical path and mechanical positioning, extend the service life of the laser head 32 and protective windows (such as sapphire sheets), and at the same time prevent the stage 10 from overheating and conducting to the sample 1 area to reduce the thermal background and noise of the XRD signal.

[0035] In one specific embodiment of the present invention, a heat insulation pad is provided between the support 20 and the base 10. The heat insulation pad is made of a high-temperature resistant material with low thermal conductivity (such as quartz, ceramic, etc.) and is processed into a suitable size and shape according to structural requirements to match the contact surfaces of the support 20 and the base 10. The heat insulation pad is placed between the two to form a thermal resistance. The heat insulation pad can significantly reduce the conduction of heat from the support 20 to the base 10, reduce the heat load and temperature rise of the base 10 and its internal cooling system, thereby protecting the optical and cooling components on the base 10, reducing thermal drift, and extending the equipment life. At the same time, it reduces background thermal radiation and diffraction noise caused by carrier heating, improving the signal-to-noise ratio and temperature control accuracy of XRD data.

[0036] In one specific embodiment of the present invention, such as Figure 3 As shown, the temperature measuring unit 40 employs a ceramic thermocouple, arranged vertically so that its measuring end can directly contact the sample 1 in a molten or flowing glassy state. The ceramic thermocouple itself is heat-resistant and chemically inert. Its vertical structure allows for precise near-field temperature measurement on conventional solid samples 1, and also enables insertion into or contact with the surface of sample 1 when it is molten or flowing. When sample 1 is in a molten or viscous flow state under laser localized heating, the interaction between the thermocouple and the liquid surface (e.g., surface tension, wetting effect) causes sample 1 to be drawn or concentrated around the thermocouple, thereby expanding the crystalline region of sample 1. Horizontally incident X-rays diffract through sample 1, better detecting bulk crystal changes.

[0037] In one specific embodiment of the present invention, a support frame 12 is provided on the base 10, and a cantilever 13 is connected to the support frame 12. A ceramic thermocouple is installed at the end of the cantilever 13 away from the support frame 12, and the thermocouple can slide vertically along the cantilever 13 and be fixed by screws. This structure allows the thermocouple to be finely positioned vertically to accommodate samples 1 of different heights or shapes (e.g., differences in boss height or thickness of sample 1 after deposition). After being adjusted to a suitable height, it is locked with screws to ensure the mechanical positioning stability of the temperature measuring end. The distal end of the cantilever 13 is arranged so that the temperature measuring end of the thermocouple is relatively far from the support frame 12, thereby facilitating the placement of the temperature measuring end at the highest point of sample 1 or a designated detection position, and allowing for quick up-and-down movement or retraction without disassembling the entire support 20 for cleaning, replacement, or to avoid mechanical interference with sample 1.

[0038] In a specific embodiment of the present invention, the ceramic thermocouple consists of a ceramic cylindrical tube with an outer diameter of approximately 1 mm and two thermocouple wires passing through the ceramic tube. Two inner holes with a diameter of approximately 0.3 mm are machined inside the ceramic tube for inserting the two thermocouple wires, including type K and type B, which can be selected according to the temperature measurement range. After exiting the tube end, the two thermocouple wires are welded at the same position to form a single-point temperature-sensing junction (temperature-sensing point), located at the lower end of the ceramic tube for contact with sample 1. A ceramic block 14 is provided at the upper end of the support 12 to fix and bind the thermocouple wires leading from the upper end of the ceramic tube, thereby effectively preventing the wires from flowing when sample 1 is in a molten state. This lifting action facilitates bulk phase detection. The entire assembly is made of ceramic material to balance high temperature resistance, chemical inertness, and electrical insulation, and its size and arrangement are compatible with the aforementioned sliding and locking structure of the cantilever 13.

[0039] like Figure 4 As shown, the present invention also provides an experimental apparatus for X-ray diffraction experiments, including a base 2, a sample stage 3, an X-ray source 4, and a detector 5.

[0040] The base 2 not only serves as a mechanical support and positioning plane, but is also designed with tilting freedom to adjust the relative angle of the sample stage 3. The sample stage 3 is mounted on the base 2, such as... Figure 5 As shown, the sample stage 3, supported by a bracket, carries the high-temperature reaction cell. It can operate directly in the atmosphere to study the reaction process with air, or the high-temperature reaction cell can be placed in a sealed vacuum chamber and the atmosphere can be controlled through the inlet and outlet ports. The vacuum chamber can be connected to online analytical instruments such as mass spectrometers (MS) for real-time monitoring of gas components and products before and after the reaction. The X-ray source 4 adopts a liquid metal target design, providing an incident light spot with a diameter of approximately 200 μm and achieving focusing of a light spot of approximately 200 μm. The photon transmission efficiency is better than 85%, and the X-ray source 4 is in a fixed position. The axis of the circular base 2 is on the same plane as the X-ray source 4 to facilitate geometric correction and stable alignment. The detector 5 is used to receive the scattered or diffracted signals from the sample 1. It can be arranged at different angles and distances according to experimental needs to meet diffraction measurement requirements. The detector 5 includes a two-dimensional area array, a linear array (1D) detector 5, a point counter, a storage fluorescent plate, and a semiconductor energy spectrum detector 5 (Si / Ge, etc.).

[0041] In one specific embodiment of the present invention, the bracket can be positioned in a first direction (vertical, ... Figure 4 (Z-direction) and second direction ( Figure 4The X-axis (perpendicular to the Z-axis and perpendicular to the X-ray emission direction Y) is used for translational adjustment to precisely position the high-temperature reaction cell relative to the fixed X-ray source 4 in the X–Z plane. By vertical and horizontal translation within the X–Z plane, the incident X-rays can be grazed onto the surface of sample 1 for surface structure analysis, while maintaining a fixed distance between sample 1 and X-ray source 4 in the Y-axis, thus avoiding changes to the optical path geometry. During actual alignment, the light source irradiation position can be initially determined using YaG fluorescence (YAG fluorescent labeling) and the support position can be coarsely adjusted. Then, XRD diffraction data can be collected and fine-tuned through diffraction signal intensity / morphology evaluation to achieve precise alignment. Since adjustment is only performed in the X–Z plane, operation is simple and compatible with the established geometric relationship of the light source / detector 5. In a specific embodiment of the invention, the detector 5 is positioned on the side of the sample stage 3 away from the X-ray source 4, avoiding the emission path and extension line of the X-ray source 4. Specific mechanisms for achieving translational adjustment can include lead screws and nuts, linear guide slides, linear motors, gear racks, hydraulic drive structures, pneumatic drive structures, etc.

[0042] In summary, this invention achieves non-contact, localized, and high-energy-density rapid heating through the combination of a lower-mounted optical fiber 31 focusing laser head 32 and a high-temperature resistant transparent polished placement plate 21. Simultaneously, it isolates the heating optical path from the sample 1 to reduce mechanical / chemical interference and minimize the thermal background of the cavity and carrier. Thermal management and protection measures such as the cooling channel 11 of the base 10, the sapphire protective window, and the heat insulation pad effectively control thermal drift, protect optical components, extend equipment life, and improve heating stability and maintainability. The pluggable sample holder 23 and slot-type positioning enable modular, repeatable sample 1 installation and rapid replacement. Combined with the slidable and lockable vertical ceramic thermocouple of the cantilever 13 and its ceramic tube / block 14 fixing structure, it provides fast-response, low-heat-capacity, and positionally stable near-field temperature measurement. It can obtain representative temperatures in molten or flowing states and expand the crystallization region through the liquid surface tension effect to enhance the bulk diffraction signal. The support can be precisely translated in the XZ plane, and the base 2 has tilting degrees of freedom. Combined with the YAG fluorescence coarse alignment and diffraction signal fine alignment process, grazing incidence or transmission geometry can be adjusted without changing the source-sample 1 distance, accommodating both surface and bulk structure analysis while ensuring geometric repeatability. The fixed, high-efficiency (>85%) liquid metal target small-spot X-ray source 4, configured with optional high-speed two-dimensional / linear array / energy dispersive X-ray detectors 5, improves spatial and temporal resolution, signal-to-noise ratio, and data representativeness, and facilitates in-situ high-temperature reaction kinetics studies in atmospheric or controlled atmospheres (with online mass spectrometry monitoring). Overall, this invention achieves high stability, high sensitivity, and high repeatability in-situ XRD characterization capabilities in terms of thermal, optical, mechanical positioning, and temperature measurement coupling, significantly enhancing the ability to capture rapid phase transitions, resolve reaction kinetics, and obtain reliable bulk / surface structure information.

[0043] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

[0044] Throughout this description, numerous specific details, such as examples of components and / or methods, are provided to provide a complete understanding of embodiments of the invention. However, those skilled in the art will recognize that embodiments of the invention may be practiced without one or more of these specific details or by other devices, systems, components, methods, parts, materials, components, etc. In other instances, well-known structures, materials, or operations have not been specifically shown or described in detail to avoid obscuring aspects of embodiments of the invention.

Claims

1. A high temperature reaction cell characterized by, include: abutment; A support platform is disposed on the base, the support platform including a placement plate for placing a sample; A laser heating unit is disposed below the support platform, and the heating laser of the laser heating unit is directed toward the sample; A temperature measuring unit, wherein the temperature measuring end of the temperature measuring unit faces the sample or is used to contact the sample; The placement sheet is made of a high-temperature resistant transparent material and is configured not to react with the sample.

2. The high-temperature reaction tank according to claim 1, characterized in that, The placement plate is provided with a protrusion for placing the sample, and the upper end face of the protrusion is the highest point of the support.

3. The high-temperature reaction tank according to claim 1, characterized in that, The support platform includes a placement platform and a sample holder. The placement platform is used to connect to the base. The placement platform is provided with a slot for inserting the sample holder. The placement piece is disposed on the sample holder. The placement platform and the sample holder have a hollow structure corresponding to the position of the placement piece.

4. The high-temperature reaction tank according to claim 1, characterized in that, The laser heating unit includes optical fibers and a laser head. The laser head is connected to one end of multiple optical fibers and is used to focus the light within the optical fibers.

5. The high-temperature reaction tank according to claim 4, characterized in that, The laser head passes through the base from bottom to top, and the base is provided with cooling channels.

6. The high-temperature reaction tank according to claim 4, characterized in that, A heat insulation pad is provided between the support platform and the base.

7. The high-temperature reaction tank according to claim 1, characterized in that, The temperature measuring unit includes a ceramic thermocouple, which is arranged vertically along its length, and the ceramic thermocouple is configured such that its temperature measuring end can contact the sample in a molten state.

8. The high-temperature reaction tank according to claim 7, characterized in that, A support frame is connected to the base, and a cantilever is connected to the support frame. The ceramic thermocouple is disposed at the end of the cantilever away from the support frame, and the ceramic thermocouple is assembled to be able to slide and lock in the vertical direction on the cantilever.

9. The high-temperature reaction tank according to claim 8, characterized in that, The ceramic thermocouple includes a ceramic tube and a thermocouple wire passing through the ceramic tube. A ceramic block is provided at the upper end of the stand, and the ceramic block is used to fix the thermocouple wire leading out from the upper end of the ceramic thermocouple.

10. An experimental apparatus, characterized in that, Applied to X-ray diffraction experiments, including: Base; A sample stage is disposed on the base, the sample stage including a high-temperature reaction tank and a support as described in any one of claims 1-9, the high-temperature reaction tank being disposed on the support; An X-ray source, wherein the X-ray source is used to irradiate the sample; A detector used to detect the sample.

11. The experimental apparatus according to claim 10, characterized in that, The support is configured to be able to translate and adjust the position of the high-temperature reaction tank in a first direction and a second direction, wherein the first direction is vertical and the second direction is perpendicular to the first direction and the emission direction of the X-ray source.

12. The experimental apparatus according to claim 10, characterized in that, The detector is positioned on the side of the sample stage away from the X-ray source, and the detector avoids the emission path of the X-ray source and its extension line.

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