CN-121994841-A - 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 device comprises a base, a tray which is arranged on the base and is provided with a placing piece for placing a sample, and a laser heating unit and a temperature measuring unit (a temperature measuring end faces or contacts the sample) which are positioned below the tray and heat laser to face the sample. The placing plate is made of transparent materials which are resistant to high temperature and inert to the sample, and does not react with the sample. Through the organic combination of high-temperature-resistant transparent placing sheet, underlying laser rapid local heating and near-field accurate temperature measurement, the rapid temperature rise and small-scale hot zone with non-contact and high energy density can be realized, meanwhile, the thermal background and interference of a sample table and a heating body are reduced, the time resolution, the bulk phase characterization capability and the data reliability of high-temperature in-situ XRD are obviously improved, and the method is suitable for in-situ research of high-temperature phase transformation, reaction dynamics, thermal stability and the like.

Inventors

• WANG ZHUJUN
• ANG CHAO

Assignees

• 上海科技大学

Dates

Publication Date

20260508

Application Date

20260211

Claims (12)

1. 1. A high temperature reaction cell, comprising: A base station; A support stand, which is arranged on the base stand and comprises a placing piece for placing a sample; a laser heating unit arranged below the supporting table, wherein heating laser of the laser heating unit faces the sample; the temperature measuring end of the temperature measuring unit faces the sample or is used for contacting with the sample; Wherein the placing plate is made of a high temperature resistant transparent material, and the placing plate is configured not to react with the sample.
2. 2. The high temperature reaction cell according to claim 1, wherein a boss for placing the sample is provided on the placing plate, and an upper end surface of the boss is a highest point of the tray table.
3. 3. The high-temperature reaction tank of claim 1, wherein the supporting platform comprises a parking platform and a sample support, the parking platform is used for being connected with the base platform, a clamping groove for the sample support to be inserted is formed in the parking platform, the placing sheet is arranged on the sample support, and the parking platform and the sample support are hollow structures corresponding to the placing sheet.
4. 4. The high temperature reaction cell of claim 1, wherein the laser heating unit comprises an optical fiber and a laser head, the laser head being connected to one end of a plurality of the optical fibers, the laser head being configured to focus light within the optical fibers.
5. 5. The high temperature reaction cell of claim 4, wherein the laser head passes through the base from bottom to top, and a cooling flow channel is arranged in the base.
6. 6. The high temperature reaction cell of claim 4, wherein a heat insulating pad is disposed between the pallet and the base.
7. 7. The high temperature reaction cell according to claim 1, wherein the temperature measuring unit comprises a ceramic thermocouple, a length direction of the ceramic thermocouple being arranged in a vertical direction, the ceramic thermocouple being configured such that a temperature measuring end thereof can be brought into contact with the sample in a molten state.
8. 8. The high temperature reaction cell according to claim 7, wherein a stand is connected to the base, a cantilever is connected to the stand, the ceramic thermocouple is provided at an end of the cantilever away from the stand, and the ceramic thermocouple is assembled to be slidable and lockable in a vertical direction on the cantilever.
9. 9. The high-temperature reaction tank according to claim 8, wherein the ceramic thermocouple comprises a ceramic tube and a thermocouple wire passing through the ceramic tube, a ceramic block is arranged at the upper end of the stand, and the ceramic block is used for fixing the thermocouple wire led out from the upper end of the ceramic thermocouple.
10. 10. An experimental set-up, characterized in that it is applied to X-ray diffraction experiments, comprising: A base; A sample stage arranged on the base, wherein the sample stage comprises the high-temperature reaction tank and a bracket according to any one of claims 1-9, and the high-temperature reaction tank is arranged on the bracket; an X-ray source for illuminating the sample; and a detector for detecting the sample.
11. 11. The experimental set-up of claim 10, wherein the support is configured to be translatable to adjust the position of the high temperature reaction cell in a first direction and a second direction, the first direction being a vertical direction, the second direction being perpendicular to the first direction and the emission direction of the X-ray source.
12. 12. The apparatus of claim 10, wherein the detector is disposed on a side of the sample stage remote from the X-ray source, the detector avoiding an emission path of the X-ray source and an extension thereof.

Description

High-temperature reaction tank and experimental device Technical Field The invention relates to the technical field of experiments, in particular to a high-temperature reaction tank and an experimental device. Background The high-temperature in-situ XRD (X-ray diffraction) experiment has important significance for researching thermal stability, phase change mechanism, sintering process, high-temperature chemical reaction and the like. The current mainstream high temperature in situ XRD platform generally employs an integral heating cavity or sample stage based on radiation or resistance to achieve temperature control by integral heating of the sample and surrounding environment. However, the heating rate and response are slow, and it is difficult to capture a fast dynamic process, and at the same time, the overall heating causes the sample volume to rise in temperature together with the sample stage and the environment, possibly causing unnecessary side reactions or interfacial interactions. Disclosure of Invention In view of the above drawbacks of the prior art, an objective of the present invention is to provide a high temperature reaction tank and an experimental apparatus for improving experimental accuracy. To achieve the above and other related objects, the present invention provides a high temperature reaction tank, comprising: A base station; A support stand, which is arranged on the base stand and comprises a placing piece for placing a sample; a laser heating unit arranged below the supporting table, wherein heating laser of the laser heating unit faces the sample; the temperature measuring end of the temperature measuring unit faces the sample or is used for contacting with the sample; Wherein the placing plate is made of a high temperature resistant transparent material, and the placing plate is configured not to react with the sample. In a specific embodiment of the present invention, a boss for placing the sample is disposed on the placing plate, and an upper end surface of the boss is a highest point of the tray. In a specific embodiment of the invention, the supporting platform comprises a parking platform and a sample support, the parking platform is used for being connected with the base platform, a clamping groove for the sample support to be inserted is formed in the parking platform, the placing sheet is arranged on the sample support, and the positions, corresponding to the placing sheet, on the parking platform and the sample support are hollow structures. In a specific embodiment of the present invention, the laser heating unit includes an optical fiber and a laser head, the laser head is connected to one ends of a plurality of the optical fibers, and the laser head is used for focusing the light rays in the optical fibers. In a specific embodiment of the invention, the laser head passes through the base station from bottom to top, and a cooling flow channel is arranged in the base station. In one embodiment of the present invention, a heat insulation pad is disposed between the pallet and the base. In a specific embodiment of the present invention, the temperature measuring unit includes a ceramic thermocouple, a length direction of which is arranged in a vertical direction, the ceramic thermocouple being configured such that a temperature measuring end thereof can be brought into contact with the sample in a molten state. In a specific embodiment of the present invention, a stand is connected to the base, a cantilever is connected to the stand, the ceramic thermocouple is disposed at an end of the cantilever away from the stand, and the ceramic thermocouple is mounted to be slidable and lockable in a vertical direction on the cantilever. In a specific embodiment of the invention, the ceramic thermocouple comprises a ceramic tube and a thermocouple wire passing through the ceramic tube, wherein a ceramic block is arranged at the upper end of the stand and is used for fixing the thermocouple wire led out from the upper end of the ceramic thermocouple. The invention also provides an experimental device, which is applied to an X-ray diffraction experiment and comprises the following components: A base; The sample stage is arranged on the base and comprises a high-temperature reaction tank and a bracket, wherein the high-temperature reaction tank is arranged on the bracket; an X-ray source for illuminating the sample; and a detector for detecting the sample. In a specific embodiment of the invention, the support is configured to be able to translationally adjust the position of the high temperature reaction cell in a first direction and a second direction, the first direction being a vertical direction, the second direction being perpendicular to the first direction and the emission direction of the X-ray source. In a specific embodiment of the present invention, the detector is disposed on a side of the sample stage away from the X-ray source, and the detector avoids the emission direc