In-situ measurement device for photothermal material structure and real-time temperature changes

Abstract

This invention discloses an in-situ measurement device for the structure and real-time temperature changes of photothermal materials, comprising: a transient spectrometer, an ATR accessory, a sample cell, an irradiation source, and a transparent pressure column. The ATR accessory includes: an ATR crystal, a first mirror group, and a second mirror group. The sample cell is positioned above the ATR crystal, with a first through-hole formed at the bottom. The top surface of the ATR crystal does not contact the bottom surface of the sample cell. A cover is fixed outside the sample cell. A resistance wire is installed inside the cover. The pressure column is vertically positioned, and its bottom is movable in the vertical direction. A second through-hole is formed on the top surface of the cover, and the bottom of the pressure column extends into the cover through the second through-hole. A first thermocouple is installed at the bottom of the pressure column, and a second thermocouple is installed inside the cover. This in-situ measurement device has a wide range of applications, enabling real-time, in-situ synchronous acquisition of the sample's structure and temperature during light or heat stimulation.

Description

Technical Field

[0001] This utility model belongs to the field of experimental instrument design technology, specifically relating to an in-situ measurement device for the structure of photothermal materials and real-time temperature changes. Background Technology

[0002] In the research and application of photothermal materials, in-depth exploration of their structural characteristics and temperature variation under irradiation conditions is of paramount importance. A strong spatiotemporal coupling effect exists between the microstructural restructuring and macroscopic thermodynamic response of photothermal materials, a characteristic that directly determines their application efficiency in photothermal conversion, photothermal storage, and photothermal catalysis. However, existing research and analytical methods have many significant limitations in addressing the detection needs of photothermal materials.

[0003] In structural analysis, currently widely used offline analysis techniques, such as X-ray diffraction (XRD), transmission electron microscopy (TEM), and infrared spectroscopy (IR), are limited by their operational procedures, which dictate that material sampling and processing can only be performed after the irradiation process. This results in researchers only being able to obtain static structural information of the material in specific states before and after irradiation, but being unable to capture the dynamic changes in the material's structure during irradiation. Consequently, it is difficult to establish an accurate and continuous correlation mechanism between structural evolution and real-time photothermal processes.

[0004] In temperature measurement, common methods include using thermocouples and infrared thermometers. While thermocouples can provide relatively accurate temperature values, they typically only measure the temperature of specific local points within the material, making it difficult to reflect the overall temperature gradient distribution and its trend over time during irradiation. Infrared thermometers, on the other hand, are susceptible to interference from environmental factors and optical penetration depth (usually <10μm), failing to capture the true internal temperature field of the material, and also exhibiting limitations in measurement accuracy and spatial resolution.

[0005] More critically, existing structural detection and temperature measurement systems operate independently, with hardware synchronization accuracy >100ms, while key responses in photothermal materials often occur within 50ms (such as the synergistic effect of lattice expansion and temperature rise in perovskite materials). This temporal mismatch renders cross-scale correlation analysis ineffective, making it difficult to establish quantitative models of photo-thermal-structure coupling. This significantly hinders a deeper understanding of the mechanisms of photothermal materials.

[0006] Given the aforementioned research challenges, there is an urgent need for an innovative measurement device that can accurately measure and analyze the structural changes and real-time temperature changes of photothermal materials in situ and synchronously during the irradiation process. Summary of the Invention

[0007] To address the shortcomings of the aforementioned technologies, the purpose of this invention is to provide an in-situ measurement device for the structure and real-time temperature changes of photothermal materials.

[0008] The objective of this utility model is achieved through the following technical solution.

[0009] An in-situ measurement device for the structure and real-time temperature change of photothermal materials includes: a transient spectrometer, an ATR accessory, a sample cell, an irradiation source, and a transparent pressure column. The ATR accessory includes: an ATR crystal, a first mirror group, and a second mirror group. The sample cell is positioned above the ATR crystal, and a first through-hole is formed at the bottom of the sample cell. The top surface of the ATR crystal does not contact the bottom surface of the sample cell. Parallel light emitted by the light source of the transient spectrometer undergoes total internal reflection within the ATR crystal and is emitted from the ATR crystal to form a first optical path. The second mirror group is used to reflect the first optical path to the detector of the transient spectrometer.

[0010] A cover is fixed to the outside of the sample cell to seal and keep the sample cell warm;

[0011] Multiple resistance wires are installed inside the enclosure.

[0012] The pressure column is vertically arranged, and the bottom of the pressure column can move in the vertical direction. A second through hole is formed on the top surface of the cover. The bottom of the pressure column extends into the cover through the second through hole. A first thermocouple is installed at the bottom of the pressure column.

[0013] Multiple second thermocouples are installed inside the enclosure, and the irradiation source is located directly above the sample cell so that the light from the irradiation source passes through the pressure column to irradiate the sample in the sample cell.

[0014] In the above technical solutions, the transient spectrometer is an ultraviolet transient spectrometer, an infrared transient spectrometer, or an ultraviolet-visible-infrared transient spectrometer.

[0015] In the above technical solution, the size of the first through hole is less than or equal to the size of the ATR crystal.

[0016] In the above technical solution, the cover is a rectangular cavity with an opening formed on the bottom surface of the cavity, and the ATR crystal is embedded in the opening.

[0017] In the above technical solution, the irradiation source is a single-band light source, a dual-band light source, or a multi-band light source.

[0018] In the above technical solution, an air inlet and an air outlet are formed on the cover.

[0019] In the above technical solution, the irradiation light source is vertically irradiated onto the sample cell.

[0020] In the above technical solution, the pressure column is made of glass.

[0021] In the above technical solution, the distance between the top surface of the ATR crystal and the bottom surface of the sample cell is no greater than 0.01 mm.

[0022] In the above technical solution, a sample is placed in the sample cell. When the sample is in a liquid state, the sample maintains a constant liquid level in the sample cell based on capillary action.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] 1. The photothermal material structure and the in-situ measurement device for real-time temperature change of this utility model have a wide range of applications. It can realize photo-stimulation or thermal stimulation of samples in different forms such as bulk materials, film materials, powders, and solutions. During the photo-stimulation or thermal stimulation process, the structure and temperature of the sample can be obtained in real time and in situ.

[0025] 2. The atmosphere inside the enclosure is controllable, providing test results under different atmospheric conditions (such as various gas atmospheres, vacuum environments, etc.), which provides strong support for the comprehensive research and application development of photothermal materials. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the in-situ measurement device for the structure of photothermal materials and real-time temperature changes.

[0027] Figure 2 This is a side view (partial) of the in-situ measurement device for the structure of photothermal materials and real-time temperature changes.

[0028] Figure 3 This is a top view (partial view) of the in-situ measurement device for the structure of photothermal materials and real-time temperature changes.

[0029] Wherein, 1: light source, 2: first reflector group, 3: second reflector group, 4: detector, 5: irradiation light source, 6: first thermocouple, 7: air inlet, 8: air outlet, 9: pressure column, 10: cover, 11: sample cell, 11-1: first through hole, 12: resistance wire, 13: second thermocouple, 14: ATR crystal. Detailed Implementation

[0030] The following description, in conjunction with the accompanying drawings, details the structure of the photothermal material and the in-situ measurement device for real-time temperature changes of this utility model.

[0031] Example 1

[0032] As attached Figures 1-3As shown, an in-situ measurement device for the structure and real-time temperature change of a photothermal material includes: a transient spectrometer, an ATR accessory, a sample cell 11, an irradiation source 5, and a transparent pressure column 9. The transient spectrometer is an ultraviolet transient spectrometer, an infrared transient spectrometer, or an ultraviolet-visible-infrared transient spectrometer.

[0033] The ATR accessory includes: an ATR crystal 14, a first reflector group 2, and a second reflector group 3. Both the first reflector group 2 and the second reflector group 3 are plane mirrors. A sample cell 11 is positioned above the ATR crystal 14, and the sample cell 11 and the ATR accessory are detachable. A sample, which is a photothermal material, is placed inside the sample cell 11. A first through-hole 11-1 is formed at the bottom of the sample cell 11 (the size of the first through-hole 11-1 is less than or equal to the size of the ATR crystal 14). The top surface of the ATR crystal 14 does not contact the bottom surface of the sample cell 11 (the distance between the top surface of the ATR crystal 14 and the bottom surface of the sample cell 11 is kept as small as possible, for example, 0.001 mm). When the sample is liquid, the sample maintains a constant liquid level in the sample cell due to capillary action. Parallel light emitted by the light source 1 of the transient spectrometer undergoes total internal reflection within the ATR crystal 14 and is emitted from the ATR crystal 14 to form a first light path. The second reflector group 3 is used to reflect the first light path to the detector 4 of the transient spectrometer.

[0034] A cover 10 is fixedly mounted outside the sample cell 11. The cover 10 is a rectangular cavity with an air inlet 7 and an air outlet 8 (both of which are pipes leading into the cover 10) formed on it. The atmosphere for sample testing can be controlled through the air inlet 7 and the air outlet 8. An opening is formed on the bottom surface of the cavity, and an ATR crystal 14 is embedded in the opening. The cover 10 is used to seal and insulate the sample cell 11.

[0035] Multiple resistance wires 12 are installed inside the cover 10;

[0036] The lower pressure column 9 is telescopic, belonging to a telescopic rod structure that can be extended and shortened. The lower pressure column 9 is vertically set, and its bottom can move in the vertical direction. A second through hole is formed on the top surface of the cover 10. The bottom of the lower pressure column 9 extends into the cover 10 through the second through hole. A first thermocouple 6 is installed at the bottom of the lower pressure column 9. There is no gap between the second through hole and the lower pressure column 9, ensuring the sealing and stability of the entire cover 10.

[0037] Four second thermocouples 13 are installed inside the enclosure 10.

[0038] The irradiation source 5 is located directly above the sample cell 11 so that the light from the irradiation source 5 passes through the pressure column 9 and irradiates the sample in the sample cell 11 perpendicularly. The irradiation source 5 is a single-band, dual-band, or multi-band light source. The size of the light spot of the irradiation source 5 is the same as the size of the cross-section of the sample in the sample cell 11 (the light spot just covers the sample, with an error within ±0.1mm).

[0039] The sample in sample cell 11 is in direct contact with the ATR crystal 14. The purpose of providing the first through hole 11-1 is to ensure good contact between the ATR crystal 14 and the sample. The sample can be in solid or liquid form. If the sample is in solid form, the pressure column 9 is used to press the sample down to ensure close contact between the sample and the ATR crystal 14. If the sample is in liquid form, close contact is not required; simply immerse the first thermocouple 6 at the bottom of the pressure column 9 into the liquid.

[0040] The transient spectrometer provides a basic testing environment for detecting changes in sample structure, and the ATR accessory can be detachably connected to the transient spectrometer.

[0041] The method of using the above-mentioned in-situ measurement device for the structure of photothermal materials and real-time temperature changes includes:

[0042] Step 1, taking the sample as a solid as an example, the sample is placed into the sample cell 11 and the sample is compacted by the pressure column 9 so that the lower surface of the sample can make good contact with the ATR crystal 14, while the upper surface of the sample is in close contact with the first thermocouple 6 to ensure the effective transmission of heat and signal.

[0043] Step 2: Turn on the resistance wire 12 to make it heat up and use the second thermocouple 13 to detect the temperature inside the enclosure 10 in real time until the temperature reaches the set temperature required for detection; ensure that the inside of the enclosure 10 is a single atmosphere or a vacuum state according to the experimental requirements to create a specific experimental environment.

[0044] Step 3: Start the transient spectrometer so that it can detect the sample in real time and capture the dynamic changes of the sample's structural characteristic peaks;

[0045] Step 4: Apply light stimulation or heat stimulation to the sample.

[0046] When the sample is light-stimulated, the irradiation source 5 is turned on, and the position and parameters of the irradiation source 5 are adjusted to ensure that the light spot coincides with the sample. The temperature change of the sample during the irradiation process is detected in real time by the first thermocouple 6 and the second thermocouple 13, and the temperature change curve over time is recorded. At the same time, the correspondence between the sample structure change and the energy change is obtained through the sample structure characteristic peaks. When the sample is thermally stimulated, the resistance wire 12 is turned on for heating. The temperature change of the sample during the heating process of the resistance wire is detected in real time by the first thermocouple 6 and the second thermocouple 13, and the temperature change curve over time is recorded. At the same time, the correspondence between the sample structure change and the energy change is obtained through the sample structure characteristic peaks.

[0047] To obtain more realistic and accurate energy and structural data, a reference experiment needs to be set up. The reference experiment is basically the same as the above-mentioned "method of using the in-situ measurement device for the structure and real-time temperature change of photothermal materials". The only difference is that no sample is placed in the sample cell. The results obtained by the reference experiment are used to calibrate and compensate the results obtained by the sample.

[0048] For some photothermal materials exhibiting photothermal energy storage phenomena, such as azophenyl materials, a portion of the light energy is converted into their own chemical structural energy during irradiation. These materials can be excited by light of specific wavelengths to release energy; simultaneously, they can also be thermally stimulated to reach a specific temperature, thus releasing energy. Combining these two different energy-charging and discharging operations with structural detection processes allows for mutual verification of the reliability of the obtained data, further validating the effectiveness and accuracy of the measuring device.

[0049] In this process, time acts as a key mediating factor, organically linking the two important parameters of temperature and sample structure, thereby enabling synchronous and in-situ sample structure and energy testing.

[0050] After the light source 1 of the transient spectrometer enters the ATR accessory, it is reflected by the first reflector group 2, adjusting the light path direction to be perpendicular to the ATR crystal 14 (usually, the ATR crystal 14 is made of diamond, but it can be flexibly replaced according to the specific needs of the sample being measured). Since the refractive index of the ATR crystal 14 is greater than that of the sample, and the incident angle of the light is greater than the critical angle, total internal reflection theoretically occurs at the crystal interface of the sample. However, in reality, some light penetrates to a certain depth (usually on the micrometer scale, called the "penetration depth") in the form of evanescent waves before returning to the ATR crystal 14. If the sample has a certain degree of light absorption, the energy of the light returning to the ATR crystal 14 will attenuate accordingly. Based on this attenuation, the characteristic peaks corresponding to the sample are obtained, thereby confirming the sample structure: chemical composition, molecular structure, and types of functional groups.

[0051] During testing, special care must be taken to ensure a tight fit between the sample and the ATR crystal 14. This is typically achieved by using a pressure post 9 to press the sample firmly. The light emitted from the ATR crystal 14 is detected by the detector 4 of the transient spectrometer and transmitted to the converter via an amplifier, thus enabling data visualization.

[0052] When the sample is photostimulated, the light emitted by the irradiation source 5 is processed by a collimating lens (not shown in the figure) to become parallel light, and then shines on the sample surface at a perpendicular angle, with the light spot size exactly covering the sample. This design ensures that all the energy generated by the irradiation source 5 directly acts on the sample, improving irradiation efficiency and accuracy. To ensure that the light from the irradiation source 5 can successfully irradiate the sample, the pressure column 9 needs to be made of high-transmittance glass.

[0053] The main function of the enclosure 10 is to maintain the specific temperature conditions required for the sample during testing. The enclosure 10 is made of ceramic insulation material, and contains multiple uniformly distributed resistance wires 12 and four second thermocouples 13 (two second thermocouples 13 are located at the top and two at the bottom of the enclosure 10). The resistance wires 12 are primarily used for heating, which is used for thermal stimulation of the sample or temperature compensation during reference experiments. The second thermocouples 13 are used to detect the real-time temperature inside the enclosure 10. Specifically, temperature is detected collaboratively by the first thermocouple 6 and the second thermocouple 13, and the average real-time temperature detected by the first thermocouple 6 and the second thermocouple 13 is taken as the sample's temperature change. The reason for designing the first thermocouple 6 and the second thermocouple 13 is that initially, the temperature distribution inside the enclosure 10 is uneven; detecting only one location would be inaccurate. As the sample releases heat, the temperature distribution inside the enclosure 10 becomes almost uniform, at which point the temperatures of the first thermocouple 6 and the second thermocouple 13 are essentially the same. The temperature data detected by the first thermocouple 6 and the second thermocouple 13 are displayed by an external secondary instrument to form specific temperature values.

[0054] The present invention has been described above by way of example. It should be noted that, without departing from the core of the present invention, any simple modifications, alterations or other equivalent substitutions that can be made by those skilled in the art without creative effort fall within the protection scope of the present invention.

Claims

1. An in-situ measurement device for the structure and real-time temperature change of a photothermal material, characterized in that, include: The transient spectrometer includes an ATR accessory, a sample cell (11), an irradiation source (5), and a transparent pressure column (9). The ATR accessory includes an ATR crystal (14), a first reflector group (2), and a second reflector group (3). The sample cell (11) is positioned above the ATR crystal (14). A first through hole (11-1) is formed at the bottom of the sample cell (11). The top surface of the ATR crystal (14) does not contact the bottom surface of the sample cell (11). Parallel light emitted by the light source (1) of the transient spectrometer undergoes total internal reflection within the ATR crystal (14) and is emitted from the ATR crystal (14) to form a first light path. The second reflector group (3) is used to reflect the first light path to the detector (4) of the transient spectrometer. A cover (10) is fixedly installed outside the sample pool (11) for sealing and heat preservation of the sample pool (11); Multiple resistance wires (12) are installed inside the cover (10); The pressure column (9) is set vertically, and the bottom of the pressure column (9) can move in the vertical direction. A second through hole is formed on the top surface of the cover (10). The bottom of the pressure column (9) extends into the cover (10) through the second through hole. A first thermocouple (6) is installed at the bottom of the pressure column (9). Multiple second thermocouples (13) are installed inside the cover (10), and the irradiation light source (5) is located directly above the sample cell (11) so that the light from the irradiation light source (5) passes through the pressure column (9) to irradiate the sample in the sample cell (11).

2. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The transient spectrometer is a UV transient spectrometer, an infrared transient spectrometer, or a UV-Vis-IR transient spectrometer.

3. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The size of the first through-hole (11-1) is less than or equal to the size of the ATR crystal (14).

4. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The cover (10) is a rectangular cavity with an opening formed on the bottom surface of the cavity, and the ATR crystal (14) is embedded in the opening.

5. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, An air inlet (7) and an air outlet (8) are formed on the cover (10).

6. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The irradiation source (5) is a single-band source, a dual-band source, or a multi-band source.

7. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The irradiation source (5) is vertically irradiated onto the sample cell (11).

8. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The pressure column (9) is made of glass.

9. The in-situ measurement device for the structure and real-time temperature change of photothermal materials according to claim 1, characterized in that, The distance between the top surface of the ATR crystal (14) and the bottom surface of the sample cell (11) is no greater than 0.01 mm.

10. The in-situ measurement device for photothermal material structure and real-time temperature change according to claim 1, characterized in that, The sample is placed in the sample cell (11). When the sample is liquid, the liquid level of the sample remains unchanged in the sample cell (11) due to capillary action.

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