Light-heat recoupling analysis system and analysis method

By using a photo-thermogravimetric analysis system, which combines a light source and a heating device, changes in sample mass can be monitored in real time. This solves the problem of differences between thermogravimetric analysis and solar-fuel conversion reactions, and achieves more efficient analytical results.

CN116148117BActive Publication Date: 2025-12-12INST OF ENGINEERING THERMOPHYSICS - CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202310106008.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-13
Publication Date
2025-12-12
Estimated Expiration
2043-02-13

AI Technical Summary

Technical Problem

Existing thermogravimetric analysis techniques cannot effectively simulate the actual conditions of solar-fuel conversion reactions, especially under the coupled driving of light and heat energy, resulting in significant differences between the analysis results and the actual reaction.

Method used

A photo-thermogravimetric coupling analysis system was designed, which combines a light source device and a heating device to simultaneously perform illumination and heating. A weight measurement device is used to monitor the changes in sample mass in real time, and an analysis device is used to process the data.

Benefits of technology

This method enables a more accurate simulation of the solar-fuel conversion reaction, improves the heating rate and uniformity, conforms to the actual conditions of the solar-fuel conversion reaction, and enhances the accuracy of the analysis.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The application discloses a light-heat recoupling analysis system and an analysis method. The light-heat recoupling analysis system comprises a heating device, a light source device, a weight measuring device and an analysis device. The heating device is suitable for heating a sample to be measured to a predetermined reaction temperature. The light source device is suitable for irradiating the sample to be measured with irradiation light of a predetermined light intensity distribution. The weight measuring device is suitable for measuring reference weights of the sample to be measured in a plurality of continuous time windows. The reference weight is the weight of the sample to be measured after different degrees of reaction over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution. The analysis device is suitable for analyzing the reference weights of the sample to be measured in the plurality of continuous time windows to obtain the result of the change of the weight of the sample to be measured over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of solar-chemical energy conversion, in particular to a light-heat re-coupling analysis system and an analysis method. BACKGROUND

[0002] Solar fuel has been widely valued at home and abroad in recent years due to its high energy density, easy transportation and storage, and the advantage of being used to prepare chemical products. The existing solar-fuel conversion approaches mainly include photochemical reaction, thermochemical reaction and light-heat synergistic reaction, and the main driving forces are light energy contained in sunlight, heat energy converted from sunlight, and the synergistic driving force of the two. An important testing method for studying the kinetics and thermodynamic characteristics of the above solar-fuel conversion reactions is to analyze the relationship between the quality change of the catalyst or reactant material and the conditions such as incident light energy flow density, incident light wavelength distribution, reaction temperature, and reaction atmosphere.

[0003] At present, the main method for studying the quality change of materials in solar-fuel conversion reactions is thermal gravimetric analysis technology. In thermal gravimetric analysis, the sample to be tested (i.e. the catalyst or reactant in the solar-fuel conversion reaction) is ground into powder, the sample to be tested is maintained in a gas environment with constant flow rate and composition, the reaction temperature is controlled by the heat output of the electric heating wire, and the mass change of the sample to be tested with the reaction temperature is recorded by a zero-position photoelectric balance. Compared with the driving force of the solar-fuel conversion reaction, the thermal gravimetric analysis cannot provide light energy input, but only heat energy input; and the heat energy input is an indirect heat transfer mode, which has slow heating rate and poor heating uniformity. The above characteristics make the thermal gravimetric analysis have great differences with the actual conditions of the solar-fuel conversion reaction, and cannot meet the analysis needs of the solar photochemical reaction, thermochemical reaction and light-heat synergistic reaction. SUMMARY

[0004] Therefore, the main purpose of the present application is to provide a light-heat re-coupling analysis system and an analysis method, so as to at least partially solve the above-mentioned and other technical problems.

[0005] According to the embodiments of the present application, as a first aspect of the present application, a light-heat re-coupling analysis system is provided, comprising:

[0006] a heating device adapted to heat the sample to be tested to a predetermined reaction temperature;

[0007] a light source device adapted to irradiate the sample to be tested with irradiation light of a predetermined light intensity distribution;

[0008] a weight measuring device adapted to measure reference weights of the sample to be tested in a plurality of continuous time windows, wherein the reference weights are weights of the sample to be tested after different degrees of reaction over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution;

[0009] an analyzing device adapted to analyze the reference weights of the sample to be tested in the plurality of continuous time windows to obtain a result of the change of the weight of the sample to be tested over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution.

[0010] According to an embodiment of the present application, the irradiation light is a light cone;

[0011] The light source device comprises:

[0012] a light source;

[0013] an optical converging unit adapted to converge the light emitted by the light source into the light cone.

[0014] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises:

[0015] a light intensity detecting device adapted to calibrate the light intensity of the center point of a light spot irradiated onto the surface of the sample to be tested, wherein the light spot is formed by the light cone irradiated onto the sample;

[0016] a photographing device adapted to photograph the light spot on the surface of the sample to obtain a photographing image;

[0017] The light intensity of the center point of the light spot calibrated by the light intensity detecting device and the photographing image are adapted to obtain the light intensity distribution of the light spot.

[0018] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises:

[0019] a light power adjusting device adapted to adjust the power of the light cone generated by the optical converging unit.

[0020] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises:

[0021] a light filtering device adapted to adjust the wavelength of the irradiation light provided by the light source device.

[0022] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises:

[0023] A reaction cavity, wherein the weight measuring device is arranged in the reaction cavity, and the reaction cavity is configured to be transparent to the irradiation light so that the irradiation light irradiates the sample.

[0024] According to an embodiment of the present application, the reaction cavity comprises a first sub-cavity and a second sub-cavity, the weight measuring device penetrates the first sub-cavity and the second sub-cavity, and one end of the sample placed on the weight measuring device is located in the first sub-cavity.

[0025] According to an embodiment of the present application, the heating device comprises:

[0026] A heating furnace, wherein the heating furnace is penetrated by the first sub-cavity, and a light transmission hole is arranged on the heating furnace, and the irradiation light irradiates the sample through the light transmission hole;

[0027] A heat preservation layer arranged on the inner wall of the heating furnace.

[0028] An electric heating wire wound on the outer wall of the first sub-cavity to heat the sample.

[0029] According to an embodiment of the present application, the sample is placed in a sample container, and the sample container is configured to make the surface of the sample equal to the size of the light spot.

[0030] According to an embodiment of the present application, the reaction cavity is filled with a predetermined kind of gas.

[0031] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises:

[0032] An attenuation sheet arranged between the camera and the light transmission hole.

[0033] A temperature measuring device arranged between the sample container and the weight measuring device, and adapted to detect the temperature of the sample.

[0034] According to an embodiment of the present application, as a second aspect of the present application, a light-heat recoupling analysis method is also provided, which utilizes the recoupling analysis system, and comprises:

[0035] Irradiating the sample with the irradiation light of a predetermined light intensity distribution by the light source device;

[0036] Heating the sample to a predetermined reaction temperature by the heating device and / or the light source device;

[0037] Irradiating the sample with the irradiation light of a predetermined light intensity distribution by the light source device;

[0038] measuring the reference weight of the sample to be tested in a plurality of continuous time windows by using a weight measuring device, wherein the reference weight is the weight of the sample to be tested after reacting over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution;

[0039] analyzing the reference weight of the sample to be tested in a plurality of continuous time windows by using an analysis device, to obtain the change of the weight of the sample to be tested over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution.

[0040] According to an embodiment of the present application, the heating device and / or the light source device are used to heat the sample to be tested to the predetermined reaction temperature, including:

[0041] The light intensity distribution of the irradiation light of the light source device is adjusted to maintain the sample at the predetermined reaction temperature.

[0042] According to an embodiment of the present application, the predetermined reaction temperature is the reaction temperature of the sample or room temperature.

[0043] According to an embodiment of the present application, the heating device and / or the light source device are used to heat the sample to be tested to the predetermined reaction temperature, including:

[0044] The sample to be tested is heated to the predetermined reaction temperature by adjusting the heat output of the heating device.

[0045] According to an embodiment of the present application, the heating device and / or the light source device are used to heat the sample to be tested to the predetermined reaction temperature, including:

[0046] The sample to be tested is heated to the predetermined reaction temperature by simultaneously adjusting the light intensity distribution of the irradiation light of the light source device and the heat output of the heating device.

[0047] According to an embodiment of the present application, the method further includes adjusting the wavelength of the irradiation light by using a light filtering device.

[0048] According to an embodiment of the present application, the actual conditions in the solar fuel conversion reaction can be simulated by using the light source device to irradiate the sample to be tested with irradiation light of a predetermined light intensity distribution, solving the problem that there is a large difference between the existing thermal gravimetric analysis and the actual solar fuel conversion reaction.

[0049] According to an embodiment of the present application, by heating the sample to be measured by using the heating device, and irradiating the sample to be measured with irradiation light of a predetermined light intensity distribution by using the light source device, measuring the reference weight of the sample to be measured in a plurality of continuous time windows by using the weight measuring device, and analyzing the reference weight of the sample to be measured in the plurality of continuous time windows by using the analysis device, the result of the change of the weight of the sample to be measured with time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution is obtained, and then the material mass change in the solar fuel conversion reaction can be analyzed. BRIEF DESCRIPTION OF DRAWINGS

[0050] Figure 1 A structure schematic diagram of a light-heat recoupling analysis system according to an embodiment of the present application is schematically shown;

[0051] Figure 2 A structure schematic diagram of another light-heat recoupling analysis system according to an embodiment of the present application is schematically shown;

[0052] Figure 3 A structure schematic diagram of still another light-heat recoupling analysis system according to an embodiment of the present application is schematically shown;

[0053] Figure 4 A structure schematic diagram of yet another light-heat recoupling analysis system according to an embodiment of the present application is schematically shown.

[0054] REFERENCE SIGNS

[0055] 1 heating device

[0056] 1-1 heating furnace body

[0057] 1-2 heat preservation layer

[0058] 1-3 electric heating wire

[0059] 2 light source device

[0060] 2-1 light source

[0061] 2-2 optical converging unit

[0062] 3 weight measuring device

[0063] 4 analysis device

[0064] 5 reaction cavity

[0065] 5-1 first sub-cavity

[0066] 5-2 second sub-cavity

[0067] 6 light intensity detecting device

[0068] 7 shooting device

[0069] 8. Optical power adjustment device

[0070] 9 samples to be tested

[0071] 10 sample containers

[0072] 11 attenuation plate

[0073] 12 temperature measuring devices

[0074] 13 Filter Devices

[0075] 14 light-transmitting holes

[0076] 15-inch rearview mirror Detailed Implementation

[0077] To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention will be further described in detail below with reference to specific embodiments and accompanying drawings.

[0078] Figure 1 The schematic diagram illustrates the principle of the optical-thermal re-coupling analysis system provided according to an embodiment of the present invention.

[0079] like Figure 1 As shown, the optical-thermal-gravity coupling analysis system includes: a heating device 1, a light source device 2, a weight measuring device 3, and an analysis device 4.

[0080] According to an embodiment of the present invention, the heating device 1 is adapted to heat the sample 9 to be tested to a predetermined reaction temperature. The light source device 2 is adapted to irradiate the sample 9 with irradiation light of a predetermined light intensity distribution; the weight measuring device 3 is adapted to measure the reference weight of the sample 9 within multiple consecutive time windows. The reference weight is the weight of the sample 9 after undergoing different degrees of reaction over time under the predetermined reaction temperature and / or under the predetermined light intensity distribution. The analysis device 4 is adapted to analyze the reference weight of the sample 9 within multiple consecutive time windows to obtain the result of the change in the weight of the sample 9 over time under the predetermined reaction temperature and / or under the predetermined light intensity distribution.

[0081] According to an embodiment of the present invention, the light intensity distribution includes the distribution of the magnitude of the light intensity irradiating the surface of the sample 9 to be tested and the distribution of the uniformity of the light intensity.

[0082] For the solar-to-fuel conversion reaction, improving the conversion efficiency or conversion ratio is the focus of research. The key to the above conversion reaction is the quality change of a specific solid reaction material (as a catalyst or a reactant in the solar-to-fuel conversion reaction). In related research, the method of stopping in the middle of the reaction, taking out the solid and weighing is usually used, but this method has a large error; in addition, in related research, the method of using a thermal gravimetric analyzer can be used by using heat instead of light, but heat and light play different roles in the solar-to-fuel conversion.

[0083] To solve the above problems, the embodiment of the present application introduces light into the traditional thermal gravimetric analyzer instrument. The "reaction while measuring" is realized, and the accuracy is improved; the method of the present application is closer to the conditions of the solar-to-fuel conversion process.

[0084] According to the embodiment of the present application, the sample to be measured 9 is a thermal catalyst, a semiconductor photocatalyst, an oxygen carrier of a chemical looping reaction or a chemical circulation reaction, a solid reactant in a chemical reaction, etc., and the effective component is in powder form. The sample to be measured acts as a catalyst or a reactant in the solar-to-fuel conversion reaction.

[0085] According to the embodiment of the present application, by using the light source device 1 to irradiate the sample to be measured 9 with irradiation light of a predetermined light intensity distribution, the actual conditions in the solar-to-fuel conversion reaction can be simulated, and the problem that there is a large difference between the existing thermal gravimetric analysis and the actual solar-to-fuel conversion reaction is solved.

[0086] According to the embodiment of the present application, by using the heating device 1 to heat the sample to be measured 9 and using the light source device 2 to irradiate the sample to be measured 9 with irradiation light of a predetermined light intensity distribution, using the weight measuring device 3 to measure the reference weight of the sample to be measured 9 in a plurality of consecutive time windows, and using the analysis device 4 to analyze the reference weight of the sample to be measured 9 in a plurality of consecutive time windows, the result of the change of the weight of the sample to be measured 9 with time under the condition of a predetermined reaction temperature and / or under the condition of a predetermined light intensity distribution is obtained, and then the material quality change in the solar-to-fuel conversion reaction can be analyzed.

[0087] According to the embodiment of the present application, the above-mentioned light-thermal gravimetric coupling analysis system further comprises: a reaction cavity 5, the weight measuring device 3 is arranged in the reaction cavity 5, and the reaction cavity 5 is configured to be able to transmit the irradiation light so that the irradiation light irradiates the sample to be measured 9. The reaction cavity 5 is a closed environment.

[0088] According to an embodiment of the present application, the weight measuring device 3 can be a null photometric balance. The reaction chamber includes a first sub-chamber 51 and a second sub-chamber 52. The null photometric balance penetrates the first sub-chamber 51 and the second sub-chamber 52. One end of the null photometric balance is placed in the first sub-chamber 51 to hold the sample 9, and the other end is placed with a counterweight. The null photometric balance is placed in the reaction chamber 5 because the null photometric balance is less susceptible to external interference due to its high measurement accuracy.

[0089] According to an embodiment of the present application, the heating device 1 includes a heating furnace body 1-1, a heat preservation layer 1-2, and an electric heating wire 1-3. The heat preservation layer 1-2 is arranged on the inner wall of the heating furnace body. The electric heating wire 1-3 is uniformly wound on the outer wall of the first sub-chamber 5-1 to uniformly heat the sample 9. The heating furnace body 2-1 is penetrated by the first sub-chamber 5-1. The heating furnace body is provided with a light transmission hole. The irradiation light is transmitted through the light transmission hole to irradiate the sample 9.

[0090] Before the sample 9 is heated by the heating device 1 and / or the sample is irradiated with the irradiation light of the predetermined light intensity distribution by the light source device 2, the reaction chamber is filled with a predetermined type of gas. The predetermined type of gas is divided into two streams. One stream of the gas is inert gas, and the flow direction is from the second sub-chamber 5-2 to the first sub-chamber 5-1. In addition to meeting the reaction requirements, the inert gas also protects the weight measuring device 3 in the second sub-chamber 5-2. The other stream of the gas can be inert gas or other gas in addition to inert gas. The other stream of the gas flows from the external pipeline to the first sub-chamber 5-1 but does not enter the second sub-chamber 5-2. The counterweight and electronic components of the null photometric balance are easily damaged by heat. If the predetermined type of gas flows in the opposite direction, the temperature of the predetermined type of gas entering the second sub-chamber 5-2 is high, which can damage the counterweight of the null photometric balance.

[0091] According to an embodiment of the present application, the light-heat recoupling analysis system further includes a light intensity detection device 6 and a shooting device 7. The light intensity detection device 6 is adapted to calibrate the light intensity of the center point of a light spot on the surface of the sample 9. The light spot is formed by the converging light cone. The shooting device 7 is adapted to shoot the light spot on the surface of the sample to obtain a shooting image. The light intensity of the center point of the light spot calibrated by the light intensity detection device 6 and the shooting image are adapted to obtain the light intensity distribution of the light spot.

[0092] According to the embodiment of the present application, the light intensity detecting device 6 can be a lambert target, and the photographing device 7 can be a CCD camera. The CCD camera can be arranged outside the heating device 1. The testing process of the light intensity distribution of the light spot irradiated on the sample row by using the lambert target and the CCD camera is as follows: the lambert target is moved to the position of the sample 9 to be tested (i.e. the lambert target is moved to the same height and the same direction as the sample 9 to be tested) so that the light spot irradiated on the sample 9 to be tested is the same as the light spot irradiated on the lambert target, and the light intensity of the center point of the light spot is calibrated by the lambert target. The CCD camera images the light spot by the light transmission hole, i.e. after the light intensity of the center point of the light spot is calibrated by the lambert target, the CCD camera images the light spot to obtain the light intensity distribution data of the whole light spot.

[0093] According to the embodiment of the present application, the sample is placed in the sample container 10, and the sample container 10 is configured to make the surface of the sample equal to the size of the light spot.

[0094] According to the embodiment of the present application, the sample container 10 can be a crucible, which is an inverted circular truncated cone. The longitudinal section angle of the circular truncated cone is greater than or equal to the converging angle of the converging light cone, so as to ensure that the side wall of the circular truncated cone does not block the light, and thus the surface of the sample 9 to be tested in the crucible is covered by the light spot.

[0095] According to the embodiment of the present application, the light-heat recoupling analysis system further comprises an attenuating sheet 11 and a temperature measuring device 12. The attenuating sheet 11 is arranged between the photographing device 7 and the light transmission hole. The temperature measuring device 12 is arranged between the sample container 10 and the weight measuring device 3, and is adapted to detect the temperature of the sample 9 to be tested. The temperature measuring device 12 can be a K-type thermocouple, which is fixed on the horizontal beam of the zero optical balance, and the measuring point is close to the bottom surface of the crucible, and is used to measure the temperature of the sample to be tested. The above data is transmitted to the analysis device 4 such as a computer for synchronous acquisition and recording.

[0096] According to the embodiment of the present application, the irradiated light is a converging light cone, and the light source device 2 comprises a light source 2-1 and an optical converging unit 2-2. The optical converging unit 2-2 is adapted to converge the light emitted by the light source 2-1 into the converging light cone. Figure 1 , Figure 2 Figure 3 and Figure 4 respectively show different forms of light sources and optical converging units.

[0097] Figure 1 The light source 2-1 in is a point light source, and the corresponding optical converging unit 2-2 is an elliptical cross-section reflecting condenser, Figure 2 The light source 2-1 in is a parallel light source, and the corresponding optical converging unit 2-2 is a disc-shaped rotating parabolic reflector, Figure 3 ​The light source 2-1 in the embodiment is a parallel light source, and the optical converging unit 2-2 is a point focusing Fresnel lens. Figures 1-3 The light source 2-1 in the embodiment can emit sunlight or simulated sunlight, and the energy distribution of each wavelength band is mainly in the range of 300-2500 nm, and the energy distribution of each wavelength band is consistent or close to the energy distribution of the AM1.5 solar spectrum. Figure 3 In the embodiment, the light power output by the light source 2-1 is 0-3 kW, for example, it can be 0 kW, 1 kW, 2 kW, 3 kW, and can be continuously adjusted. The light cone emitted by the point focusing Fresnel lens is projected on the reflector. By adjusting the reflector, the angle between the central axis of the light cone and the central axis of the crucible is less than 0.2°. The diameter of the light spot is equal to the diameter of the bottom surface of the crucible, and both are 5-8 mm. The average light intensity of the light spot is 0-1300 kW m -2 (for example, it can be 0 kW m -2、 , 200 kW m -2 , 400 kW m -2 ) and continuously adjustable.

[0098] Figure 4 The light source 2-1 in the embodiment can be a laser array composed of multiple lasers of different wavelengths. The wavelength of the laser emitted by each laser is a single-wavelength laser in the range of 300-2500 nm. The laser array generates parallel coherent light. By using multiple lasers of different wavelengths in the range, a laser array is formed. The optical converging unit 2-2 is a plurality of selective transmission filters and / or a filter group composed of a plurality of selective transmission filters, which combines different beams in the laser array into one beam. The wavelength range of the combined laser beam is between 300-2500 nm, and the distribution ratio of the light power in the wavelength range of 300-2500 nm is close to the distribution ratio in the AM1.5 solar spectrum. By adjusting the output power of the laser array, the light intensity of the combined laser beam can be continuously adjustable in the range of 1-1700 kW m -2 .

[0099] With reference to Figures 1-3 , according to the embodiment of the present application, the above-mentioned light-heat recoupling analysis system further comprises a light power adjusting device 8 adapted to adjust the power of the light cone generated by the optical converging unit 2-2.

[0100] According to an embodiment of the present application, the light power adjusting device 8 can be a grating. The grating opening degree is continuously adjustable from 0-100%, and the time interval for adjusting the opening degree is as low as 20 ms. There are two working modes for the light source 2-1: in the continuous working mode, the opening degree of the grating is fixed at a certain value from 0-100% and remains unchanged; in the intermittent working mode, the opening degree of the grating is switched between 0% and 100% in cycles, the 100% opening degree is light illumination, and the 0% opening degree is no light illumination, and the time interval of light illumination and no light illumination is adjustable with a minimum unit of 20 ms.

[0101] According to an embodiment of the present application, the light-heat recoupling analysis system further comprises a light filtering device 13 adapted to adjust the wavelength of the light cone.

[0102] According to an embodiment of the present application, the light filtering device 13 can be a filter, and the base material of the filter and the material of the first sub-cavity are both high-transmittance quartz glass, the working temperature is room temperature-1200℃, and the transmittance of the filter to the 300-2500 nm spectral band is >95% within the working temperature range.

[0103] According to an embodiment of the present application, the working temperature of the grating, the light concentrator, and the reflector is room temperature-1200℃, and the optical properties are stable within the working temperature range. The working temperature of the electric heating furnace body, the electric heating wire, and the crucible is room temperature-1200℃, and the physicochemical properties are stable within the working temperature range, without volatilization or sublimation.

[0104] Based on the above-mentioned coupling analysis system, an embodiment of the present application further provides a light-heat recoupling analysis method, which comprises the following operations S1-S4.

[0105] In operation S1, the light source device is used to irradiate the predetermined light intensity distribution of the irradiation light to the sample to be measured.

[0106] In operation S2, the heating device or the light source device is used to heat the sample to be measured to a predetermined reaction temperature.

[0107] In operation S3, the weight measuring device is used to measure the reference weight of the sample to be measured within a plurality of continuous time windows, wherein the reference weight is the weight of the sample to be measured after reaction over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution.

[0108] In operation S4, the analysis device is used to analyze the reference weight of the sample to be measured within a plurality of continuous time windows, to obtain the change of the weight of the sample to be measured over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution.

[0109] According to an embodiment of the present application, the heating of the sample to be measured to a predetermined reaction temperature by the heating device or the light source device in operation S2 comprises operations S21-S23.

[0110] In operation S21, the light intensity distribution of the light source device is adjusted to maintain the sample at the predetermined reaction temperature. The predetermined reaction temperature is the reaction temperature of the sample or room temperature.

[0111] According to an embodiment of the present application, when the predetermined reaction temperature is the reaction temperature of the sample, it is a direct light focusing heating method, and when the predetermined reaction temperature is room temperature, it is a separate light irradiation without heating method.

[0112] According to an embodiment of the present application, the direct light focusing heating method specifically comprises operation S211: turning on the light source and adjusting the grating opening to be greater than 0%. The electric heating wire is turned off. A predetermined type of gas is introduced into the reaction chamber to obtain a reaction atmosphere. The reaction temperature of the sample to be measured is maintained by adjusting the light source output power and the grating opening to be greater than 0%. The relationship between the mass of the sample to be measured and the light focusing energy flux density and the light focusing heat collection temperature is studied by using a null optical balance. It is suitable for chemical reactions driven by light energy and heat energy, in which light energy is the main driving force.

[0113] According to an embodiment of the present application, the separate light irradiation without heating method specifically comprises operation S212: turning on the light source and adjusting the grating opening to be greater than 0%. The electric heating wire is turned off. A reaction atmosphere is introduced into the reaction chamber. The sample to be measured is cooled by adjusting the light source output power, the grating opening or using an intermittent working mode, and is maintained at room temperature by using liquid nitrogen. The relationship between the mass of the sample to be measured and the light spot energy flux density is studied by using a null optical balance. It is suitable for chemical reactions driven by light energy.

[0114] According to an embodiment of the present application, the heating of the sample to be measured to a predetermined reaction temperature by the heating device and / or the light source device comprises:

[0115] In operation S22, the sample to be measured is heated to the predetermined reaction temperature by adjusting the heat output of the heating device.

[0116] According to an embodiment of the present application, operation S22 is a separate heating without light irradiation method: the light source is removed or the grating opening is adjusted to 0%. A reaction atmosphere is introduced into the reaction chamber. The sample to be measured is heated to the reaction temperature by adjusting the heat output of the electric heating wire. The relationship between the mass of the sample to be measured and the reaction temperature is studied by using a null optical balance. It is suitable for chemical reactions driven by heat energy.

[0117] According to an embodiment of the present application, the heating of the sample to be measured to a predetermined reaction temperature by the heating device and / or the light source device comprises:

[0118] The operation S23 adjusts the light intensity distribution of the irradiation light of the light source device and the heat power output by the heating device simultaneously, and heats the sample to be measured to a predetermined reaction temperature.

[0119] According to the embodiment of the present application, the operation S23 is an electrically assisted light focusing heating method: the light source is turned on and the grating opening is adjusted to be greater than 0%. The electric heating wire is turned on. The reaction atmosphere is introduced into the reaction cavity. The sample to be measured is maintained at the reaction temperature by adjusting the light power output of the light source, the grating opening, and the heat power output of the electric heating wire. The zero position photoelectric balance is used to study the relationship between the mass of the sample to be measured and the light focusing energy flux density and the light focusing heat temperature. The method is suitable for the coupling driving of light energy and heat energy, and the chemical reaction driven by the heat energy is the main driving force.

[0120] According to the embodiment of the present application, the above method further comprises adjusting the wavelength of the irradiation light by using a light filtering device. The wavelength distribution affects the chemical reaction and is one of the focuses of the study of solar-driven chemical reactions. Different samples to be measured require different wavelengths, and therefore the wavelength needs to be adjusted for different samples to be measured.

[0121] The light-heat recoupling analysis system and analysis method provided by the embodiment of the present application can use light focusing solar energy or other light sources, and assist with an electric heating wire to irradiate and / or directly heat the sample to be measured. The relationship between the mass change of the sample to be measured and the light focusing energy flux density, the reaction temperature, and the reaction atmosphere under the conditions of separate heating without irradiation, separate irradiation without heating, and simultaneous light focusing and heating can be obtained. The method is helpful for the study of the reaction mechanism and performance.

[0122] The light-heat recoupling analysis system and analysis method can provide light focusing light energy input to the sample to be measured, directly generate light focusing heat on the sample to be measured, have fast heating rate, good uniformity, and good mass stability, and are simple to operate, and meet the actual conditions of the photochemical reaction, the thermal chemical reaction, and the light-heat coupling reaction of the solar-chemical energy conversion.

[0123] The above specific embodiments further specifically describe the purpose, technical solutions, and advantages of the present application. It should be understood that the above specific embodiments are only specific embodiments of the present application and are not used to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A photothermal weight coupling analysis system, comprising: a heating device adapted to heat a sample to be tested to a predetermined reaction temperature; a light source device adapted to irradiate the sample to be tested with an irradiation light of a predetermined light intensity distribution; a weight measuring device adapted to measure a reference weight of the sample to be tested in a plurality of consecutive time windows, wherein the reference weight is a weight of the sample to be tested after different degrees of reaction over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution; an analysis device adapted to analyze the reference weight of the sample to be tested in the plurality of consecutive time windows to obtain a result of a change in weight of the sample to be tested over time under the condition of the predetermined reaction temperature and / or under the condition of the predetermined light intensity distribution; wherein the irradiation light is a light cone; the photothermal weight coupling analysis system further comprises: a light intensity detecting device adapted to calibrate a light intensity of a center point of a light spot on a surface of the sample to be tested, wherein the light spot is formed by the light cone irradiating onto the sample; the light intensity detecting device is a lambertian target; a shooting device adapted to shoot the light spot on the surface of the sample to obtain a shooting image; wherein the light intensity of the center point of the light spot calibrated by the light intensity detecting device and the shooting image are adapted to obtain a light intensity distribution of the light spot; wherein the light source device comprises: a light source; the light source device emits light with a wavelength in a range of 300 nm to 2500 nm and an energy distribution consistent with or close to an AM1.5 standard solar spectrum; an optical converging unit adapted to converge the light emitted by the light source into the light cone; The average light intensity of the light spot is 0-1300 kW m -2 and continuously adjustable. 2.The photothermal weight coupling analysis system according to claim 1, further comprising: a light power adjusting device adapted to adjust a power of the light cone generated by the optical converging unit. 3.The photothermal weight coupling analysis system according to claim 1, further comprising: a light filtering device adapted to adjust a wavelength of the irradiation light provided by the light source device. 4.The photothermal weight coupling analysis system according to claim 1, further comprising: a reaction cavity, wherein the weight measuring device is arranged in the reaction cavity, and the reaction cavity is configured to be transparent to the irradiation light so that the irradiation light irradiates onto the sample to be tested.

5. The photothermal recoupling analysis system of claim 4, wherein, The reaction cavity comprises a first sub-cavity and a second sub-cavity, the weight measuring device penetrates through the first sub-cavity and the second sub-cavity, and an end of the weight measuring device where the sample to be tested is placed is located in the first sub-cavity.

6. The photothermal recoupling analysis system of claim 5, wherein, The heating device comprises: a heating furnace body, wherein the first sub-cavity penetrates through the heating furnace body, the heating furnace body is provided with a light transmission hole, and the irradiation light irradiates onto the sample to be tested through the light transmission hole; a heat preservation layer arranged on an inner wall of the heating furnace body; an electric heating wire wound on an outer wall of the first sub-cavity to heat the sample to be tested.

7. The photothermal recoupling analysis system of claim 1, wherein, The sample is placed in a sample container, and the sample container is configured so that a surface of the sample is equal in size to the light spot.

8. The photothermal recoupling analysis system of claim 4, wherein, The reaction cavity is filled with a predetermined kind of gas.

9. The photo-thermal recoupling analysis system of claim 6, further comprising: an attenuating sheet disposed between the camera and the light passage hole; a temperature measuring device disposed between the sample container and the weight measuring device, and adapted to measure the temperature of the sample.

10. A photo-thermal recoupling analysis method using the recoupling analysis system of any one of claims 1-9, comprising: illuminating the sample with a predetermined light intensity distribution of illumination light using the light source device; heating the sample to a predetermined reaction temperature using the heating device and / or the light source device; measuring the reference weight of the sample in a plurality of consecutive time windows using the weight measuring device, wherein the reference weight is the weight of the sample after reacting over time under the predetermined reaction temperature and / or under the predetermined light intensity distribution; analyzing the reference weight of the sample in the plurality of consecutive time windows using the analysis device to obtain the change of the weight of the sample over time under the predetermined reaction temperature and / or under the predetermined light intensity distribution.

11. The method of claim 10, wherein, heating the sample to a predetermined reaction temperature using the heating device and / or the light source device, comprising: adjusting the light intensity distribution of the illumination light of the light source device to maintain the sample at the predetermined reaction temperature.

12. The method of claim 11, wherein, the predetermined reaction temperature is the reaction temperature of the sample or room temperature.

13. The method of claim 10, wherein, heating the sample to a predetermined reaction temperature using the heating device and / or the light source device, comprising:

14. The method of claim 10, wherein, adjusting the heat output of the heating device to heat the sample to the predetermined reaction temperature. heating the sample to a predetermined reaction temperature using the heating device and / or the light source device, comprising:

15. The method of claim 10, wherein, simultaneously adjusting the light intensity distribution of the illumination light of the light source device and the heat output of the heating device to heat the sample to the predetermined reaction temperature. the method further comprising: adjusting the wavelength of the illumination light using the filter device.

Citation Information

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