Infrared imaging system, detection method and device based on infrared imaging system
The dynamic changes in the surface oxygen vacancies of metal oxides are monitored in real time through infrared imaging systems, which solves the problem of difficulty in quantitative measurement in the prior art, and reduces energy consumption in the field of carbon dioxide capture, achieving the effect of efficient screening of high-performance CO2 absorbers.
Patent Information
- Application Number
- CN202510213294.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-25
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2045-02-25
AI Technical Summary
The prior art is difficult to monitor and quantitatively measure the dynamic changes in the surface oxygen vacancies of metal oxides in real time, and in the field of carbon dioxide capture, high regeneration energy consumption limits the application of absorbents.
An infrared imaging system is adopted, including an in-situ reaction cell module, an infrared optical imaging module and a data processing module. The infrared image of the surface of the reaction sample is obtained through the infrared optical imaging module. The data processing module performs data analysis, extracts kinetic curves, and fits them using preset kinetic equations to determine the kinetic data of the reaction sample.
It realizes efficient and high-throughput measurement of the reaction kinetics of metal oxide surfaces and gas molecules, and can screen out high-performance CO2 absorbers from a large number of potentially excellent absorber formulations, reducing energy consumption.
Smart Images

Figure CN119688786B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of heterogeneous interface reaction research, and in particular to an infrared imaging system, and a detection method and device based on the infrared imaging system. Background Art
[0002] This section is intended to provide a background or context for the embodiments of the invention described herein. No description herein is admitted to be prior art by virtue of its inclusion in this section.
[0003] For gas-solid interfacial reactions, metal oxides are one of the most important solid materials and have important applications in heterogeneous catalysis, photocatalysis, and electronic and chemical sensing. They are not only catalytic active centers, but also serve as supporting structures to promote reactions. The oxygen vacancy structure on the surface of metal oxides is crucial for heterogeneous catalysis. Oxygen vacancies are formed by lattice oxygen deficiency under high temperature or reducing conditions. Since they were proposed, they have been confirmed by scanning tunneling microscopy (STM), atomic force microscopy (AFM) and other technologies. They are surface reaction active sites that affect the electronic and chemical properties of the material surface, thereby regulating the kinetics and mechanism of chemical reactions. Oxygen vacancies on the surface of transition metal oxides are highly active and easily adsorb and activate oxygen molecules to form active oxygen species. Changes in the concentration of these species affect the chemical and electronic properties of the material surface. Although techniques such as electron paramagnetic resonance (EPR), nuclear magnetic resonance spectroscopy (NMR), and X-ray photoelectron spectroscopy (XPS) can quantitatively characterize surface active oxygen species, it is difficult to monitor their dynamic changes in real time, and these techniques lack sufficient measurement flux to achieve efficient kinetic detection.
[0004] For carbon dioxide (CO 2 ) capture, which is of great significance in reducing greenhouse gas emissions. At present, alkaline absorbents based on organic amines are widely used because of their considerable absorption performance, mature industrial technology and low material cost. However, the high regeneration energy consumption greatly limits their further application on carbon dioxide. Based on high-throughput screening strategies, it is expected to screen out high-performance CO from a large number of potential excellent absorbent formulations. 2 Therefore, it is particularly urgent to develop a high-throughput screening strategy. Summary of the invention
[0005] The embodiment of the present invention provides an infrared imaging system for efficiently and high-throughput quantification of the interaction between heterogeneous interfaces, realizing the reaction kinetics measurement between metal oxide surfaces and gas molecules, and screening out high-performance CO from a large number of potential excellent absorbent formulations. 2 absorbent, the infrared imaging system comprises: an in-situ reaction cell module, an infrared optical imaging module and a data processing module;
[0006] The in-situ reaction pool module comprises an in-situ gas circulation pool, a mass flow meter and a gas source; the in-situ gas circulation pool comprises a gas circulation chamber, a heating platform, and a metal oxide library substrate arranged in the gas circulation chamber and placed on the heating platform; the metal oxide library substrate is provided with a plurality of holes for placing reaction samples; the reaction samples comprise solid samples or gas samples; the gas source is used to transmit the reaction gas to the gas circulation chamber of the in-situ gas circulation pool through the mass flow meter; the mass flow meter is used to control the concentration and flow rate of the reaction gas; the heating platform is used to heat the reaction sample;
[0007] The infrared optical imaging module is used to obtain an infrared image of the surface of the reaction sample and send the infrared image to the data processing module;
[0008] The data processing module is used to perform data analysis on the received infrared image and extract a kinetic curve from the infrared image;
[0009] When the reaction sample is a solid sample, the data processing module is further used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve;
[0010] When the reaction sample is a liquid sample, the data processing module is further used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface.
[0011] The present invention also provides a detection method based on an infrared imaging system, which is used to efficiently and high-throughput quantify the interaction between heterogeneous interfaces, realize the reaction kinetics measurement between metal oxide surfaces and gas molecules, and screen out high-performance CO from a large number of potential excellent absorbent formulations. 2 The absorbent is applied to the above infrared imaging system, comprising:
[0012] Acquire an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a gas sample;
[0013] Perform data analysis on infrared images and extract kinetic curves from them;
[0014] When the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or the kinetic curve is fitted using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve;
[0015] When the reaction sample is a liquid sample, the kinetic curve is fitted using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface.
[0016] The present invention also provides a detection device based on an infrared imaging system, which is used to quantify the interaction between heterogeneous interfaces efficiently and at high throughput, to measure the reaction kinetics between metal oxide surfaces and gas molecules, and to screen out high-performance CO from a large number of potential excellent absorbent formulations. 2 The device includes the above-mentioned infrared imaging system, and further includes:
[0017] An acquisition module, used to acquire an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a gas sample;
[0018] Data analysis module, used to analyze infrared images and extract kinetic curves from infrared images;
[0019] A kinetic data determination module, for fitting a kinetic curve using a preset adsorption kinetic equation to determine kinetic data on the surface of the reaction sample when the reaction sample is a solid sample, and / or fitting the kinetic curve using a heat dissipation kinetic equation to determine thermodynamic data on the surface of the reaction sample; the kinetic curve is an infrared image intensity curve;
[0020] The thermodynamic data determination module is used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the surface of the reaction sample when the reaction sample is a liquid sample.
[0021] An embodiment of the present invention further provides a computer device, including a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor implements the above-mentioned detection method based on the infrared imaging system when executing the computer program.
[0022] An embodiment of the present invention further provides a computer-readable storage medium, wherein the computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the above-mentioned detection method based on the infrared imaging system is implemented.
[0023] An embodiment of the present invention further provides a computer program product, which includes a computer program. When the computer program is executed by a processor, the above-mentioned detection method based on the infrared imaging system is implemented.
[0024] Compared with the oxygen vacancy characteristic detection technical solution of the metal oxide surface in the prior art, the embodiment of the present invention uses an in-situ reaction pool module, an infrared optical imaging module and a data processing module; the in-situ reaction pool module includes an in-situ gas circulation pool, a mass flow meter and a gas source; the in-situ gas circulation pool includes a gas circulation cavity, a heating platform, and a metal oxide library substrate arranged in the gas circulation cavity and placed on the heating platform; a plurality of holes for placing reaction samples are arranged on the metal oxide library substrate; the reaction sample includes a solid sample or a gas sample; the gas source is used to transmit the reaction gas to the gas circulation cavity of the in-situ gas circulation pool through the mass flow meter; the mass flow meter is used to control the concentration and flow rate of the reaction gas; the heating platform is used to heat the reaction sample; the infrared optical imaging module is used to obtain an infrared image of the reaction sample surface, and send the infrared image to the data processing module ; A data processing module is used to perform data analysis on the received infrared image and extract a kinetic curve from the infrared image; when the reaction sample is a solid sample, the data processing module is also used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or, to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve; when the reaction sample is a liquid sample, the data processing module is also used to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface, which can efficiently and high-throughput quantify the interaction between heterogeneous interfaces, realize the reaction kinetic measurement of metal oxide surfaces and gas molecules, and screen out high-performance CO from a large number of potential excellent absorbent formulations. 2 Absorbent. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the prior art descriptions. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. In the drawings:
[0026] Figure 1 is a schematic diagram of an infrared imaging system in an embodiment of the present invention;
[0027] Figure 2 is a schematic diagram of a specific example of an infrared imaging system in an embodiment of the present invention;
[0028] Figure 3 is a schematic diagram of a specific example of an infrared imaging system in an embodiment of the present invention;
[0029] Figure 4 is a schematic diagram of an infrared optical imaging module according to an embodiment of the present invention;
[0030] Figure 5 The bright field image and infrared image of the metal oxide library substrate on which various reaction samples are placed in an embodiment of the present invention;
[0031] Figure 6 is a flow chart of a detection method based on an infrared imaging system in an embodiment of the present invention;
[0032] Figure 7 It is a reaction kinetic curve of multiple adsorption and desorption cycles between carbon monoxide molecules and the surface of zinc oxide powder and an enlarged diagram of part of the curve in an embodiment of the present invention;
[0033] Figure 8 The kinetic curve diagram of the surface of zinc oxide powder and tungsten trioxide powder in the embodiment of the present invention and the correlation diagram between the apparent response kinetic constant and the partial pressure of carbon monoxide gas;
[0034] Fig. 9 It is a schematic diagram of infrared intensity variation images of the surfaces of multiple metal oxide samples and kinetic curves and fitting curves of metal oxide samples in a metal oxide library substrate in an embodiment of the present invention;
[0035] Fig.10 The near infrared spectrum of carbon monoxide before and after adsorption on the surface of zinc oxide and the spectrum fitting curve diagram in the embodiment of the present invention;
[0036] Fig.11 The near infrared spectrum evolution spectrum of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle and the surface infrared radiation rate a in the embodiment of the present invention are shown in FIG. ε Evolution dynamics graph;
[0037] Fig.12 It is a kinetic curve diagram of the surface temperature change of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle in the embodiment of the present invention;
[0038] Fig.13 This is a correlation diagram between the surface emissivity and the surface radiation infrared signal intensity of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle in an embodiment of the present invention;
[0039] Fig.14 It is a bright field image, infrared image, kinetic curve diagram of temperature change during adsorption of carbon dioxide molecules and organic amine alkali solutions of different concentrations in the embodiment of the present invention, and a temperature rise process diagram of an ideal adiabatic system during the reaction process after kinetic fitting;
[0040] Fig.15 It is a structural block diagram of a detection device based on an infrared imaging system in an embodiment of the present invention;
[0041] Fig.16Schematic diagram of the computer device structure in an embodiment of the present invention. DETAILED DESCRIPTION
[0042] To make the purpose, technical solution and advantages of the embodiments of the present invention more clear, the embodiments of the present invention are further described in detail below in conjunction with the accompanying drawings. Here, the exemplary embodiments of the present invention and their descriptions are used to explain the present invention, but are not intended to limit the present invention.
[0043] The acquisition, storage, use, and processing of data in the technical solution of this application comply with the relevant provisions of laws and regulations.
[0044] The in situ introduction of reducing gases such as carbon monoxide (CO) combined with conductivity, electrochemistry, gas chromatography (GC), infrared spectroscopy (IR) and Raman spectroscopy can be used to study the characteristics of oxygen vacancies, but these techniques lack sufficient measurement throughput to achieve efficient kinetic detection.
[0045] Infrared imaging technology is generally considered to be a high-throughput tool set for studying the thermal properties of material surfaces and is widely used in thermal imaging studies of material surfaces. However, it is more noteworthy that the emissivity of the material surface in the infrared band is closely related to the dielectric properties of its surface. Infrared imaging technology is not only a measurement technology that is sensitive to the temperature of the material surface, but also a measurement technology that is sensitive to the dielectric state of the material surface. In addition, infrared imaging technology does not require the introduction of an additional excitation light source, and the thermal radiation information of the material itself can intrinsically reflect the dielectric properties of its surface. In the present invention, for the gas-solid interface, the infrared emissivity of the transition metal oxide surface changes with the introduction of the reaction gas molecule (CO) atmosphere under high temperature conditions. This is because as the reaction gas molecules combine with the surface active oxygen species and adsorb on the material surface, the dielectric properties of the material surface are changed, causing its emissivity in the infrared band to change. Based on this, the present invention proposes a method for realizing in-situ high-throughput gas-solid interface adsorption reaction kinetics measurement using infrared imaging technology. Through the fitting of the Langmuir adsorption kinetic model, the molecular binding kinetics and dissociation kinetics and equilibrium constants of the gas-solid interface can be quantitatively measured. For the gas-liquid interface, the alkaline solution is 2 After the gas molecules are adsorbed, the surface temperature changes due to the intense reaction heat. The technical principle of infrared thermal imaging can be used to measure the heat release kinetic characteristics of the reaction during the adsorption process. The heat dissipation kinetic equation can be used to accurately quantify the heat release characteristics of different CO 2 The technology not only provides a new way to efficiently monitor the kinetics of heterogeneous interfacial reactions, but also brings new perspectives to the research of catalysis, sensing and gas adsorption.
[0046] In order to solve the problems of the prior art, an embodiment of the present invention provides an infrared imaging system. Figure 1 Schematic diagram of an infrared imaging system in an embodiment of the present invention. Figure 1 As shown, the infrared imaging system in the embodiment of the present invention may include: an in-situ reaction pool module, an infrared optical imaging module and a data processing module;
[0047] The in-situ reaction pool module includes an in-situ gas circulation pool, a mass flow meter and a gas source; the in-situ gas circulation pool includes a gas circulation chamber, a heating platform, and a metal oxide library substrate arranged in the gas circulation chamber and placed on the heating platform; the metal oxide library substrate is provided with a plurality of holes for placing reaction samples; the reaction samples include solid samples or gas samples; the gas source is used to transmit the reaction gas to the gas circulation chamber of the in-situ gas circulation pool through the mass flow meter; the mass flow meter is used to control the concentration and flow rate of the reaction gas; the heating platform is used to heat the reaction sample;
[0048] The infrared optical imaging module is used to obtain an infrared image of the surface of the reaction sample and send the infrared image to the data processing module;
[0049] A data processing module is used to perform data analysis on the received infrared images and extract kinetic curves from the infrared images;
[0050] When the reaction sample is a solid sample, the data processing module is further used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve;
[0051] When the reaction sample is a liquid sample, the data processing module is also used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface.
[0052] The infrared imaging system provided by the embodiment of the present invention performs real-time in-situ infrared optical imaging through an infrared optical imaging module, and the data processing module performs data analysis and processing on the image to obtain the adsorption reaction kinetic curve of the heterogeneous interface. For the gas-solid interface adsorption reaction process, the Langmuir kinetic equation is used to perform data fitting to obtain the adsorption reaction kinetic constant and the adsorption reaction equilibrium constant, which can quantitatively measure the intermolecular binding kinetics and dissociation kinetics and equilibrium constant of the gas-solid interface, and compare the adsorption intensity differences between different samples.
[0053] For the gas-liquid interface adsorption reaction process, the heat dissipation kinetic equation is used to obtain the adsorption reaction enthalpy change value. According to the temperature change kinetic characteristics, the heat dissipation kinetic equation can be used to accurately quantify the CO content of different organic amine solutions. 2Adsorption enthalpy information is used to measure the gas adsorption capacity of the sample. The present invention directly uses the thermal radiation information of the sample to reflect its surface chemical state and temperature change characteristics, and quantifies the interaction between heterogeneous interfaces efficiently and with high throughput through kinetic data analysis, which is expected to become a new method for studying the properties of heterogeneous interfaces.
[0054] The technical principle and implementation effects of the present invention are further described below in conjunction with the accompanying drawings and specific embodiments. However, the following embodiments are only used to illustrate the present invention in detail and do not limit the scope of the present invention in any way.
[0055] In one embodiment, the in-situ gas circulation cell also includes an infrared optical window; the infrared optical window is used to allow the infrared light emitted from the surface of the metal oxide sample to exit the in-situ gas circulation cell; the infrared optical window is made of a material whose transmittance in the short-wave infrared region is greater than a preset transmittance; the metal oxide library substrate is located directly below the infrared optical window.
[0056] In one embodiment, the infrared optical imaging module may include a short-wave infrared camera; the short-wave infrared camera has a sensitive wavelength of 0.9 microns to 1.7 microns; the short-wave infrared camera is used to obtain infrared images of the surface of the reaction sample without introducing an additional light source.
[0057] In one embodiment, the reaction sample may include a solid sample or a liquid sample. In the embodiment of the present invention, the solid sample is exemplified by metal oxide powder, and the liquid sample is exemplified by organic amine alkali solution.
[0058] Figure 2 FIG. 1 is a schematic diagram of a specific example of an infrared imaging system in an embodiment of the present invention. Figure 2 As shown, in one embodiment, the infrared imaging system may specifically include: 1-gas source, 2-mass flow meter, 3-short-wave infrared camera, 4-in-situ gas flow cell, 5-temperature controller, 6-infrared optical window, 7-thermocouple, 8-metal oxide library substrate, 9-ceramic heating rod, and 10-heating platform body.
[0059] In this embodiment, if Figure 2 As shown, the in-situ gas circulation pool 4 may be provided with an infrared optical window and a heating platform, the metal oxide reservoir substrate 8 may be made of stainless steel, and the heating platform body 10 may be made of copper.
[0060] In this embodiment, if Figure 2 As shown, the gas source 1 may include nitrogen and carbon monoxide, wherein the nitrogen is used as an inert gas to provide an inert atmosphere for the gas flow cell, and the carbon monoxide is used as a reaction gas to react with the reaction sample in the metal oxide library substrate. It can be seen that the gas source is also used to deliver nitrogen or other inert gases to the gas flow chamber of the in-situ gas flow cell.
[0061] In one embodiment, the gas circulation chamber is provided with an air inlet and an air outlet; wherein the gas source is sequentially transmitted to the gas circulation chamber through a mass flow meter and the air inlet; the air outlet is connected to an exhaust gas treatment module; the exhaust gas treatment module is used to store and process the acquired gas; and the in-situ gas circulation pool is used to provide a reaction channel for the reaction gas and the reaction sample.
[0062] In this embodiment, if Figure 2 As shown, the mass flow meter 2 is connected between the gas source 1 and the in-situ gas circulation pool 4, and is connected to the in-situ gas circulation pool 4 through the air inlet. The mass flow meter 2 provides two control devices for controlling nitrogen and carbon monoxide in the gas source 1 respectively, and the control devices can be valves. The function of the mass flow meter 2 is to control the concentration and flow rate of the inert gas and / or the reaction gas. The gas source is sequentially transmitted to the gas circulation chamber through the mass flow meter and the air inlet, and flows out from the air outlet, and the air outlet is connected to the tail gas treatment module ( Figure 2 The tail gas treatment module is used to store and process the acquired gas; the in-situ gas flow cell is used to provide a reaction channel between the reaction gas and the reaction sample, and to maintain and control the reaction temperature of the reaction sample.
[0063] In one embodiment, Figure 2 As shown, the infrared optical imaging module may include a short-wave infrared camera 3, and the in-situ gas circulation pool 4 may also include an infrared optical window 6; the short-wave infrared camera 3 obtains an infrared image of the surface of the reaction sample placed in the metal oxide library substrate 8 located directly below the infrared optical window 6 through the infrared optical window 6.
[0064] The infrared optical window 6 may be a sapphire (Al 2 O 3 ) material, the wavelength range of the short-wave infrared region is: 0.9 microns-1.7 microns. You can also choose optical glass made of quartz material that can transmit short-wave infrared band.
[0065] In one embodiment, a data processing module is used to perform data analysis and kinetic model fitting on the received infrared images; the infrared optical imaging module is used to perform time-lapse photography of infrared optical imaging of each sample surface during the kinetics of the heterogeneous interface adsorption reaction to obtain infrared optical time series images, and the kinetic curve of the infrared response of the sample surface is extracted by the data processing module and used for different kinetic model analyses.
[0066] In one embodiment, the data processing module is specifically used to: extract the infrared signal response kinetic curve of each sample surface in the infrared image according to the time series; for the gas-solid reaction system, use the Langmuir adsorption kinetic equation or the heat dissipation kinetic equation to fit the kinetic data of each curve, and extract the gas-solid interface adsorption reaction kinetic rate constant; for the gas-liquid reaction system, use the heat dissipation kinetic equation to fit the data of each curve, and calculate the gas-liquid adsorption reaction enthalpy.
[0067] Figure 3 FIG. 1 is a schematic diagram of a specific example of an infrared imaging system in an embodiment of the present invention. Figure 3 As shown, the structure of the in-situ gas flow cell is further introduced below.
[0068] In-situ gas flow cell including heating stage ( Figure 3 7, 9, and 10 are respectively a part of the heating stage), and are arranged in the gas flow chamber ( Figure 3 The metal oxide library substrate 8 is placed in a heating platform (not shown).
[0069] In one embodiment, the heating platform is made of brass with a thermal conductivity higher than a preset thermal conductivity; the heating platform includes a ceramic heating rod and a thermocouple; the ceramic heating rod and the thermocouple are used to heat or cool the reaction sample in the metal oxide library substrate to a preset temperature, or maintain a constant temperature.
[0070] In this embodiment, if Figure 2 As shown, the heating platform body 10 can be a copper heating platform; the heating platform can also include a ceramic heating rod 9 and a thermocouple 7; the ceramic heating rod 9 and the thermocouple 7 are used to heat or cool the reaction sample in the metal oxide library substrate to a preset temperature, or maintain a constant temperature.
[0071] In one embodiment, Figure 2 As shown, the infrared imaging system may further include a temperature controller 5, which is connected to the ceramic heating rod 9 and is used to control the ceramic heating rod 9 to control the temperature rise and fall of the heating stage.
[0072] In one embodiment, the metal oxide library substrate is inert to the reaction gas; the infrared emissivity of the metal oxide library substrate is lower than a preset infrared emissivity; and the thermal conductivity of the metal oxide library substrate is higher than a preset thermal conductivity.
[0073] The metal oxide library substrate has an inert infrared response to the reaction gas, and should have a low infrared emissivity and good thermal conductivity. Taking the study of carbon monoxide gas and reaction sample kinetics test as an example, the material selected for the metal oxide library substrate can be stainless steel with chrome plating on the surface; the metal oxide library substrate is used to fill a variety of metal oxide powders. 2Taking the thermodynamic test of the reaction between gas and alkaline solution as an example, the liquid sample plate (metal oxide library substrate) used has a low infrared emissivity.
[0074] In order to further study the changes in the infrared emission spectrum during the adsorption and desorption process of gas molecules on the material surface, the above-mentioned infrared imaging system was modified as follows: a short-wave infrared (spectrometric) spectrometer compatible with the imaging band of the short-wave infrared camera was connected to the front-end interface of the short-wave infrared camera, and an infrared optical lens was installed to converge and collect the infrared spectral lines emitted by the metal oxide surface. Figure 4 FIG. 1 is a schematic diagram of an infrared optical imaging module according to an embodiment of the present invention. Figure 4 As shown, in one embodiment, the infrared optical imaging module may include a short-wave infrared camera 11, a short-wave infrared spectrometer 12 and an infrared optical lens 13; the imaging band of the short-wave infrared spectrometer 12 matches the short-wave infrared camera 11; the photosensitive band of the short-wave infrared camera 11 is 0.9-1.7 microns; the infrared optical lens 13 is used to obtain the infrared light emitted from the surface of the reaction sample; the short-wave infrared spectrometer 12 is used to generate an infrared image based on the infrared light obtained by the infrared optical lens 13, and project the infrared image to the short-wave infrared camera 11.
[0075] In this embodiment, the short-wave infrared camera has a sensitive wavelength of 0.9-1.7 microns. In this wavelength, most gas molecules can be regarded as infrared heat-transmitting bodies, that is, the infrared transmittance can be regarded as 100%. The short-wave infrared camera can directly perform infrared imaging on the heated reaction sample without introducing additional light sources.
[0076] In one embodiment, Figure 4 As shown, in addition to directly using the short-wave infrared camera 11, a short-wave infrared spectrometer 12 matching its imaging band can be connected in front of the short-wave infrared camera 11 for infrared spectrum imaging analysis, and an infrared optical lens 13 can be connected to converge the infrared light emitted from the surface of the metal oxide powder. The short-wave infrared spectrometer 12 can be used to further record the time series spectra of the infrared spectrum of the reaction sample surface during the gas-solid interface reaction kinetics. The time series spectra are sent to the data processing module for data analysis, which can further analyze the changes in infrared emissivity and surface temperature of the metal oxide material surface during the reaction kinetics.
[0077] In order to realize in-situ online dynamic evolution observation, in one embodiment, the infrared optical imaging module is specifically used to acquire infrared images by time-delay shooting at a preset frame rate; the infrared images are image sequences; and the infrared images are sent to the data processing module in a time sequence.
[0078] Figure 5 The bright field image and infrared image of the metal oxide library substrate on which various reaction samples are placed in the embodiment of the present invention, wherein: Figure 5 (a) is a bright field image of a metal oxide library substrate on which a variety of reaction samples are placed at a certain moment in an embodiment of the present invention. Figure 5 (b) is an infrared image of a metal oxide library substrate with multiple reaction samples placed at a certain moment in an embodiment of the present invention. Figure 5 As shown in (a), stainless steel with low infrared emissivity is used as the metal oxide library substrate, and about 1 mg of metal oxide powder is filled into the substrate hole. A short-wave infrared (0.9 micron-1.6 micron) camera is used to monitor the infrared signal changes of the sample in the metal oxide library substrate in the high-temperature in-situ gas flow cell. The short-wave infrared imaging is shown in Figure 5 As shown in (b), under thermal equilibrium conditions, there are significant differences in infrared optical intensity between various reaction samples. The darker the color, the lower the infrared optical intensity of the reaction sample.
[0079] In one embodiment, when the reaction sample is a solid sample, the data processing module is specifically used to: extract a kinetic curve of the reaction sample surface in the infrared image according to the time series; the kinetic curve includes an adsorption kinetic curve and a desorption kinetic curve; the adsorption kinetic curve is an infrared image intensity curve during the process of adsorbing the reaction gas on the reaction sample surface; the desorption kinetic curve is an infrared image intensity curve during the process of desorbing the reaction gas on the reaction sample surface; the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the preset adsorption kinetic equation is determined by the Langmuir adsorption law; the gas-solid interface reaction equilibrium constant is determined based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process.
[0080] In this embodiment, an infrared optical imaging module is used to directly perform high-throughput infrared imaging on the gas-solid interface reaction process. The gas-solid interface reaction process mainly includes (taking the carbon monoxide reaction kinetics process as an example):
[0081] The infrared optical imaging module starts time-lapse photography at a certain frame rate to capture infrared images of the reaction sample in an inert nitrogen atmosphere as the baseline of the kinetic curve;
[0082] Start the gas adsorption process and switch the nitrogen atmosphere to a carbon monoxide gas atmosphere with a certain concentration;
[0083] When the surface of the metal oxide powder in the metal oxide library reaches adsorption saturation, the CO gas atmosphere of a certain concentration is switched to a nitrogen atmosphere, and the CO molecules adsorbed on the surface begin to desorb until the desorption is completely restored to the initial state;
[0084] The captured infrared images are sent to the data processing module in time series and the kinetic curves are extracted.
[0085] In one embodiment, the preset adsorption kinetic equation is:
[0086] ;
[0087] ;
[0088] Among them, R t is the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared radiation rate when the sample surface reaches the maximum adsorption state; ε 0 is the initial infrared radiation rate of the site on the surface of the reaction sample.
[0089] The data processing module extracts the infrared signal intensity of each reaction sample surface in the time series image captured by the infrared optical imaging module and obtains the gas-solid interface reaction kinetic curve. The Langmuir kinetic model is used to fit the data to obtain the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the kinetic characteristics are judged according to the fitting parameters; the gas-solid interface reaction equilibrium constant can be obtained based on the adsorption kinetic rate constant and desorption kinetic rate constant obtained by fitting.
[0090] In one embodiment, the data processing module is also used to: analyze the infrared image collected by the infrared spectrometer and projected on the infrared camera into an infrared spectrum; use a preset Planck blackbody radiation equation to perform data fitting on the infrared spectrum to determine the emissivity change characteristics and temperature change characteristics of the reaction sample surface; the preset Planck blackbody radiation equation is determined by Planck's blackbody radiation law.
[0091] The data processing module analyzes the infrared images collected by the short-wave infrared spectrometer and projected onto the short-wave infrared camera into infrared spectra; it uses the Planck blackbody radiation data model to fit the time series infrared spectra, and further analyzes the changing characteristics of the emissivity and temperature of the material surface during the reaction kinetics.
[0092] Compared with the oxygen vacancy characteristic detection technical solution of the metal oxide surface in the prior art, the embodiment of the present invention uses an in-situ reaction pool module, an infrared optical imaging module and a data processing module; the in-situ reaction pool module includes an in-situ gas circulation pool, a mass flow meter and a gas source; the in-situ gas circulation pool includes a gas circulation cavity, a heating platform, and a metal oxide library substrate arranged in the gas circulation cavity and placed on the heating platform; a plurality of holes for placing reaction samples are arranged on the metal oxide library substrate; the reaction sample includes a solid sample or a gas sample; the gas source is used to transmit the reaction gas to the gas circulation cavity of the in-situ gas circulation pool through the mass flow meter; the mass flow meter is used to control the concentration and flow rate of the reaction gas; the heating platform is used to heat the reaction sample; the infrared optical imaging module is used to obtain an infrared image of the reaction sample surface, and send the infrared image to the data processing module ; A data processing module is used to perform data analysis on the received infrared image and extract a kinetic curve from the infrared image; when the reaction sample is a solid sample, the data processing module is also used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or, to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve; when the reaction sample is a liquid sample, the data processing module is also used to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface, which can efficiently and high-throughput quantify the interaction between heterogeneous interfaces, realize the reaction kinetic measurement of metal oxide surfaces and gas molecules, and screen out high-performance CO from a large number of potential excellent absorbent formulations. 2 Absorbent.
[0093] In order to efficiently realize in-situ high-throughput measurement of gas molecule reaction kinetics on the surface of transition metal oxides, an embodiment of the present invention further provides a detection method based on an infrared imaging system, which is applied to the above infrared imaging system. Figure 6 FIG. 1 is a flow chart of a detection method based on an infrared imaging system in an embodiment of the present invention. Figure 6 As shown, the detection method based on the infrared imaging system may include:
[0094] Step 601, obtaining an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a gas sample;
[0095] Step 602, performing data analysis on the infrared image, and extracting a kinetic curve from the infrared image;
[0096] Step 603, when the reaction sample is a solid sample, a preset adsorption kinetic equation is used to fit the kinetic curve to determine the kinetic data of the reaction sample surface, and / or a heat dissipation kinetic equation is used to fit the kinetic curve to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve;
[0097] Step 604: When the reaction sample is a liquid sample, the kinetic curve is fitted using a heat dissipation kinetic equation to determine thermodynamic data on the surface of the reaction sample.
[0098] In step 601, an infrared image of the surface of a reaction sample is acquired using an infrared optical imaging module in an infrared imaging system.
[0099] In one embodiment, data analysis is performed on the infrared image, and a kinetic curve is extracted from the infrared image, which may include: extracting a kinetic curve of the reaction sample surface in the infrared image according to a time series; the kinetic curve includes an adsorption kinetic curve and a desorption kinetic curve; the adsorption kinetic curve is an infrared image intensity curve during the process of adsorbing reaction gas on the reaction sample surface; the desorption kinetic curve is an infrared image intensity curve during the process of desorbing reaction gas from the reaction sample surface.
[0100] In this embodiment, when the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, which may include: fitting the kinetic curve using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the preset adsorption kinetic equation is determined by the Langmuir adsorption law; and determining the gas-solid interface reaction equilibrium constant based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process.
[0101] In this embodiment, when the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, including: fitting the kinetic curve using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; determining the gas-solid interface reaction equilibrium constant based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process.
[0102] In one embodiment, the preset adsorption kinetic equation is:
[0103] ;
[0104] ;
[0105] Among them, R tis the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared radiation rate when the sample surface reaches the maximum adsorption state; ε 0 is the initial infrared radiation rate of the site on the surface of the reaction sample.
[0106] In one embodiment, the detection method based on the infrared imaging system may also include: parsing the infrared image into an infrared spectrum; performing data fitting on the infrared spectrum using a preset Planck blackbody radiation equation to determine the emissivity change characteristics and temperature change characteristics of the reaction sample surface; the preset Planck blackbody radiation equation is determined by Planck blackbody radiation law.
[0107] According to Planck's blackbody radiation law, we know that the infrared excitation E of an object is λ,T,ε Follow the equation:
[0108] ;
[0109] Among them, ε em is the infrared emissivity of the object surface; ε is the dielectric constant of the object in the infrared band; C 1 , C 2 is a constant, λ is the wavelength, and T is the absolute temperature.
[0110] Therefore, under isothermal conditions, the infrared emission intensity of an object is related to its surface infrared emissivity within a certain wavelength range. The difference in infrared emissivity of different materials can be explained based on the dielectric mechanism, that is, the infrared emissivity of different materials and their surface dielectric properties satisfy the following equation:
[0111] ;
[0112] Among them, ε em is the infrared emissivity of the object surface, and ε is the dielectric constant of the object in the infrared band.
[0113] Transition metal oxides are a class of semiconductor materials that are widely used in many fields. In the study of semiconductor materials, dielectric properties are a key parameter, which is closely related to carrier concentration and mobility. Many research results have pointed out that surface oxygen vacancy defects have a significant impact on the electronic structure and charge transport properties of semiconductors. In particular, when oxygen vacancies on the surface of metal oxides are occupied by active adsorbed oxygen and react with reducing gases such as carbon monoxide (CO), the local electronic structure and dielectric properties will be changed, thereby affecting the infrared emissivity of the material.
[0114] In one embodiment, the infrared camera can directly perform infrared imaging of each metal oxide powder in the metal oxide reservoir. During the reaction process of the reaction gas and the sample to be tested in the in-situ reaction pool, the infrared light on the sample surface passes through the infrared optical window and is collected and imaged on the infrared camera; the concentration and flow rate of the reaction atmosphere are controlled by a mass flow meter.
[0115] Take the reaction kinetics measurement of CO gas molecules and metal oxide powder as a specific case. When the reaction gas carbon monoxide is introduced into the in-situ reaction pool, the surface infrared intensity of the metal oxide changes due to the reaction of CO gas molecules with the surface of the metal oxide, and the infrared response characteristics of the metal oxide surface can be recorded in real time by an infrared camera. The specific experimental operation steps are as follows:
[0116] Step 1) Fill each hole of the metal oxide library substrate with about 1 mg of metal oxide sample and place it on a heating table, and seal the in-situ gas flow cell;
[0117] Step 2) Turn on the mass flow meter to introduce a nitrogen atmosphere at a certain flow rate to purge the in-situ gas flow cell until the in-situ gas flow cell is filled with a pure nitrogen inert atmosphere. Turn on the heating stage and the temperature control system to heat the metal oxide sample to a specified reaction temperature at a certain heating rate;
[0118] Step 3) maintaining the metal oxide sample at the reaction temperature, and turning on the short-wave infrared camera to start time-lapse photography at a certain shooting frequency, and the intensity of the infrared image recorded at this time is used as the intensity baseline;
[0119] Step 4) Gas adsorption process: the inert atmosphere in the in-situ gas flow cell is switched to a CO gas atmosphere of a certain concentration, the metal oxide sample surface begins to adsorb carbon monoxide gas molecules, and the infrared signal intensity begins to respond over time. The infrared image intensity curve recorded in this section is the adsorption kinetics curve;
[0120] Step 5) Gas desorption process: Pure nitrogen atmosphere is introduced to purge carbon monoxide gas molecules in the in-situ gas flow cell and on the surface of the metal oxide sample. As the carbon monoxide gas partial pressure decreases, the carbon monoxide molecules adsorbed on the surface of the metal oxide begin to desorb, and the infrared signal intensity begins to recover to the initial baseline intensity. The infrared image intensity curve recorded in this section is the desorption kinetic curve; this step also includes a metal oxide surface regeneration process, that is, continuing to maintain the nitrogen atmosphere purge and increasing the temperature to accelerate the gas desorption rate until the gas molecules adsorbed on the metal oxide surface are completely desorbed;
[0121] Step 6) Take step 3) - step 5) as one test cycle and repeat several cycles;
[0122] Step 7) The infrared response kinetic curves of the surfaces of the metal oxide powders in the infrared images recorded in steps 3) to 6) are fitted using the Langmuir kinetic model.
[0123] Figure 7 The kinetic curves of the reaction of carbon monoxide molecules with the surface of zinc oxide powder for multiple adsorption and desorption cycles and a partial enlarged view of the curves in the embodiment of the present invention are shown. Taking the kinetic characteristics of the reaction of zinc oxide powder with carbon monoxide molecules as an example, multiple cycles are tested according to the above steps. Figure 7 (a) is a kinetic curve of the reaction of carbon monoxide molecules with the surface of zinc oxide powder for multiple adsorption and desorption cycles in an embodiment of the present invention. Figure 7 As shown in (a), zinc oxide powder exhibits good repeatability in multiple adsorption and desorption cycles. The adsorption-desorption cycle reaction kinetic curve is a graph showing the relationship between the optical response (dimensionless) and time. Figure 7 The example in (a) is period-1 to period-3. Figure 7 (b) is an enlarged view of a portion of the curve of the reaction kinetic curve of multiple adsorption and desorption cycles between carbon monoxide molecules and the surface of zinc oxide powder in an embodiment of the present invention. Figure 7 As shown in (b), the rising part of the curve in cycle-1 is the adsorption process, the falling part is the desorption process, and the part where the optical response remains flat after 3000s is the high-temperature regeneration baseline.
[0124] In one embodiment, the detection method based on the infrared imaging system further includes:
[0125] The preset adsorption kinetic equation is determined according to the Langmuir adsorption law.
[0126] In one embodiment, the preset adsorption kinetic equation is:
[0127] ;
[0128] ;
[0129] Among them, R t is the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared radiation rate when the sample surface reaches the maximum adsorption state; ε 0 is the initial infrared radiation rate of the site on the surface of the reaction sample.
[0130] In one embodiment, after extracting the kinetic curve from the infrared image, different analysis methods can be used for the kinetic curve according to the difference between the gas-solid interface reaction system and the gas-liquid reaction system:
[0131] For the gas-solid interface reaction system, the extracted infrared response kinetic curves are fitted with a batch Langmuir kinetic model to obtain the adsorption-desorption reaction kinetic rate constant and the reaction equilibrium constant; for the gas-liquid reaction system, the extracted infrared response kinetic curves are fitted with a batch heat dissipation kinetic model, and the reaction enthalpy is further calculated.
[0132] In one embodiment, the Langmuir adsorption law is widely used to describe the chemical adsorption process at a multiphase interface, and the adsorption reaction equation of the adsorption process is:
[0133] (1)
[0134] Where A, B and AB represent adsorbed molecules, adsorption sites and adsorption binding substances, respectively. According to the Langmuir adsorption hypothesis, all adsorption sites on the material surface are equivalent and there is no interaction between adsorbate molecules. Therefore, the material surface can be divided into several independent adsorption sites. When a gas molecule occupies an adsorption site on the surface of a material, it is assumed that the initial infrared emissivity of the site is ε 0 , the infrared radiation rate of gas molecules after adsorption becomes ε i , so the adsorption coverage of gas molecules on the material surface is θ n It can be described as:
[0135] (2)
[0136] Where n represents the number of adsorption vacancies occupied by adsorbed molecules, m represents the total amount of adsorption vacancies on the material surface, and Δε nis the change in infrared emissivity of the material surface, Δε m It is the change value of infrared radiation rate when the material surface reaches the maximum adsorption state. The response value of infrared signal R t and gas molecule coverage θ t There are the following relationships;
[0137] (3)
[0138] The differential equation for gas-solid interface adsorption kinetics has the following form:
[0139] (4)
[0140] Among them, Q reflects the weights contributed by the pseudo-first-order and pseudo-second-order kinetic models. When the Q value approaches 0, the adsorption kinetics as a whole exhibits pseudo-first-order kinetic characteristics; when the Q value approaches 1, the adsorption kinetics exhibit pseudo-second-order kinetic characteristics; ε 0 is the initial infrared radiation rate of the sample surface site, ΔI t is the change of infrared optical intensity over time; Δε t is the infrared radiation rate changing with time; I 0 is the infrared optical intensity at the initial state; ka is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m It is the change in infrared radiation rate when the sample surface reaches the maximum adsorption state.
[0141] The apparent pseudo-first-order kinetic constant is denoted as k 1 =k a p i / θ e , the apparent pseudo-second-order kinetic constant is denoted as k 2 =k a p i / θ e 2 , k a is the intrinsic adsorption kinetic constant, p i is the gas partial pressure, θ and θ e are adsorption coverage and equilibrium adsorption coverage respectively, and t is the time. The above equation is integrated:
[0142] (5)
[0143] in,
[0144] (6)
[0145] Substituting the Langmuir kinetic equation (5) into equation (3), the adsorption kinetic equation related to the infrared optical response value can be obtained:
[0146] (7)
[0147] The kinetic curve fitting involved in the present invention is all fitted using the mathematical model of formula (7) above. The adsorption kinetic constant k can be obtained by performing kinetic fitting on the adsorption process and the desorption process respectively. a and the desorption kinetic constant k d .
[0148] In one embodiment, the apparent pseudo-first-order kinetic constant for the adsorption process is experimentally determined as k 1 Depends on the gas partial pressure p i ,
[0149] (8)
[0150] The desorption process response kinetic constant k' 1 =k d To accurately measure the adsorption kinetic constant k of gas on the material surface a and the desorption kinetic constant k d The embodiment of the present invention tests the adsorption-desorption response kinetic constants of the metal oxide surface under different gas partial pressures.
[0151] Figure 8 The kinetic curves of the surfaces of zinc oxide powder and tungsten trioxide powder and the correlation diagram between the apparent response kinetic constant and the partial pressure of carbon monoxide gas in the embodiment of the present invention are shown in FIG. Figure 8 (a) is a kinetic curve diagram of the surface of zinc oxide powder in an embodiment of the present invention; Figure 8 (b) is a graph showing the correlation between the apparent response kinetic constant of the zinc oxide powder surface and the partial pressure of carbon monoxide gas in an embodiment of the present invention. Figure 8 (c) is a kinetic curve diagram of the surface of tungsten trioxide powder in an embodiment of the present invention. Figure 8 (d) is a graph showing the correlation between the apparent response kinetic constant of the tungsten trioxide powder surface and the partial pressure of carbon monoxide gas in the embodiment of the present invention. Figure 8 As shown, zinc oxide (ZnO) and tungsten trioxide (WO 3 ), the apparent response kinetic constants during the adsorption process under different carbon monoxide gas partial pressures k 1 Linear dependence on the gas partial pressure p i The corresponding Langmuir kinetic equation fitting results are shown in Table 1 below.
[0152] Table 1
[0153]
[0154] For the equilibrium adsorption process, the equilibrium adsorption intensity constant K can be defined as:
[0155] (9)
[0156] From the experimental results in Table 1, it can be seen that the fitting parameter Q of zinc oxide (ZnO) is close to 0, showing a typical first-order adsorption kinetic behavior, while tungsten trioxide (WO 3 )The fitting parameter Q approaches 1, showing typical second-order adsorption kinetic behavior. The kinetic measurement results show that the response kinetic constant of the adsorption process is linearly correlated with the gas concentration, while the response kinetic constant of the desorption process is independent of the initial gas concentration. Therefore, according to formula (8), we can accurately measure the intrinsic adsorption rate constant and intrinsic desorption rate constant of metal oxides.
[0157] In one embodiment, a short-wave infrared camera is used to simultaneously record infrared images of gas molecules adsorption and desorption processes on the surfaces of multiple reaction samples. Fig. 9 It is a schematic diagram of the infrared intensity change images of the surfaces of multiple reaction samples and the kinetic curves and fitting curves of the reaction samples in the metal oxide library substrate in the embodiment of the present invention. Fig. 9 (a) is an image of the infrared intensity variation of the surfaces of multiple reaction samples in an embodiment of the present invention. Fig. 9 As shown in (a), the infrared intensity change image is a time series of multiple images. Fig. 9 (b) is a schematic diagram of the reaction sample kinetic curve and fitting curve in the metal oxide library substrate in the embodiment of the present invention. The reaction sample includes: WO 3 、In 2 O 3 SnO 2 Cr 2 O 3 , Fe 3 O 4 、TiO 2 (Anatase), CeO 2 , ZnO, TiO 2 (Rutile), MoO 3 , α-Fe 2 O 3 、V2O 5 For example, the infrared response kinetic curve (the response value R of the infrared signal) is extracted in batches through the data processing module. t The relationship curve between the two time) and data fitting are performed, and the results are as follows Fig. 9 The kinetic data of each reaction sample of the metal oxide library substrate measured in the experiment are shown in Table 2.
[0158] Table 2
[0159]
[0160] According to the kinetic measurement results, ZnO, SnO 2 、In 2 O 3 It exhibits typical pseudo-first-order adsorption kinetics (Q approaches 0), WO 3 、MoO 3 Cr 2 O 3 、V 2 O 5 It exhibits typical pseudo-secondary adsorption kinetic characteristics (Q approaches 1). The results of the adsorption kinetics of rutile powder surface show that its adsorption characteristics do not follow a simple pseudo-first-order model and a pseudo-second-order model. About 30% of the kinetic model contribution comes from the pseudo-second-order model, and about 70% of the kinetic model contribution comes from the pseudo-first-order model, indicating that there are carbonate intermediates with multiple adsorption modes, among which the proportion of monodentate carbonate intermediates is greater than that of bidentate carbonate intermediates. Another example is CeO 2 The contribution of the pseudo-secondary model to the adsorption pattern on the powder surface is greater than that of the pseudo-first-order model, indicating that the proportion of bidentate carbonate intermediates is greater than that of monodentate carbonate intermediates.
[0161] The equilibrium adsorption intensity constant K reflects the adsorption intensity of carbonate intermediates generated on the surface of metal oxides at this temperature (300°C). According to the measurement results, the adsorption intensity of carbonate intermediates generated on the surfaces of different metal oxides is in the following order: WO 3 > In 2 O 3 > SnO 2 > Cr 2 O 3 > Fe 3 O 4 > TiO 2 (Anatase) > CeO 2 > ZnO > TiO 2 (Rutile) > MoO 3 > α-Fe 2 O 3 > V2O 5 .
[0162] Fig.10 : is the near infrared spectrum and spectrum fitting curve diagram of carbon monoxide before and after adsorption on the zinc oxide surface in the embodiment of the present invention. The state before adsorption is the initial state, such as Fig.10As shown in the figure, the experimental observation is that the signal intensity of the material surface captured by infrared imaging in the initial state and the adsorption state has changed significantly. By comparing the near-infrared spectra before and after the adsorption of CO gas molecules, it is found that after CO combines with the oxygen adsorbed on the surface of the metal oxide, no obvious carbonate intermediate characteristic peak appears, but the overall infrared spectrum shifts. The optical signal intensity I recorded by the infrared imaging system λ,T Infrared excursion E with the material surface λ,T There are the following relations:
[0163] (10)
[0164] Where A is a parameter related to the infrared imaging system.
[0165] Fig.11 The near infrared spectrum evolution spectrum of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle and the surface infrared radiation rate a in the embodiment of the present invention are shown in FIG. ε Evolution kinetics graph. Fig.11 (a) is a near infrared spectrum evolution spectrum of carbon monoxide on the surface of zinc oxide during the adsorption and desorption cycle in an embodiment of the present invention. In one embodiment, an infrared optical intensity curve of carbon monoxide adsorption and desorption process on the surface of ZnO powder is recorded. Further, after carbon monoxide is saturated on the surface of ZnO powder, N is introduced. 2 The evolution of the near-infrared spectrum during the desorption process, such as Fig.11 As shown in (a).
[0166] The intensity of the emission spectrum on the surface of a material has the following relationship with the material's emissivity:
[0167] (11)
[0168] in, a e and b T They are parameters related to the material surface emissivity and the material surface temperature, C 1 , C 2 is a constant, l is the wavelength, T is the absolute temperature. Fitting the near-infrared spectral data recorded at different wavelengths, the initial state and adsorption state are as follows Fig.10 shown. Fig.11 (b) is the infrared radiation rate of carbon monoxide on the surface of zinc oxide during the adsorption and desorption cycle in the embodiment of the present invention. a e Evolution kinetics curve, extract the emissivity of the ZnO surface at a specific time from the fitting results ae , the kinetic curves of the changes in the radiation rate of metal oxides during adsorption and desorption were obtained, such as Fig.11 As shown in (b), the adsorption process is 0s~400s, and the desorption process is 400s~600s. In addition, Fig.12 The surface temperature kinetic curve of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle is shown in Figure 2. b T (Unit is K) The curves during adsorption and desorption are as follows Fig.12 As shown, the adsorption process is 0s~400s, and the desorption process is 400s~600s. The characteristics of the temperature kinetic curve show that the temperature fluctuation is small during the adsorption and desorption process, so it can be regarded as a thermal equilibrium process. Fig.13 This is a correlation diagram of the surface emissivity and the surface radiation infrared signal intensity of carbon monoxide on the zinc oxide surface during the adsorption and desorption cycle in the embodiment of the present invention, and the infrared optical intensity and the emissivity a e The original data and linear fitting curve are as follows Fig.13 As shown in the figure, the optical intensity of short-wave infrared imaging is equivalent to the integral of the near-infrared spectrum intensity. Therefore, in the adsorption state, the infrared optical intensity is proportional to the radiance. a e This shows that infrared imaging technology has the ability to perform high-throughput kinetic measurements.
[0169] Fig.14 It is a bright field image, infrared image, kinetic curve diagram of temperature change during adsorption of carbon dioxide molecules and organic amine alkali solutions of different concentrations in the embodiment of the present invention, and a temperature rise process diagram of an ideal adiabatic system during the reaction process after kinetic fitting; Fig.14 (a) is a bright field image of a sample library of organic amine alkali solutions with different ratios and concentrations in an embodiment of the present invention. In one embodiment, for the study of thermal temperature kinetics of adsorption at the gas-liquid interface, the infrared imaging system uses a resin plate with a relatively low infrared emissivity to fill the CO 2 Adsorption of organic amine alkali, such as Fig.14 As shown in (a) in the figure. Fig.14 In (a), #1, #2, #3, #4, #5, and #6 are used as examples for introduction.
[0170] Fig.14 (b) is an infrared image of a sample library of organic amine alkali solutions with different ratios and concentrations in an embodiment of the present invention. The infrared camera can directly perform infrared imaging on the temperature data of organic amine alkali solutions with different ratios and concentrations in the metal oxide library substrate. The infrared images of the sample library of organic amine alkali solutions with different ratios and concentrations are shown in FIG. Fig.14 As shown in (b), the infrared optical intensity increases from low to high, and the color in the infrared image increases from dark to light.2 The exothermic kinetic measurement of the reaction between gas molecules and organic amine alkali solution is used as a specific example. When the reaction gas carbon dioxide is introduced into the in-situ gas flow cell, the CO2 gas molecules react with the surface of the organic amine alkali solution and release heat, causing the temperature to rise, resulting in a response of the infrared intensity of the surface. Fig.14 (c) is a kinetic curve diagram of temperature change during the adsorption of carbon dioxide molecules and organic amine alkali solutions of different concentrations in the embodiment of the present invention. The infrared response characteristics of the alkali solution surface can be recorded in real time by an infrared camera. The infrared thermal imaging temperature response curves of the alkali solution surfaces #1, #2, #3, #4, #5, and #6 are shown in FIG. Fig.14 As shown in (c). The specific experimental steps are as follows:
[0171] Step 1) Encapsulate organic amine alkali solutions with different ratios and concentrations in an in-situ gas flow cell.
[0172] Step 2) Open the mass flow meter to introduce a nitrogen atmosphere at a certain flow rate to purge the in-situ gas flow cell until the in-situ gas flow cell is maintained in a pure nitrogen inert atmosphere.
[0173] Step 3) Keep the sample to be tested at the reaction temperature, and turn on the infrared camera to start time-lapse photography at a certain shooting frequency. The intensity of the infrared image recorded at this time is used as the intensity baseline.
[0174] Step 4) Gas reaction process: Switch the inert atmosphere in the in-situ gas flow cell to a certain concentration of CO 2 In the gas atmosphere, the surface of the alkali solution begins to adsorb carbon dioxide gas molecules, reacts and releases heat to start heating up, and the infrared signal intensity begins to respond over time. The infrared image intensity curve recorded in this section is the kinetic curve of the temperature rise during the reaction process.
[0175] Step 5) Reaction end process: As the reaction continues, the alkali solution is gradually consumed, the reaction rate decreases, the heat released is less than the heat dissipated by the system into the air, the system temperature begins to drop, and after the reaction is completely finished, it returns to the baseline stage. This is a complete reaction process.
[0176] Step 6) Recording the solution cooling process: In addition to the process of step 4-step 5, a liquid with a certain temperature higher than room temperature is added to the in-situ gas circulation pool, and the infrared camera is turned on to record the changes in the infrared signal during the temperature drop process.
[0177] Step 7) Fit the temperature with the temperature drop rate in step 6 to obtain the temperature drop rate caused by heat dissipation at different temperatures.
[0178] Step 8) Based on the kinetic curves obtained in steps 4-5 and taking the temperature dissipation obtained in step 7 as the processing condition, the temperature data in the reaction is analyzed to obtain the temperature rise of an ideal adiabatic system without heat dissipation.
[0179] Fig.14 (d) is a temperature rise process diagram of an ideal adiabatic system in the reaction process after kinetic fitting of the adsorption process of carbon dioxide molecules and organic amine alkali solutions of different concentrations in an embodiment of the present invention. In one embodiment, the temperature drop curve obtained in the above process with respect to time is derived, and then the obtained cooling rate value is fitted to the temperature value. The temperature change curves of the simulated adiabatic systems on the surfaces of organic amine alkali solutions #1, #2, #3, #4, #5, and #6 are shown in FIG. Fig.14 As shown in (d), the heat dissipation coefficient of the corresponding organic amine alkali solution transferring temperature to the environment in this temperature range is obtained. The fitting equation used in the fitting process is:
[0180] (12)
[0181] The coefficient h 1 It represents the coefficient of heat dissipation caused by heat transfer and convection from organic amine alkali solution to the surrounding environment, and the unit is J·(K·s) -1 ;h 2 The coefficient representing the heat dissipation process caused by the alkali solution radiating heat to the surrounding environment, with the unit of J·(K 4 ·s) -1 ; T is the real-time temperature; T 0 is the ambient temperature of the solution, in °C; t is the time, in seconds.
[0182] After obtaining the heat dissipation equation, the kinetic curve of temperature change is processed. The temperature value at each moment is accumulated with the temperature drop due to heat dissipation at all previous moments to obtain the theoretical temperature change of the system under the simulated adiabatic system.
[0183] By simulating the temperature rise obtained by a complete reaction in an adiabatic system, combined with the heat capacity of the system and the known properties of the solution, the reaction heat in the solution reaction process can be calculated. The calculation formula is as follows:
[0184] (13)
[0185] Where c is the heat capacity of the system, in J·K -1 ;M r is the mass fraction of the organic amine alkali substance reacting in the solution; To calculate the final temperature rise value in the simulated adiabatic system, the unit is K; V is the volume of the organic amine alkali solution added to the in-situ reaction tank, the unit is ml; is the heat of reaction of organic amine alkali solution, in kJ / ml.
[0186] Determination of different alkaline solutions CO 2 The absorption reaction heat values are shown in Table 3 below.
[0187] Table 3
[0188]
[0189] The present invention also provides a detection device based on an infrared imaging system, as described in the following embodiments. Since the principle of the device to solve the problem is similar to that of the detection method based on the infrared imaging system, the implementation of the device can refer to the implementation of the detection method based on the infrared imaging system, and the repeated parts will not be repeated.
[0190] Fig.15 FIG. 1 is a structural block diagram of a detection device based on an infrared imaging system in an embodiment of the present invention. Fig.15 As shown, the detection device based on the infrared imaging system includes the above-mentioned infrared imaging system and may further include:
[0191] The acquisition module 1501 is used to acquire an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a gas sample;
[0192] The data analysis module 1502 is used to perform data analysis on the infrared image and extract a kinetic curve from the infrared image;
[0193] The kinetic data determination module 1503 is used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the surface of the reaction sample when the reaction sample is a solid sample, and / or to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the surface of the reaction sample; the kinetic curve is an infrared image intensity curve;
[0194] Thermodynamic data determination module 1504 is used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the surface of the reaction sample when the reaction sample is a liquid sample.
[0195] In one embodiment, the detection device based on the infrared imaging system may further include: an image analysis module for:
[0196] Analyze infrared images into infrared spectra;
[0197] The infrared spectrum is fitted using a preset Planck blackbody radiation equation to determine the emissivity change characteristics and temperature change characteristics of the reaction sample surface; the preset Planck blackbody radiation equation is determined by Planck's blackbody radiation law.
[0198] In one embodiment, the data analysis module 1502 is specifically configured to:
[0199] Extracting a kinetic curve of the reaction sample surface in the infrared image according to the time series; the kinetic curve includes an adsorption kinetic curve and a desorption kinetic curve; the adsorption kinetic curve is an infrared image intensity curve during the process of adsorbing the reaction gas on the reaction sample surface; the desorption kinetic curve is an infrared image intensity curve during the process of desorbing the reaction gas on the reaction sample surface;
[0200] When the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data on the surface of the reaction sample, including:
[0201] The kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the preset adsorption kinetic equation is determined by the Langmuir adsorption law; based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process, the gas-solid interface reaction equilibrium constant is determined.
[0202] In one embodiment, the preset adsorption kinetic equation is:
[0203] ;
[0204] ;
[0205] Among them, R t is the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared radiation rate when the sample surface reaches the maximum adsorption state; ε 0 is the initial infrared radiation rate of the site on the surface of the reaction sample.
[0206] Based on the above invention concept, Fig.16As shown, the present invention also proposes a computer device 1600, including a memory 1610, a processor 1620, and a computer program 1630 stored in the memory 1610 and executable on the processor 1620, wherein the processor 1620 implements the aforementioned detection method based on the infrared imaging system when executing the computer program 1630.
[0207] Based on the aforementioned inventive concept, the present invention proposes a computer-readable storage medium, wherein the computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the aforementioned detection method based on the infrared imaging system is implemented.
[0208] Based on the aforementioned inventive concept, the present invention proposes a computer program product, wherein the computer program product comprises a computer program, and when the computer program is executed by a processor, a detection method based on an infrared imaging system is implemented.
[0209] The embodiment of the present invention proposes a method for realizing in-situ high-throughput measurement of gas molecule reaction kinetics on transition metal oxide surfaces using infrared imaging technology. Through the fitting of the Langmuir adsorption kinetic model, it is possible to distinguish the adsorption patterns of gas molecules on different metal oxide surfaces and quantitatively measure the binding kinetics and dissociation kinetics of adsorbed oxygen and gas molecules on different metal oxide surfaces as well as the reaction equilibrium constant. This technology not only provides a new way to efficiently monitor the evolution kinetics of adsorbed oxygen on metal oxide surfaces, but also brings new perspectives to the research in the fields of catalysis and sensing.
[0210] The embodiment of the present invention provides a method for realizing in-situ high-throughput analysis of organic amine alkali solution and CO by using infrared imaging technology. 2 Reaction heat analysis. Data analysis was performed using a heat dissipation kinetic model, and the differences in reaction enthalpy between different alkali solution formulations were further calculated. This technology is expected to be used as a high-throughput strategy for large-scale screening of potential excellent CO 2 Absorbent.
[0211] It will be appreciated by those skilled in the art that embodiments of the present invention may be provided as methods, systems, or computer program products. Therefore, the present invention may take the form of a complete hardware embodiment, a complete software embodiment, or an embodiment combining software and hardware. Furthermore, the present invention may take the form of a computer program product implemented on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) containing computer-usable program code.
[0212] The present invention is described with reference to flowcharts and / or block diagrams of methods, devices (systems), and computer program products according to embodiments of the present invention. It should be understood that each process and / or block in the flowchart and / or block diagram, as well as the combination of processes and / or blocks in the flowchart and / or block diagram, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, a special-purpose computer, an embedded processor, or other programmable data processing device to generate a machine, so that the instructions executed by the processor of the computer or other programmable data processing device generate instructions for implementing the processes in the flowchart and / or block diagram. Figure 1 A process or multiple processes and / or boxes Figure 1 A device that provides the functions specified in a block or multiple blocks.
[0213] These computer program instructions may also be stored in a computer-readable memory capable of directing a computer or other programmable data processing device to operate in a specific manner, so that the instructions stored in the computer-readable memory produce an article of manufacture comprising an instruction device, which implements the process Figure 1 A process or multiple processes and / or boxes Figure 1 A function specified in one or more boxes.
[0214] These computer program instructions can also be loaded onto a computer or other programmable data processing device so that a series of operating steps are executed on the computer or other programmable device to produce a computer-implemented process, thereby providing instructions for implementing the process. Figure 1 A process or multiple processes and / or boxes Figure 1 The steps for the functions specified in one or more boxes.
[0215] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. An infrared imaging system, characterized in that: include: In-situ reaction cell module, infrared optical imaging module and data processing module; The in-situ reaction pool module includes an in-situ gas circulation pool, a mass flow meter and a gas source; the in-situ gas circulation pool includes a gas circulation chamber, a heating platform, and a metal oxide library substrate arranged in the gas circulation chamber and placed on the heating platform; the metal oxide library substrate is provided with a plurality of holes for placing reaction samples; the reaction samples include solid samples or liquid samples; the gas source is used to transmit the reaction gas to the gas circulation chamber of the in-situ gas circulation pool through the mass flow meter; the mass flow meter is used to control the concentration and flow rate of the reaction gas; the heating platform is used to heat the reaction sample; The infrared optical imaging module is used to obtain an infrared image of the surface of the reaction sample and send the infrared image to the data processing module; The data processing module is used to perform data analysis on the received infrared image and extract a kinetic curve from the infrared image; When the reaction sample is a solid sample, the data processing module is further used to fit the kinetic curve using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or to fit the kinetic curve using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve; When the reaction sample is a liquid sample, the data processing module is further used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface.
2. The infrared imaging system according to claim 1, characterized in that: The in-situ gas circulation cell also includes an infrared optical window; the infrared optical window is used to allow the infrared light emitted from the surface of the reaction sample to emit out of the in-situ gas circulation cell; the infrared optical window is made of a material whose transmittance in the short-wave infrared region is greater than a preset transmittance; the metal oxide library substrate is located directly below the infrared optical window.
3. The infrared imaging system according to claim 1, characterized in that: The gas circulation chamber is provided with an air inlet and an air outlet; wherein the gas source is sequentially transmitted to the gas circulation chamber through the mass flow meter and the air inlet; the air outlet is connected to an exhaust gas treatment module; the exhaust gas treatment module is used to store and process the acquired gas; the in-situ gas circulation pool is used to provide a reaction channel for the reaction gas and the reaction sample.
4. The infrared imaging system according to claim 1, characterized in that: The infrared optical imaging module includes a short-wave infrared camera; the photosensitivity band of the short-wave infrared camera is 0.9 microns-1.7 microns; the short-wave infrared camera is used to obtain an infrared image of the surface of the reaction sample without introducing an additional light source.
5. The infrared imaging system according to claim 4, characterized in that: The infrared optical imaging module also includes: a short-wave infrared spectrometer and an infrared optical lens; the imaging band of the short-wave infrared spectrometer matches the short-wave infrared camera; The infrared optical lens is used to obtain infrared light emitted from the surface of the reaction sample; The short-wave infrared spectrometer is used to generate an infrared image according to the infrared light obtained by the infrared optical lens, and project the infrared image to the short-wave infrared camera.
6. The infrared imaging system according to claim 5, characterized in that: The data processing module is further used for: The infrared image collected by the infrared spectrometer and projected onto the infrared camera is analyzed into an infrared spectrum graph; The infrared spectrum is fitted using a preset Planck blackbody radiation equation to determine the emissivity change characteristics and temperature change characteristics of the reaction sample surface; the preset Planck blackbody radiation equation is determined by Planck's blackbody radiation law.
7. The infrared imaging system according to claim 1, characterized in that: The infrared optical imaging module is specifically used for delayed shooting according to a preset frame rate to obtain infrared images; the infrared images are image sequences; and the infrared images are sent to the data processing module according to a time sequence.
8. The infrared imaging system according to claim 7, characterized in that: When the reaction sample is a solid sample, the data processing module is specifically used for: Extracting a kinetic curve of the reaction sample surface in the infrared image according to the time series; the kinetic curve includes an adsorption kinetic curve and a desorption kinetic curve; the adsorption kinetic curve is an infrared image intensity curve during the process of adsorbing the reaction gas on the reaction sample surface; the desorption kinetic curve is an infrared image intensity curve during the process of desorbing the reaction gas on the reaction sample surface; The kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the preset adsorption kinetic equation is determined by the Langmuir adsorption law; The equilibrium constant of the gas-solid interface reaction is determined based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process.
9. The infrared imaging system according to claim 8, characterized in that: The preset adsorption kinetic equation is: ; ; ; Among them, R t is the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared emissivity of the reaction sample surface when it reaches the maximum adsorption state; ε0 is the initial infrared emissivity of the site on the reaction sample surface.
10. The infrared imaging system according to claim 1, characterized in that: The metal oxide library substrate is inert to the reaction gas; the infrared emissivity of the metal oxide library substrate is lower than the preset infrared emissivity; and the thermal conductivity of the metal oxide library substrate is higher than the preset thermal conductivity.
11. The infrared imaging system according to claim 1, characterized in that: The heating platform is made of brass with a thermal conductivity higher than a preset thermal conductivity; the heating platform includes a ceramic heating rod and a thermocouple; the ceramic heating rod and the thermocouple are used to heat or cool the reaction sample in the metal oxide library substrate to a preset temperature, or to maintain a constant temperature.
12. A detection method based on an infrared imaging system, characterized in that: The infrared imaging system according to any one of claims 1 to 11 comprises: Acquire an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a liquid sample; Perform data analysis on infrared images and extract kinetic curves from them; When the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data of the reaction sample surface, and / or the kinetic curve is fitted using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface; the kinetic curve is an infrared image intensity curve; When the reaction sample is a liquid sample, the kinetic curve is fitted using a heat dissipation kinetic equation to determine the thermodynamic data of the reaction sample surface.
13. The detection method based on the infrared imaging system according to claim 12, characterized in that: Also includes: Analyze infrared images into infrared spectra; The infrared spectrum is fitted using a preset Planck blackbody radiation equation to determine the emissivity change characteristics and temperature change characteristics of the reaction sample surface; the preset Planck blackbody radiation equation is determined by Planck's blackbody radiation law.
14. The detection method based on the infrared imaging system according to claim 12, characterized in that: Perform data analysis on infrared images and extract kinetic curves from them, including: Extracting a kinetic curve of the reaction sample surface in the infrared image according to the time series; the kinetic curve includes an adsorption kinetic curve and a desorption kinetic curve; the adsorption kinetic curve is an infrared image intensity curve during the process of adsorbing the reaction gas on the reaction sample surface; the desorption kinetic curve is an infrared image intensity curve during the process of desorbing the reaction gas on the reaction sample surface; When the reaction sample is a solid sample, the kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic data on the surface of the reaction sample, including: The kinetic curve is fitted using a preset adsorption kinetic equation to determine the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process; the preset adsorption kinetic equation is determined by the Langmuir adsorption law; based on the kinetic rate constant of the adsorption process and the kinetic rate constant of the desorption process, the gas-solid interface reaction equilibrium constant is determined.
15. The detection method based on the infrared imaging system according to claim 14, characterized in that: The preset adsorption kinetic equation is: ; ; ; Among them, R t is the response value of the infrared signal; Q reflects the weights contributed by the pseudo-first-order kinetic model and the pseudo-second-order kinetic model. When the Q value approaches 0, the adsorption kinetic characteristics show pseudo-first-order kinetic characteristics, and when the Q value approaches 1, the adsorption kinetic characteristics show pseudo-second-order kinetic characteristics; t is the time; k a is the intrinsic adsorption kinetic constant; p i is the partial pressure of adsorbate gas; θ e is the equilibrium adsorption coverage; Δε m is the change in infrared emissivity of the reaction sample surface when it reaches the maximum adsorption state; ε0 is the initial infrared emissivity of the site on the reaction sample surface.
16. A detection device based on an infrared imaging system, characterized in that: The infrared imaging system according to any one of claims 1 to 11 further comprises: An acquisition module, used to acquire an infrared image of the surface of a reaction sample; the reaction sample includes a solid sample or a liquid sample; Data analysis module, used to analyze infrared images and extract kinetic curves from infrared images; A kinetic data determination module, for fitting a kinetic curve using a preset adsorption kinetic equation to determine kinetic data on the surface of the reaction sample when the reaction sample is a solid sample, and / or fitting the kinetic curve using a heat dissipation kinetic equation to determine thermodynamic data on the surface of the reaction sample; the kinetic curve is an infrared image intensity curve; The thermodynamic data determination module is used to fit the kinetic curve using the heat dissipation kinetic equation to determine the thermodynamic data of the surface of the reaction sample when the reaction sample is a liquid sample.
17. A computer device comprising a memory, a processor, and a computer program stored in the memory and executable on the processor, characterized in that: When the processor executes the computer program, the method according to any one of claims 12 to 15 is implemented.
18. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores a computer program, and when the computer program is executed by a processor, the method according to any one of claims 12 to 15 is implemented.
19. A computer program product, characterized in that The computer program product comprises a computer program, and when the computer program is executed by a processor, the method according to any one of claims 12 to 15 is implemented.
Citation Information
Patent Citations
Coal spontaneous combustion characteristic parameter determination experiment platform
CN111999343A
Method for predicting ignition condition of metal combustion
CN115184396A