An electro-thermal coupled in-situ diffuse reflectance infrared reaction device
By employing an insulating sample cell and an electrode sheet bonded to the inner wall in the in-situ diffuse reflection infrared reaction device, the structural modification and uneven contact issues caused by electrode introduction were resolved. This achieved stable electrical contact and gas tightness in the electro-thermal coupled catalytic reaction, improving the uniformity and safety of the catalytic reaction.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI
- Filing Date
- 2025-06-11
- Publication Date
- 2026-06-09
AI Technical Summary
Existing in-situ diffuse reflection infrared reaction devices require structural modifications when introducing electrodes, and suffer from uneven electrical contact and are prone to short circuits and gas leaks, making it difficult to meet the reliability requirements of electro-thermal coupled catalytic reactions.
The sample cell and inner wall are made of insulating material and the electrode sheet is attached to the inner wall. The electrode rod is connected to the observation window by sealing and fixing it on the top cover. This ensures stable electrical contact between the electrode and the catalyst in the sample cell. The sealant prevents the leakage of reaction gas, thus realizing in-situ infrared characterization of electro-thermal coupled catalytic reaction.
Stable electrical contact and gas tightness were achieved in the electro-thermal coupled catalytic reaction, avoiding short circuits and gas leakage problems, improving the uniformity of the catalytic reaction and experimental safety, and meeting the reliability requirements of complex catalytic reaction systems.
Smart Images
Figure CN224341429U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of infrared spectroscopy detection equipment technology, and more specifically, to an electro-thermal coupled in-situ diffuse reflection infrared reaction device. Background Technology
[0002] Diffuse reflectance infrared spectroscopy is a research method based on absorption and scattering, particularly suitable for determining the surface structure and adsorbed species of solid powder samples. This technique offers significant advantages in studying the microstructure and reactivity of materials, as well as exploring reaction mechanisms, and is an important method for researching catalytic reactions.
[0003] Currently, common in-situ diffuse reflectance infrared reaction devices can achieve temperature control for traditional thermocatalytic reactions, but they lack electro-thermal coupling capabilities. In catalysis research, electro-thermal coupling is an effective means to improve catalytic reaction efficiency. For example, applying an external electric field to a solid catalyst to assist the reaction, or directly driving the reaction using the electrothermal effect generated by current flowing through a solid catalyst, can alter the catalytic mechanism and significantly enhance the intrinsic activity of the catalyst.
[0004] To perform thermo-electric coupled catalytic reactions, patent CN115791672A discloses a reaction cell and an in-situ diffuse reflectance infrared detector. The electric field is applied by embedding electrodes and insulating pads within the reaction cell body. However, this structure requires destructive modification of the reaction cell body, which not only increases processing costs and complexity but also poses the risk of short circuits caused by contact between the electrodes and the reaction cell body, as well as the risk of reaction gas leakage. At the same time, this scheme uses a sieve plate to support the powdered catalyst, which cannot guarantee uniform electrical contact between the powder and the electrodes, and does not form an independent insulating space. This can easily lead to direct contact between the sample and the metal cell body, causing electrical short circuits, making it difficult to meet the reliability requirements of complex catalytic reaction systems. Utility Model Content
[0005] To address the shortcomings of existing technologies, this invention aims to solve the problems of structural modification required for electrode introduction, uneven electrical contact, and susceptibility to short circuits and gas leakage in existing in-situ diffuse reflection infrared reaction devices, in order to achieve in-situ diffuse reflection infrared characterization of the electro-thermal coupled catalytic reaction mechanism.
[0006] To achieve the above objectives, this utility model provides an electro-thermal coupled in-situ diffuse reflection infrared reaction device, comprising:
[0007] case;
[0008] A top cover is disposed on the top of the housing, forming a cavity between the top cover and the housing, and an observation window is provided on the top cover;
[0009] A sample cell is disposed within the cavity, and the sample cell is made of an insulating material;
[0010] Two electrode rods are inserted through the observation window and are sealed and fixedly connected to the observation window.
[0011] Two electrode plates are spaced apart within the sample cell and are attached to the inner wall of the sample cell. Each of the two electrode plates is electrically connected to the corresponding electrode rod via a wire.
[0012] This invention avoids the structural modifications required by existing devices to introduce electrodes by inserting an electrode rod through the top cover and sealing it with the observation window, along with electrode plates attached to the sample cell and inner wall. Simultaneously, the insulated sample cell isolates the catalyst sample from the electrical contact with the shell, allowing the electrode plates to form stable electrical contact with the catalyst sample in the sample cell. The sealed electrode rod prevents reaction gas leakage, thus effectively solving the problems of uneven electrical contact and easy short-circuit leakage in existing technologies, achieving in-situ infrared characterization of electro-thermal coupled catalytic reactions.
[0013] Furthermore, the gap between the electrode rod and the observation window is filled with sealant. The sealant fills the gap between the electrode rod and the observation window to prevent leakage of reactive gases, ensuring the airtightness of the chamber and experimental safety.
[0014] Furthermore, the observation window is made of quartz, and the sample cell is made of ceramic or quartz. The quartz observation window ensures infrared light transmittance, while the ceramic / quartz sample cell provides a high-temperature resistant insulating environment, ensuring compatibility between the electro-thermal coupling reaction and infrared characterization.
[0015] Furthermore, a positioning platform with a positioning groove is provided inside the housing, and the sample cell is embedded in the positioning groove. This positioning structure facilitates the positioning, installation, and removal of the sample cell, improving the ease of use of the device.
[0016] Furthermore, one side of the electrode sheet is provided with an adhesive layer, which is bonded to the inner wall of the sample cell. The electrode sheet is fixed by the adhesive layer, ensuring a stable connection between the electrode sheet and the sample cell.
[0017] Furthermore, the sample cell is a cylinder or cuboid with an open top. The sample cell has a regular structure, adaptable to catalysts of different shapes.
[0018] Furthermore, the two electrode plates are symmetrically mounted on the inner wall at opposite positions along the axis of the sample cell. This symmetrical mounting of the electrode plates ensures a uniform distribution of the electric field within the sample cell, optimizing the uniformity of the electro-thermal coupled catalytic reaction.
[0019] Furthermore, the top cover is hemispherical, and it is provided with a light incident window and a light exit window. The light incident window, the light exit window, and the observation window are arranged at equal angular intervals with the center of the top cover as the symmetrical point. The hemispherical top cover, together with the equally distributed light incident window, exit window, and observation window, ensures the symmetry of the infrared light path and improves the accuracy of in-situ diffuse reflection infrared detection.
[0020] Furthermore, a heating element is provided inside the shell. By heating the cavity with the heating element, the reaction temperature can be controlled.
[0021] Furthermore, the housing has a coolant channel inside its wall, and the housing is equipped with an inlet pipe and an outlet pipe, which are connected to the coolant channel. This achieves cooling of the housing and prevents overheating and damage to the infrared equipment.
[0022] Furthermore, the housing is equipped with an inlet pipe, an outlet pipe, and a vacuum pipe, which are connected to the cavity. This supports precise control of the reaction atmosphere (such as introducing reaction gas or creating a vacuum) to meet the needs of different catalytic reactions.
[0023] In summary, the present invention has the following advantages over the prior art:
[0024] (1) The present invention seals and fixes the electrode rod in the observation window and connects it with the electrode plate with the wire. It can form a stable electrical circuit without modifying the reaction device, thus avoiding short circuit and reaction gas leakage from the structure. At the same time, it does not interfere with the internal optical path and has the advantages of low modification cost and easy operation in the laboratory.
[0025] (2) This utility model uses an insulating sample cell and attaches an electrode sheet to the inner wall. Through the insulating isolation effect of the sample cell, the electrical contact between the test catalyst sample and the metal shell is completely eliminated, ensuring stable and uniform electrical contact.
[0026] (3) This invention can simultaneously power and heat the sample, and combined with in-situ diffuse reflectance infrared characterization technology, it provides a systematic solution for the study of electro-thermal coupled catalytic reaction mechanism. Attached Figure Description
[0027] Figure 1 This is a top view of the electro-thermal coupled in-situ diffuse reflection infrared reactive device in the embodiment.
[0028] Figure 2 This is a cross-sectional view of the electro-thermal coupled in-situ diffuse reflection infrared reaction device in the embodiment.
[0029] Figure 3 The images shown are in-situ diffuse reflectance infrared spectra recorded under different input electrical power in the examples.
[0030] Explanation of reference numerals in the attached figures:
[0031] 1-Shell, 11-Positioning stage, 12-Inlet pipe, 13-Outlet pipe, 2-Top cover, 21-Observation window, 22-Light incident window, 23-Light exit window, 24-Fixed flange, 3-Cavity, 31-Inlet pipe, 32-Outlet pipe, 33-Vacuum tube, 4-Sample cell, 51-First electrode rod, 52-Second electrode rod, 61-First electrode plate, 62-Second electrode plate, 71-First wire, 72-Second wire, 8-Heating element. Detailed Implementation
[0032] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. The components of the embodiments of this utility model described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.
[0033] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.
[0034] It should be noted that similar symbols and letters in the following figures indicate similar items; therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.
[0035] In the description of this utility model, it should be noted that the terms "upper", "lower", "left", "right", "inner", "outer", "front", "rear", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship that the utility model product is usually placed in during use. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.
[0036] Combination Figure 1 and Figure 2As shown, this embodiment discloses an electro-thermal coupled in-situ diffuse reflection infrared reaction device, including a housing 1 and a top cover 2 covering the top of the housing 1, forming a cavity 3 between the top cover 2 and the housing 1. The top cover 2 has an observation window 21 for observing the state inside the cavity 3. A first electrode rod 51 and a second electrode rod 52 pass through the observation window 21 and are sealed and fixedly connected to the observation window 21 to prevent leakage of reaction gas. One end of the electrode rod enters the cavity 3, and the other end is located in the external space. An insulating sample cell 4 is provided inside the cavity 3 for holding a catalyst sample. A first electrode plate 61 and a second electrode plate 62 are installed inside the sample cell 4, spaced apart and attached to the inner wall of the sample cell 4. The first electrode plate 61 and the second electrode plate 62 can form a stable electrical contact with the catalyst sample inside the sample cell 4. The insulating sample cell 4 isolates the catalyst sample from the electrical contact between the housing 1 and the sample cell 4. The first electrode plate 61 is electrically connected to the first electrode rod 51 via a first wire 71, and the second electrode plate 62 is electrically connected to the second electrode rod 52 via a second wire 72.
[0037] In this embodiment, a fixing flange 24 is provided at the bottom edge of the top cover 2, and bolt holes are provided on the fixing flange 24. The top cover 2 and the housing 1 are fixedly connected by bolts. A sealing gasket is provided between the fixing flange 24 and the housing 1 to ensure the airtightness of the cavity 3.
[0038] In some embodiments, two electrode rods are vertically inserted through the observation window 21, and the gap between the electrode rods and the observation window 21 is filled with sealant to prevent leakage of reactive gas and ensure the airtightness of the cavity 3.
[0039] In this embodiment, the housing 1 is also provided with an inlet pipe 31, an outlet pipe 32, and a vacuum pipe 33 that communicate with the cavity 3, supporting precise control of the reaction atmosphere and meeting the needs of different catalytic reactions. A heating element is provided inside the housing to control the reaction temperature; the heating element 8 is preferably an electric heating element.
[0040] The interior wall of the housing 1 has a coolant channel. The housing 1 is provided with an inlet pipe 12 and an outlet pipe 13. The inlet pipe 12 and the outlet pipe 13 are connected to the coolant channel. By introducing coolant, the housing 1 is cooled down to prevent it from overheating and damaging the infrared equipment.
[0041] In this embodiment, the top cover 2 is a hemispherical structure, with light incident windows 22, light exit windows 23, and observation windows 21 arranged at equal angular intervals around the center of the sphere to ensure symmetrical infrared light paths. The observation windows 21, light incident windows 22, and light exit windows 23 are preferably made of quartz to ensure infrared light transmittance.
[0042] In this embodiment, a positioning platform 11 is provided inside the housing 1. The positioning platform 11 has a positioning groove with an open top. The sample cell 4 is embedded in the positioning groove for easy positioning, installation, and disassembly. The sample cell 4 is a cuboid with an open top, made of quartz. The first electrode plate 61 and the second electrode plate 62 are installed on two opposite inner walls of the sample cell 4. Symmetrical installation allows the electric field to be evenly distributed within the sample cell 4. In other embodiments, the sample cell 4 has a cylindrical structure made of ceramic, which can accommodate catalysts of different shapes. The two electrode plates are symmetrically installed on opposite positions on the inner walls along the axis of the sample cell 4.
[0043] In some embodiments, an adhesive layer is provided on one side of the first electrode sheet 61 and the second electrode sheet 62. The adhesive layer is bonded to the inner wall of the sample cell 4 to ensure a stable connection between the electrode sheet and the sample cell 4 and to ensure stable and uniform electrical contact.
[0044] In the above-described embodiment of the electro-thermal coupled in-situ diffuse reflectance infrared reaction device, the catalyst sample is placed in the sample cell 4. The first electrode rod 51 and the second electrode rod 52 are respectively connected to an external power source. Current is conducted through the first wire 71 and the second wire 72 to the first electrode plate 61 and the second electrode plate 62 to form an electric field, allowing the current to flow through the conductive sample in the sample cell 4, thereby realizing the electro-thermal coupled catalytic reaction. In some embodiments, a heating element 8 is simultaneously used to heat the conductive sample. Infrared light irradiates the sample surface through the light incident window 22, and the reflected light enters the detection system through the light exit window 23. The observation window 21 is used to monitor the reaction status in real time. This device has the advantages of simple structure, uniform electrical contact, resistance to short circuits, and good airtightness, and can realize in-situ diffuse reflectance infrared characterization of the electro-thermal coupled catalytic reaction mechanism.
[0045] The function of the above-mentioned electro-thermal coupled in-situ diffuse reflectance infrared reaction device was verified as follows: An activated carbon catalyst (Ni-La / AC) co-loaded with nickel and lanthanum oxide was loaded into sample cell 4 and installed inside the infrared absorber. Argon gas containing methane and carbon dioxide was introduced into the chamber, with volume fractions of 1% and 2% for methane and carbon dioxide, respectively. An adjustable regulated DC power supply was connected to the first and second electrode rods respectively. The power was turned on, and the electrical power supplied to the catalyst was gradually increased, while the infrared absorption analyzer recorded the spectra during this process.
[0046] The results are as follows Figure 3 As shown, with the increase of electric power, the characteristic peaks of gaseous methane and carbon dioxide gradually weakened, and the characteristic peak of gaseous carbon monoxide appeared, indicating that a methane-carbon dioxide dry reforming reaction (CH4+CO2→2CO+2H2) occurred under the energized condition. Characteristic peaks of intermediate products, such as carboxylates and lanthanum oxycarbonate (La2O2CO3), were also observed.
[0047] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and not to limit it; although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.
Claims
1. An electro-thermal coupled in-situ diffuse reflection infrared reactive device, characterized in that, include: Shell (1); A top cover (2) is provided on the top of the housing (1), and a cavity (3) is formed between the top cover (2) and the housing (1). An observation window (21) is provided on the top cover (2). A sample cell (4) is disposed inside the cavity (3), and the sample cell (4) is made of insulating material; Two electrode rods (51, 52) are inserted through the observation window (21) and are sealed and fixedly connected to the observation window (21); Two electrode plates (61, 62) are spaced apart in the sample cell (4) and attached to the inner wall of the sample cell (4). The two electrode plates are electrically connected to the corresponding electrode rods (51, 52) through a wire (71, 72).
2. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The gap between the electrode rods (51, 52) and the observation window (21) is filled with sealant.
3. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The observation window (21) is made of quartz, and the sample cell (4) is made of ceramic or quartz.
4. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The housing (1) is provided with a positioning platform (11), the positioning platform (11) has a positioning groove, and the sample pool (4) is embedded in the positioning groove.
5. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, One side of the electrode sheet (61, 62) is provided with an adhesive layer, which is bonded to the inner wall of the sample cell (4).
6. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The sample cell (4) is a cylinder or cuboid with an open top.
7. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 6, characterized in that, The two electrode plates (61, 62) are symmetrically installed on the inner wall at opposite positions along the axis of the sample cell (4).
8. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The top cover (2) is hemispherical, and the top cover (2) is provided with a light incident window (22) and a light exit window (23). The light incident window (22), the light exit window (23) and the observation window (21) are arranged at equal angular intervals with the center of the top cover (2) as the symmetrical point.
9. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The housing (1) is provided with a heating element (8) inside, and the interior of the wall of the housing (1) has a coolant channel. The housing (1) is provided with an inlet pipe (12) and an outlet pipe (13), and the inlet pipe (12) and the outlet pipe (13) are connected to the coolant channel.
10. The electro-thermal coupled in-situ diffuse reflection infrared reaction device according to claim 1, characterized in that, The housing (1) is provided with an air inlet pipe (31), an air outlet pipe (32) and a vacuum pipe (33), and the air inlet pipe (31), the air outlet pipe (32) and the vacuum pipe (33) are connected to the cavity (3).