An attenuated total reflection in-situ infrared characterization system

Abstract

The utility model relates to a kind of attenuated total reflection in situ infrared characterization systems, and the system includes base plate, the crystal base being placed on base plate and the integrated heating body being connected together and placed on crystal base in situ infrared cell body. The outer wall of in situ infrared cell body is provided with in situ cell heat preservation layer;In situ infrared cell body is equipped with air inlet and air outlet, air inlet and air outlet penetrate in situ cell heat preservation layer;The top of integrated heating body is equipped with attenuated total reflection in situ cell top cover, and the attenuated total reflection in situ cell top cover is equipped with top cover heat preservation layer;Attenuated total reflection in situ cell top cover is equipped with pressure sensor, and pressure sensor passes through top cover heat preservation layer;In situ cell top cover is equipped with temperature control pressure measurement line, and temperature control pressure measurement line passes through top cover heat preservation layer and is connected with temperature control pressure measurement device. The utility model can realize the in situ observation of various substances, the purpose of dynamically tracking the phase change of catalyst in catalytic reaction process, can meet the characterization demand under the severe experimental condition of temperature, pressure change etc.

Description

Technical Field

[0001] This utility model relates to the field of in-situ infrared technology, and in particular to an attenuated total reflection in-situ infrared characterization system. Background Technology

[0002] Infrared spectroscopy is one of the key methods for qualitative identification of compounds and their structures. In particular, in-situ infrared spectroscopy not only reveals the static adsorption of various molecules on material surfaces, but also, under certain reaction conditions, allows for the study of adsorbed species types, structures, and bonding mechanisms, making it the most widely used characterization and identification tool in chemical research. As an important tool for identifying compounds and conducting molecular structure research, infrared spectrometers have wide applications in many fields, including chemistry, chemical engineering, petrochemicals, pharmaceutical chemistry, polymer materials research, biomedical research, and forensic identification.

[0003] Existing in-situ infrared spectroscopy techniques generally suffer from a narrow range of applications, with their characterization capabilities largely limited to monitoring gas-solid reaction systems. For more complex reaction systems such as gas-liquid-solid multiphase reactions and liquid-phase catalysis, they cannot conduct real-time and in-depth mechanistic studies of reactants during the dynamic reaction process. They struggle to accurately capture key intermediate signals and structural changes during the reaction, thus hindering the identification and exploration of reaction intermediate species. This severely impedes research progress in related fields, limits the breadth and depth of research, and restricts the development of research directions. Utility Model Content

[0004] The technical problem to be solved by this invention is to provide an attenuation total reflection in-situ infrared characterization system that enables in-situ observation of various substances and dynamic tracking of the phase changes of catalysts during catalytic reactions.

[0005] To address the aforementioned problems, this utility model provides an attenuated total internal reflection in-situ infrared characterization system, characterized in that: the system comprises a base plate, a crystal base placed on the base plate, and an in-situ infrared cell and an integrated heating element connected together on the crystal base; the outer wall of the in-situ infrared cell is provided with an in-situ cell insulation layer; the in-situ infrared cell is provided with an air inlet and an air outlet, which penetrate the in-situ cell insulation layer; the top of the integrated heating element is provided with an attenuated total internal reflection in-situ cell top cover, which is provided with a top cover insulation layer; a pressure sensor is provided on the attenuated total internal reflection in-situ cell top cover, and the pressure sensor passes through the top cover insulation layer; a temperature control and pressure measuring line is provided on the in-situ cell top cover, which passes through the top cover insulation layer and is connected to a temperature control and pressure measuring device.

[0006] The in-situ infrared cell is a hollow cylinder I; the outer wall of the cylinder I has four grooves I evenly distributed along its length, and each groove I has a fixing hole at its lower part; the top of the cylinder has four screw holes I evenly distributed; the air inlet and the air outlet are symmetrically arranged on the outer wall between two adjacent grooves I; the integrated heating element is inserted into the cavity of the cylinder I and passes through the crystal base to contact the base plate.

[0007] The crystal base is fitted into the center of the base plate.

[0008] The base plate is rectangular, with two positioning holes in the center. The center-to-center distance between the two positioning holes is 65mm, and they match the two positioning pins on the attenuating total reflection accessory (ATR). The outer diameter of the positioning pin is in clearance fit or transition fit with the inner diameter of the positioning hole.

[0009] The crystal base has a circular slot at its center, a slot at its bottom that matches the positioning hole in the base plate, and screw holes II at its four corners. The screw holes II match the screw holes I in the in-situ infrared cell. The integrated heating element is inserted into the circular slot and contacts the positioning hole in the base plate.

[0010] The in-situ pool insulation layer is a hollow cylinder II; the inner wall of the cylinder II has four grooves II evenly distributed along its length, each groove II matching the size of the groove I in the in-situ infrared pool and corresponding to it; the outer wall of the cylinder corresponding to the air inlet and the air outlet is provided with a through hole, and a through groove is provided above the through hole.

[0011] The top cover of the attenuated total reflection in-situ pool is respectively equipped with fixing screws V, VI, VII and VIII, which are inserted into the corresponding screw holes III on the insulation layer of the top cover.

[0012] The top cover insulation layer is respectively provided with fixing screw I, fixing screw II, fixing screw III and fixing screw IV, which are inserted into the corresponding screw hole IV on the top cover of the attenuated total reflection in-situ cell.

[0013] The air inlet is connected to an external gas cylinder.

[0014] The exhaust port is connected to the external exhaust gas.

[0015] This utility model has the following advantages compared with the prior art: 1. In this utility model, the crystal base is the core component, which can confine infrared light to a micron-level depth on the sample surface and collect surface signals such as adsorbed molecules on the catalyst surface and species on the carbon material surface. This fundamentally avoids the strong absorption and scattering interference of the solvent and the carbon material itself, and solves the problems of weak infrared signals and difficulty in identifying characteristic peaks in traditional infrared methods.

[0016] 2. The in-situ reaction cell in this invention provides a controllable gas-liquid environment for testing, and can inject different solvents and introduce reaction gases in real time to achieve simultaneous reaction and characterization, and dynamically track gas-liquid-solid reactions, thin film catalytic degradation and other processes.

[0017] 3. The system described in this utility model, in conjunction with an infrared spectrometer, further amplifies weak surface signals and improves the signal-to-noise ratio, ensuring accurate identification of key information such as active site types and surface chemical changes.

[0018] 4. This utility model is concentrated in three dimensions: environmental adaptability, surface specificity, and real-time tracking, and its advantages are realized through the collaborative design of core components. In terms of environmental adaptability, the crystal base is compatible with sample forms such as thin films, bulk catalysts, and carbon materials, as well as system types such as gas, liquid, and gas-liquid-solid, breaking the limitations of traditional infrared spectroscopy on testing scenarios; the surface specificity stems from the "surface focusing" characteristic of the crystal base, which can accurately remove bulk interference and capture only the surface species signals that are key to the reaction; the real-time tracking is jointly ensured by the controllable environment of the in-situ reaction cell and the high response speed of the infrared spectrometer, which can dynamically record the generation and disappearance of species in the reaction, providing continuous data for mechanism analysis.

[0019] 5. This invention not only enables precise control of reaction environment parameters under harsh conditions of dynamic temperature and pressure changes through the integration of temperature and pressure control modules, but also comprehensively adapts to various catalytic reaction scenarios such as gas-liquid-solid and liquid phase reactions. Simultaneously, the system dynamically tracks the phase changes of the catalyst during the catalytic reaction, thereby obtaining complete and accurate reaction data. This provides reliable characterization evidence for the study of material reaction mechanisms and catalyst performance analysis, and has extremely high application value in the scientific research field. Attached Figure Description

[0020] The specific embodiments of this utility model will be further described in detail below with reference to the accompanying drawings.

[0021] Figure 1 This is a schematic diagram of the structure of this utility model.

[0022] Figure 2 This is a schematic diagram of the in-situ infrared cell in this utility model.

[0023] Figure 3 This is a schematic diagram of the structure of the in-situ pool insulation layer in this utility model.

[0024] Figure 4This is a schematic diagram of the base plate in this utility model.

[0025] Figure 5 This is a schematic diagram of the structure of the attenuation total reflection in-situ pool top cover in this utility model.

[0026] Figure 6 This is a schematic diagram of the structure of the top cover insulation layer in this utility model.

[0027] Figure 7 This is a schematic diagram of the crystal base in this utility model.

[0028] Figure 8 This is a schematic diagram showing the completed installation of this utility model.

[0029] In the diagram: 1—Pressure sensor; 2—Top cover insulation layer; 3—Attenuated total reflection in-situ pool top cover; 4—Integrated heating element; 5—In-situ infrared pool body; 51—Groove I; 52—Fixing hole; 53—Screw hole I; 6—In-situ pool insulation layer; 61—Groove II; 62—Through hole; 63—Through groove; 7—Air inlet; 8—Air outlet; 9—Base plate; 91—Positioning hole; 10—Crystal base; 101—Screw hole II; 11—Temperature control and pressure measurement line; 12—Fixing screw I; 13—Fixing screw II; 14—Fixing screw III; 15—Fixing screw IV; 16—Fixing screw V; 17—Fixing screw VI; 18—Fixing screw VII; 19—Fixing screw VIII. Detailed Implementation

[0030] like Figures 1-8 As shown, an attenuated total reflection in-situ infrared characterization system includes a base plate 9, a crystal base 10 placed on the base plate 9, and an in-situ infrared cell 5 and an integrated heating element 4 connected together on the crystal base 10. The outer wall of the in-situ infrared cell 5 is provided with an in-situ cell insulation layer 6. The in-situ infrared cell 5 is provided with an air inlet 7 and an air outlet 8, which penetrate the in-situ cell insulation layer 6. The top of the integrated heating element 4 is provided with an attenuated total reflection in-situ cell top cover 3, which is provided with a top cover insulation layer 2. The attenuated total reflection in-situ cell top cover 3 is provided with a pressure sensor 1, which passes through the top cover insulation layer 2. The in-situ cell top cover 3 is provided with a temperature control and pressure measuring line 11, which passes through the top cover insulation layer 2 and is connected to a temperature control and pressure measuring device.

[0031] in: The temperature and pressure control device was provided by YUDIAN Technology Co., Ltd. (Beijing).

[0032] The integrated heating element 4 is provided by OPEANDO (Beijing) Technology Co., Ltd. The integrated heating element 4 enables precise temperature and pressure control of the sample within the chamber, and has the ability to provide real-time feedback of temperature and pressure.

[0033] The in-situ infrared pool body 5 is a hollow cylinder I; the outer wall of the cylinder I has four grooves I51 evenly distributed along its length, and each groove I51 has a fixing hole 52 at its lower part; the top of the cylinder has four screw holes I53 evenly distributed; the air inlet 7 and the air outlet 8 are symmetrically arranged on the outer wall between two adjacent grooves I51; the integrated heating element 4 is inserted into the cavity of the cylinder I and passes through the crystal base 10 to contact the base plate 9.

[0034] The crystal base 10 is fitted into the center of the base plate 9.

[0035] The base plate 9 is rectangular, with two positioning holes 91 in the center. The center distance between the two positioning holes 91 is 65mm, and they match the two positioning pins on the attenuating total reflection accessory ATR. The outer diameter of the positioning pin is in clearance fit or transition fit with the inner diameter of the positioning hole 91.

[0036] The crystal base 10 has a circular slot at its center, a slot at its bottom that matches the positioning hole 91 in the base plate 9, and screw holes II 101 at each of its four corners at the top. Screw holes II 101 match screw holes I 53 in the in-situ infrared pool 5. The integrated heating element 4 is inserted into the circular slot and contacts the positioning hole 91 in the base plate 9. The crystal base 10 and the in-situ infrared pool 5 are fixed together with screws.

[0037] The in-situ pool insulation layer 6 is a hollow cylinder II. Four grooves II 61 are evenly distributed along the length of the inner wall of cylinder II. Each groove II 61 matches the size of groove I 51 in the in-situ infrared pool body 5 and is connected to it one-to-one. Through holes 62 are provided on the outer wall of the cylinder corresponding to the air inlet 7 and air outlet 8. A through groove 63 is provided above the through hole 62. The in-situ pool insulation layer 6 is fitted over the outside of the in-situ infrared pool body 5, and grooves I 51 and II 61 form a closed cylinder. The purpose of providing the through groove 63 is to fix the position of the inlet and outlet pipelines.

[0038] The top cover 3 of the attenuated total reflection in-situ pool is respectively equipped with fixing screws V16, VI17, VII18 and VIII19, which are inserted into the corresponding screw holes III on the top cover insulation layer 2.

[0039] The top cover insulation layer 2 is respectively provided with fixing screws I12, II13, III14 and IV15. These fixing screws I12, II13, III14 and IV15 are inserted into the corresponding screw holes IV on the top cover 3 of the attenuated total reflection in-situ pool.

[0040] Inlet 7 is connected to an external gas cylinder. Outlet 8 is connected to an external exhaust gas outlet.

[0041] Instructions for use: First, turn on the infrared spectrometer. Align the two positioning holes 91 of the base plate 9 with the positioning pins of the attenuated total reflection accessory along the axial direction, inserting the two positioning pins into the two positioning holes 91 one-to-one. Precise matching with a 65mm spacing achieves the positioning purpose. Then, connect the base plate 9, crystal base 10, and in-situ infrared cell 5 in sequence; place the sample at the bottom of the in-situ infrared cell 5 (see details). Figure 2 (Hollow cylinder in the middle). After completion, place the in-situ cell top cover 3 on the in-situ infrared cell 5, and tighten the fixing screws I12, II13, III14, IV15, V16, VI17, VII18, and VIII19 respectively. Then apply a preset pressure to the base plate 9 to ensure that the connecting surfaces of this utility model and the accessory are tightly fitted without relative displacement, thus completing the stable connection between the two and ensuring the accuracy and repeatability of the subsequent attenuation total reflectance spectroscopy test.

[0042] Connect the temperature and pressure control line 11, turn on the external temperature and pressure control device, turn on the external gas cylinder, and the reaction gas enters the sample surface inside the in-situ infrared cell 5 through the inlet 7, and then exits from the reaction gas outlet 8; set the temperature and pressure inside the in-situ cell 5 through the temperature and pressure control device.

[0043] During the test, infrared light is attenuated by the total internal reflection accessory of the red spectrometer and reflected to the crystal base before reaching the sample surface. The structural changes of the sample during the reaction process are detected under different temperatures, atmospheres and pressures.

[0044] Once the test is complete, shut down the temperature and pressure control device, gas cylinder, and infrared spectrometer in sequence.

Claims

1. An attenuated total internal reflection in-situ infrared characterization system, characterized in that: The system includes a base plate (9), a crystal base (10) placed on the base plate (9), and an in-situ infrared pool (5) and an integrated heating element (4) connected together on the crystal base (10); the outer wall of the in-situ infrared pool (5) is provided with an in-situ pool insulation layer (6); the in-situ infrared pool (5) is provided with an air inlet (7) and an air outlet (8), which penetrate the in-situ pool insulation layer (6); The integrated heating element (4) is provided with an attenuated total reflection in-situ pool top cover (3), and the attenuated total reflection in-situ pool top cover (3) is provided with a top cover insulation layer (2); the attenuated total reflection in-situ pool top cover (3) is provided with a pressure sensor (1), and the pressure sensor (1) passes through the top cover insulation layer (2); the in-situ pool top cover (3) is provided with a temperature control and pressure measuring line (11), and the temperature control and pressure measuring line (11) passes through the top cover insulation layer (2) and is connected to a temperature control and pressure measuring device.

2. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The in-situ infrared pool body (5) is a hollow cylinder I; the outer wall of the cylinder I is evenly distributed with four grooves I (51) along the length direction, and each groove I (51) is provided with a fixing hole (52) at the bottom; the top of the cylinder is evenly distributed with four screw holes I (53); the air inlet (7) and the air outlet (8) are symmetrically arranged on the outer wall between two adjacent grooves I (51); the integrated heating element (4) is inserted into the cavity of the cylinder I and passes through the crystal base (10) to contact the base plate (9).

3. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1 or 2, characterized in that: The crystal base (10) is fitted into the center of the base plate (9).

4. The attenuated total internal reflection in-situ infrared characterization system as described in claim 3, characterized in that: The base plate (9) is rectangular and has two positioning holes (91) in the center. The center distance between the two positioning holes (91) is 65mm and matches the two positioning pins on the attenuated total reflection accessory ATR. The outer diameter of the positioning pin is in clearance fit or transition fit with the inner diameter of the positioning hole (91).

5. The attenuated total internal reflection in-situ infrared characterization system as described in claim 3, characterized in that: The crystal base (10) has a circular slot at its center and a slot at its bottom that matches the positioning hole (91) in the base plate (9). The top four corners are provided with screw holes II (101). The screw holes II (101) match the screw holes I (53) in the in-situ infrared pool (5). The integrated heating element (4) is inserted into the circular slot and contacts the positioning hole (91) in the base plate (9).

6. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The in-situ pool insulation layer (6) is a hollow cylinder II; the inner wall of the cylinder II is evenly distributed with four grooves II (61) along the length direction, and each groove II (61) matches the size of the groove I (51) in the in-situ infrared pool (5) and is connected to it one by one; the outer wall of the cylinder corresponding to the air inlet (7) and the air outlet (8) is provided with a through hole (62), and a through groove (63) is provided above the through hole (62).

7. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The top cover (3) of the attenuated total reflection in situ pool is provided with fixing screws V (16), VI (17), VII (18) and VIII (19), which are inserted into the corresponding screw holes III on the top cover insulation layer (2).

8. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The top cover insulation layer (2) is provided with fixing screws I (12), II (13), III (14) and IV (15), which are inserted into the corresponding screw holes IV on the top cover (3) of the attenuated total reflection in situ pool.

9. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The air inlet (7) is connected to an external gas cylinder.

10. The attenuated total internal reflection in-situ infrared characterization system as described in claim 1, characterized in that: The exhaust port (8) is connected to the exhaust gas.

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