High temperature high pressure in-situ testing device

Abstract

The utility model belongs to in situ test research, specifically relates to a high temperature and high pressure in situ testing device, including the casing of tubular, the casing's cylinder chamber constitutes the closed cavity, is provided with the sample holder for placing sample in the closed cavity, the casing is from one side to opposite another side is provided with the passage that passes through the casing, sample holder and is used for the ray to pass through, the sample is placed in the through -hole that the passage formed on the sample holder, is provided with the light window on the port of the passage on the casing cylinder wall, the outside of casing is provided with the air -inlet and outlet interface that communicates the sealed cavity, is provided with the heat -insulating cylinder in the closed cavity, the heat -insulating cylinder and the cylinder wall of casing seal and fit, the passage passes through the heat -insulating cylinder, heating device is located in the sample holder's frame body in the heat -insulating cylinder chamber, the frame body of sample holder and the heat -insulating cylinder chamber wall between the heat -insulating cylinder chamber are arranged and form the air gap interval, the air gap interval and the heat -insulating cylinder mutually cooperate, can better inhibit the high temperature on the sample holder to the outer shell transmission.

Description

Technical Field

[0001] This utility model relates to in-situ testing research, specifically to a high-temperature and high-pressure in-situ testing device. Background Technology

[0002] X-ray absorption fine structure (XAFS) spectroscopy, due to its locality, element selectivity, sensitivity, orientation, and versatility, has become a powerful tool for studying the structure of matter, with wide applications in materials science, energy, chemistry, environmental science, and life sciences. In catalyst research, in-situ XAFS real-time spectral measurements provide crucial information about catalyst structure, interfacial coordination structures, electronic structures of catalytic active centers, and kinetics, making it a vital tool for catalyst research. With the increasing demand for high-temperature chemical reactions, selecting and developing in-situ testing devices suitable for high-temperature and high-pressure environments is of paramount importance.

[0003] The patent document entitled "High-throughput High-Temperature In-situ X-ray Absorption Spectroscopy Research Device and Its Operation Method" (Publication No. CN202411399625.X, hereinafter referred to as Document 1) discloses a technical solution including a vacuum furnace module with an opening at the top, X-ray incident light-passing holes and corresponding X-ray exit light-passing holes with their optical axes aligned on two opposite sides, and a vacuum interface for connecting to an external vacuum pumping device on the other side; and a heating module that extends into and connects to the vacuum furnace module through the opening of the vacuum furnace module, including a sample holder, heating elements and thermocouples. The heating elements and thermocouples are positioned adjacent to the sample holder and heat the sample holder and measure its temperature.

[0004] The patent document entitled "A High Temperature and High Pressure In-situ Infrared Spectroscopy Testing Device" (publication number CN209878501U, hereinafter referred to as Document 2) discloses a technical solution including a reaction chamber, the inside of which is a sealed cavity isolated from the outside, a sample cavity for placing samples is set in the sealed cavity, and a heating device is set outside the sample cavity; the reaction chamber is also provided with an inlet and an outlet that can be opened or closed. This solution can realize the testing and research of catalysts under high temperature or even high pressure conditions.

[0005] In the technical solutions disclosed in the aforementioned documents, a heating device is installed in a sealed chamber to meet the requirements of in-situ testing under high temperature and high pressure conditions. Therefore, it is particularly important to avoid the safety hazards of overheating of the external testing device, which could lead to damage or burns to personnel. Although a heat insulation sleeve is used to insulate the heating wire in Reference 2, the heat insulation sleeve, heating wire, and reaction chamber are all arranged in close proximity. The heat dissipated from the heating wire to the reaction chamber depends entirely on the heat insulation effect of the heat insulation sleeve itself, and the insulation effect needs improvement. Summary of the Invention

[0006] This invention provides a high-temperature and high-pressure in-situ testing device that improves the suppression of heat conduction between the heating device and the external body of the testing device, avoiding damage caused by overheating of the external body or the safety hazard of burns from contact with personnel.

[0007] To achieve the above objectives, the technical solution adopted is as follows: a high-temperature and high-pressure in-situ testing device, comprising a cylindrical shell, the cavity of which forms a sealed cavity, a sample holder for placing samples is provided inside the sealed cavity, a channel is provided from one side of the shell to the opposite side, penetrating the shell and the sample holder and allowing X-rays to pass through, the sample is placed in a through hole formed by the channel on the sample holder, a light-transmitting window is provided at the port of the channel on the shell wall, an inlet and outlet port for communicating with the sealed cavity is provided on the outside of the shell, a heat insulation cylinder is provided inside the sealed cavity, the heat insulation cylinder is sealed and fitted to the shell wall, the channel penetrates the heat insulation cylinder, the sample holder is placed inside the cavity of the heat insulation cylinder, the opening of the heat insulation cylinder and the frame of the sample holder located at the corresponding position of the opening of the heat insulation cylinder form a sealed fit, the frame of the sample holder located inside the heat insulation cylinder cavity is spaced apart from the wall of the heat insulation cylinder cavity, and a heating device is located inside the frame.

[0008] Compared with the prior art, the technical effect of this utility model is as follows: the heating device is located in the sample rack inside the heat insulation cylinder chamber. The sample rack inside the heat insulation cylinder chamber and the heat insulation cylinder chamber wall are arranged at intervals to form an air gap. The air gap and the heat insulation cylinder cooperate with each other to better suppress the high temperature on the sample rack from being transferred to the outer shell. This protects the shell from overheating and damage, while also preventing burns to personnel. Attached Figure Description

[0009] Figure 1 This is a three-dimensional appearance schematic diagram of the present utility model;

[0010] Figure 2 This is a schematic diagram showing the protective cover separated from the housing.

[0011] Figure 3 This is a schematic diagram showing the assembly state of the heat insulation cylinder and the sample holder.

[0012] Figure 4This is a top view of the present invention;

[0013] Figure 5 for Figure 4 NN-direction cross-sectional view;

[0014] Figure 6 This is the front view of the present invention;

[0015] Figure 7 for Figure 6 KK-direction sectional view in the middle;

[0016] Figure 8 for Figure 7 A partial structural diagram. Detailed Implementation

[0017] The following is in conjunction with the appendix Figure 1-8 The present invention will be further described in detail below, including related content:

[0018] A high-temperature and high-pressure in-situ testing device includes a cylindrical shell 10, the cavity of which forms a sealed cavity 11. A sample holder 20 for placing a sample A is disposed within the sealed cavity 11. A channel P, penetrating the shell 10 and the sample holder 20 and allowing X-rays to pass through, is provided from one side of the shell 10 to the opposite side. Sample A is placed within a through hole formed by channel P on the sample holder 20. A light-transmitting window 30 is provided at the port of channel P on the cylindrical wall of the shell 10. A connecting sealed cavity 1 is provided outside the shell 10. The inlet and outlet ports 12a and 12b of the housing 11 are provided. A heat insulation cylinder 40 is provided in the sealed cavity 11. The heat insulation cylinder 40 is sealed and fitted to the cylinder wall of the housing 10. The channel P passes through the heat insulation cylinder 40. The sample holder 20 is placed inside the cylinder cavity of the heat insulation cylinder 40. The cylinder opening of the heat insulation cylinder 40 and the frame of the sample holder 20 located at the corresponding position of the cylinder opening of the heat insulation cylinder 40 form a sealed fit. The frame of the sample holder 20 located in the cavity of the heat insulation cylinder 40 is arranged at intervals between the frame of the heat insulation cylinder 40 and the cavity wall of the heat insulation cylinder 40, and the heating device 50 is located in the frame.

[0019] In the above technical solution, the heating device 50 is located inside the sample holder 20 within the chamber of the heat insulation cylinder 40. An air gap is formed between the sample holder 20 and the chamber wall of the heat insulation cylinder 40. Air gap heat transfer is less efficient than direct contact heat transfer. Through the interaction between the air gap and the heat insulation cylinder 40, the high temperature on the sample holder 20 can be better suppressed from transferring to the outer shell 10, protecting the shell 10 from overheating and damage, while also preventing burns to personnel.

[0020] The heat insulation cylinder 40 is sealed to the wall of the shell 10 to prevent high-temperature gas from existing between the heat insulation cylinder 40 and the shell 10, thus avoiding severe overheating of the shell 10. Although there is contact between the heat insulation cylinder 40 and the high-temperature gas in the through hole formed in the shell 10 through the channel P, the contact area is small, and the impact on the shell 10's heating is negligible.

[0021] The inlet and outlet ports 12a and 12b of the externally disposed sealing cavity 11 can be connected to a vacuum source or a gas source to meet the requirements of sealing or vacuum. Of course, it is also possible to connect to different gas sources to meet the testing requirements in different gas environments.

[0022] It should be noted that the technical principles of X-ray absorption fine structure spectroscopy and the setup of the experimental environment are common knowledge in this field, and will not be discussed in detail here.

[0023] As a preferred solution, combined with Figure 2 , Figure 3 as well as Figure 5 As shown, the opening of the heat insulation cylinder 40 extends to the outside of the housing 10, forming a sealed fit between them. A plate-shaped sample holder 20 is inserted into the cavity from the opening of the heat insulation cylinder 40, with the plate surface of the sample holder 20 perpendicular to the through direction of the channel P. A flange 21 protruding towards the wall of the heat insulation cylinder 40 is provided on the plate end of the sample holder 20 near the opening of the heat insulation cylinder 40, and the flange 21 is sealed to the opening of the heat insulation cylinder 40. In this design, the flange 21 seals the opening of the heat insulation cylinder 40, and a sealed fit is formed between the opening of the heat insulation cylinder 40 and the housing 10, thereby forming an effective sealed cavity 11 within the housing 10.

[0024] Furthermore, such as Figure 5 As shown, the heating device 50 includes a heating rod 51 and a temperature sensor 52, both of which are embedded in the plate of the sample holder 20. The heating rod 51 is used to heat the sample holder 20 and indirectly heat the sealed cavity 11, while the temperature sensor 52 is used to monitor the ambient temperature inside the sealed cavity 11 in real time to control the experimental temperature.

[0025] As a preferred option, the heat insulation cylinder 40 is made of zirconia ceramic, which has good heat insulation performance.

[0026] Combination Figure 1 , Figure 7 as well as Figure 8As shown, the light-transmitting window 30 and the housing 10 are detachably fixed together. The light-transmitting window 30 includes a flange 31, and a through hole 311 communicating with the channel P is provided in the middle of the flange 31. A light-transmitting plate 32 for sealing the hole area is provided on the through hole 311. When it is necessary to replace sample A on the sample holder 20, the flange 31 of the light-transmitting window 30 can be removed from the housing 10. Then, the through hole formed by the channel P in the housing 10 and the heat insulation cylinder 40 can be used by technicians to insert tools to replace sample A on the sample holder 20.

[0027] It should be noted that the light-transmitting plate 32 allows X-rays to pass through and can be made of polyimide film or beryllium, which has high X-ray transmittance.

[0028] Furthermore, the through hole of channel P on the sample holder 20 forms a stepped hole. A tubular pressure sleeve 22 is installed in the large-diameter section of the stepped hole. The pressure sleeve 22 and the hole wall of the stepped hole form a detachable fixed fit. Sample A is sandwiched between the stepped surface of the stepped hole and the pressure sleeve 22. By removing the pressure sleeve 22, it can be removed from the stepped hole, allowing sample A to be replaced within the through hole on the sample holder 20. Conversely, by installing the pressure sleeve 22 in the stepped hole, sample A can be sandwiched between the stepped surface of the stepped hole and the pressure sleeve 22, thus fixing sample A to meet experimental requirements.

[0029] As a preferred solution, combined with Figure 1 , Figure 5 as well as Figure 7 As shown, a cold circulation component 60 is also provided on the shell 10. The cold circulation component 60 includes a refrigerant inlet and outlet 61a and 61b provided on the outer wall of the shell 10. A pipe 62 for refrigerant circulation is provided inside the shell 10. One end of the pipe 62 is connected to the refrigerant inlet 61a and the other end is connected to the refrigerant outlet 61b. By supplying refrigerant (such as water) into the pipe 62 inside the shell 10, the refrigerant can absorb heat from the shell 10 through heat conduction and carry it away through the refrigerant outlet 61b.

[0030] like Figure 1 , Figure 2 as well as Figure 5 As shown, a protective cover 13 is placed on the opening of the housing 10. The plate end of the sample holder 20 at the opening of the heat insulation cylinder 40 is located inside the protective cover 13. The protective cover 13 is provided with a wire hole 131 for the electrical wires of the heating device 50 to pass through. The protective cover 13 is provided to cover the opening of the heat insulation cylinder 40 and the plate end of the sample holder 20 at that location to avoid the risk of personnel contact.

Claims

1. A high-temperature and high-pressure in-situ testing device, comprising a cylindrical shell (10), the cylindrical cavity of the shell (10) forming a sealed cavity (11), a sample holder (20) for placing a sample (A) is provided inside the sealed cavity (11), a channel (P) is provided from one side to the opposite side of the shell (10) penetrating the shell (10) and the sample holder (20) and allowing X-rays to pass through, the sample (A) is placed in a through hole formed in the sample holder (20) by the channel (P), a light-transmitting window (30) is provided at the port of the channel (P) located on the cylindrical wall of the shell (10), and an inlet and outlet port (12a, 12b) communicating with the sealed cavity (11) is provided outside the shell (10), characterized in that: A heat insulation cylinder (40) is provided inside the sealed cavity (11). The heat insulation cylinder (40) is sealed and fitted to the cylinder wall of the shell (10). The channel (P) passes through the heat insulation cylinder (40). The sample holder (20) is placed inside the cylinder cavity of the heat insulation cylinder (40). The cylinder opening of the heat insulation cylinder (40) and the frame of the sample holder (20) located at the corresponding position of the cylinder opening of the heat insulation cylinder (40) form a sealed fit. The frame of the sample holder (20) located in the cavity of the heat insulation cylinder (40) is arranged at intervals between the frame of the sample holder (20) and the cavity wall of the heat insulation cylinder (40), and the heating device (50) is located in the frame.

2. The high-temperature and high-pressure in-situ testing device according to claim 1, characterized in that: The opening of the heat insulation cylinder (40) extends to the outside of the shell (10) and the two form a sealed fit. The plate-shaped sample holder (20) is inserted into the cavity from the opening of the heat insulation cylinder (40) and the plate surface of the sample holder (20) is perpendicular to the through direction of the channel (P). The plate end of the sample holder (20) near the opening of the heat insulation cylinder (40) is provided with a flange (21) protruding towards the wall of the heat insulation cylinder (40). The flange (21) is sealed to the opening of the heat insulation cylinder (40).

3. The high-temperature and high-pressure in-situ testing device according to claim 2, characterized in that: The heating device (50) includes a heating rod (51) and a temperature sensor (52), both of which are embedded in the plate of the sample holder (20).

4. The high-temperature and high-pressure in-situ testing device according to claim 1, characterized in that: The heat insulation cylinder (40) is made of zirconia ceramic.

5. The high-temperature and high-pressure in-situ testing device according to claim 1 or 2, characterized in that: The light-transmitting window (30) and the housing (10) are detachably fixed together. The light-transmitting window (30) includes a flange (31). The center of the flange (31) is provided with a through hole (311) communicating with the channel (P). A light-transmitting plate (32) for sealing the hole area is provided on the through hole (311).

6. The high-temperature and high-pressure in-situ testing device according to claim 1, characterized in that: The through hole of the channel (P) on the sample holder (20) forms a stepped hole. A tubular pressure sleeve (22) is provided in the large diameter section of the stepped hole. The pressure sleeve (22) and the hole wall of the stepped hole form a detachable fixed fit. The sample (A) is sandwiched between the stepped surface of the stepped hole and the pressure sleeve (22).

7. The high-temperature and high-pressure in-situ testing device according to claim 1, characterized in that: The shell (10) is also provided with a cold circulation component (60), which includes a refrigerant inlet and outlet (61a, 61b) provided on the outer wall of the shell (10). The shell (10) is provided with a pipe (62) for refrigerant circulation inside the cylinder wall. One end of the pipe (62) is connected to the refrigerant inlet (61a) and the other end is connected to the refrigerant outlet (61b).

8. The high-temperature and high-pressure in-situ testing device according to claim 1 or 3, characterized in that: The shell (10) is covered with a protective cover (13). The plate end of the sample holder (20) at the opening of the heat insulation cylinder (40) is located inside the protective cover (13). The protective cover (13) is provided with a wire hole (131) for the electric wire of the heating device (50) to pass through.

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