In-situ high temperature and high pressure reaction device

Abstract

The present invention provides an in-situ high-temperature and high-pressure reaction device, which is used to solve multiple defects and shortcomings in existing high-temperature and high-pressure reaction chamber products. For example: it is impossible to interconnect with an ultra-high vacuum cavity, it is impossible to achieve rapid annealing with liquid nitrogen, it is impossible to achieve local heating, etc. The device includes: a vacuum cavity, a reaction pool, a heating device, a refrigeration device, a pressurized gas circuit and a feeding device. By implementing the technical solution of the present invention, a laser heater is used in conjunction with a sapphire light-transmitting cavity, and the device can achieve local laser heating and simplify the structure of the reaction pool; a high-strength sapphire light-transmitting cavity is used to bear pressure, and the device can achieve a high-pressure atmosphere; the reaction pool cavity is connected to the feeding device and is movably connected to the feeding device to achieve the reuse of the reaction device; the feeding device and the vacuum cavity, and the reaction pool are mechanically sealed, with good sealing effect and simple structure.

Description

Technical Field

[0001] The invention relates to the field of ultra-high vacuum reactors, and in particular to an in-situ high-temperature and high-pressure reaction device. Background Art

[0002] High temperature and high pressure reaction cells can be used to study multiphase catalysis, gas-solid interaction, photochemical reaction and oxidation mechanism research under controlled environment. Usually, high temperature and high pressure reaction cells have two gas inlets, one for air inlet and one for air outlet. The reaction cell is filled with oxygen, nitrogen and other gases up to 10 atmospheres through the air inlet to meet the high pressure requirements. The sample is heated by laser, and liquid nitrogen is quickly introduced to cool and quench the sample in the cavity after the sample reacts with the high pressure gas. In order to prevent the reaction cell from freezing when encountering water vapor at low temperature, the reaction cell must be placed in an ultra-high vacuum cavity. On the one hand, the high pressure in the reaction cell forms a huge pressure difference with the vacuum environment of the vacuum cavity. On the other hand, the materials selected for the reaction cell in the entire temperature range from the liquid nitrogen temperature zone to the high temperature of 1000 degrees will have a large thermal expansion and contraction effect. These have put forward strict requirements for the sealing of the reaction cell window in the vacuum cavity and repeated sealing. In the prior art, there is still no perfect solution to the problem of high temperature and high pressure reaction chamber, nor is there a product with high stability, simple structure and reusability.

[0003] Therefore, there is a need for an in-situ high-temperature and high-pressure reaction device with high stability, simple structure and reusability. Summary of the invention

[0004] In order to solve the above technical problems, the present invention discloses an in-situ high temperature and high pressure reaction device, and the technical solution of the present invention is implemented as follows:

[0005] An in-situ high-temperature and high-pressure reaction device comprises: a vacuum chamber, a reaction pool, a heating device, a refrigeration device, a pressurized gas circuit and a feeding device; wherein the vacuum chamber is provided with a cooling opening, a feeding opening and a vacuum chamber air hole; the refrigeration device extends into the vacuum chamber and is sealedly connected to the cooling opening; the reaction pool comprises a sample stage and a reaction pool chamber, and the sample stage is fixed to the refrigeration device; the feeding device is sealedly connected to the vacuum chamber, and the reaction pool chamber is fixed to the feeding device, and when the feeding device is completely fed into the vacuum chamber, the reaction pool chamber is sealedly connected to the sample stage; the sample is fixed on the sample stage, and the heating device heats the sample; the vacuum chamber air hole is connected to an external vacuum system, and the pressurized gas circuit connects the reaction pool and an external high-pressure gas source.

[0006] Preferably, the heating device is a laser heater, the vacuum chamber is provided with a heating window, the reaction pool chamber includes a light-transmitting cavity and a cavity support; the light-transmitting cavity is sealingly connected to the cavity support, the cavity support includes a fixed end and a sealing end, the fixed end is fixed to the feeding device, when the feeding device is completely fed into the vacuum chamber, the sealing end is sealingly connected to the sample stage, and the laser heater, the heating window, the light-transmitting cavity and the sample are located on the same optical path.

[0007] Preferably, the sealing end is provided with a knife edge that fits the shape of the sample stage, and when the feeding device is completely fed into the vacuum chamber, the sealing end is metal-sealed with the sample stage.

[0008] Preferably, the light-transmitting cavity is made of sapphire or quartz.

[0009] Preferably, the feeding device comprises a screw and a bellows, the bellows is mechanically sealed with the vacuum chamber, and the screw is arranged on the axis of the bellows; the bellows is sealingly connected to the reaction pool chamber, and the screw is connected to the reaction pool chamber.

[0010] Preferably, the feeding device further comprises a corrugated guide rod, which is fixed inside the vacuum chamber and connected to the bellows.

[0011] Preferably, the refrigeration device comprises a cold head and a coolant channel; and the sample stage is fixed to the cold head.

[0012] Preferably, the material of the cold head includes copper, silver or aluminum.

[0013] Preferably, the vacuum chamber is provided with windows, and the number of the windows is greater than or equal to one.

[0014] Preferably, the pressurized gas circuit is an air duct, and the air duct is arranged inside the bellows and connected to the reaction pool cavity.

[0015] The technical solution of the present invention can solve the technical problems in the prior art that there is no perfect solution for high-temperature and high-pressure reaction chambers, and there is no product with high stability, simple structure and reusability; by implementing the technical solution of the present invention, a laser heater is used in conjunction with a sapphire light-transmitting cavity, and the device can realize laser local heating and simplify the structure of the reaction pool; a high-strength sapphire light-transmitting cavity is used to bear pressure, and the device can realize a high-pressure atmosphere; the reaction pool cavity is connected to a feed-in device and can be movably used to realize the reuse of the reaction device; the feed-in device and the vacuum cavity and the reaction pool are mechanically sealed, and the sealing effect is good and the structure is simple. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only one embodiment of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0017] Figure 1 It is a schematic diagram of the overall structure of a device according to a specific embodiment of the present invention;

[0018] Figure 2 It is a schematic diagram of the structure of an unsealed reaction cell and a feeding device according to a specific embodiment of the present invention;

[0019] Figure 3 It is a schematic diagram of the structure of an unsealed reaction pool according to a specific embodiment of the present invention.

[0020] In the above drawings, the figure numbers represent:

[0021] 1-vacuum chamber; 2-reaction pool; 201-sample stage; 202-reaction pool chamber; 2021-light-transmitting chamber; 2022-chamber bracket; 2023-fixed end; 2024-sealed end; 2025-connecting column; 2026-knife edge; 3-heating device; 4-refrigeration device; 401-cold head; 402-coolant channel; 5-pressurized gas path; 501-air guide tube; 6-feeding device; 601-screw 602-bellows; 603-corrugated guide rod; 7-vacuum chamber air hole; 8-cooling opening; 9-feeding opening; 10-window; 11-heating window. DETAILED DESCRIPTION

[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] In a specific embodiment of the present invention, an in-situ high temperature and high pressure reaction device, such as Figure 1 , Figure 2 and Figure 3As shown, it includes: a vacuum chamber 1, a reaction pool 2, a heating device 3, a refrigeration device 4, a pressurized gas circuit 5 and a feeding device 6; wherein the vacuum chamber 1 is provided with a cooling opening 8, a feeding opening 9 and a vacuum air hole; the refrigeration device 4 extends into the vacuum chamber 1 and is sealed and connected to the cooling opening 8; the reaction pool 2 includes a sample stage 201 and a reaction pool chamber 202, and the sample stage 201 is fixed to the refrigeration device 4; the feeding device 6 is sealed and connected to the vacuum chamber 1, and the reaction pool chamber 202 is fixed to the feeding device 6, and when the feeding device 6 is completely fed into the vacuum chamber 1, the reaction pool chamber 202 is sealed and connected to the sample stage 201; the sample is fixed on the sample stage 201, and the heating device 3 heats the sample; the vacuum chamber air hole 7 is connected to the external vacuum system, and the pressurized gas circuit 5 connects the reaction pool and the external high-pressure gas source.

[0024] When the feeding device 6 is fully fed into the vacuum chamber 1, a closed environment with a sample stage 201 is formed inside the reaction pool 2, which is the first sealed chamber. The space inside the vacuum chamber 1 and outside the reaction pool 2 is the second sealed chamber. During the use of the device, the user first puts the sample into the sample stage 201, and then fully feeds the feeding device 6 into the vacuum chamber 1. The user injects nitrogen, neon or oxygen into the first sealed chamber as a protective gas or reaction gas through the pressurized gas line 5, and heats the sample through the heating device 3 to achieve a high-temperature and high-pressure reaction. The heating temperature and gas pressure can be selected according to the type of sample and the type of reaction. The vacuum chamber 1 and the reaction pool chamber 202 can be made of high-strength metal materials such as stainless steel, which is conducive to achieving a high-temperature and high-pressure environment in the first chamber. The heating device 3 can use a heating wire, a heating tube or an electron beam heating device connected to the sample stage 201, or a laser heater arranged in the second sealed chamber or outside the vacuum chamber 1. When the device heats the sample, the user can select a suitable laser heater according to the temperature required for the reaction, the type of sample and other parameters. The sample stage 201 and the reaction pool chamber 202 may be sealed by using a sealing gasket or other method.

[0025] The refrigeration device 4 is used to cool the sample stage 201. After the sample reaction is completed, the refrigeration device 4 cools the sample to a specific reaction low temperature or room temperature through the heat transfer effect of the sample stage 201, allowing the sample to react at a low temperature, or restores the sample to room temperature, making it convenient for the user to take out the sample for standby use.

[0026] When conducting experiments on highly reactive samples, in order to prevent the sample from reacting with oxygen, carbon dioxide and other gases in the air when it comes into contact with the air under conditions of residual heat, the user can use an external vacuum pump to evacuate the second sealed chamber to a high vacuum through the vacuum chamber air hole 7 to improve the reliability of the reactor. Pumping the second sealed chamber to a high vacuum can also prevent the water vapor in the second sealed chamber from condensing on the surface of the reaction pool 2 when the refrigeration device 4 is used to cool the sample stage 201, thereby preventing the reaction pool 2 from being damaged. This can extend the life of the device, reduce the failure rate of the device, and make the device suitable for ultra-low temperature reactions.

[0027] The user can place the sample after taking out the feeding device 6 or the cooling device, or can set a manipulator connected to the vacuum chamber 1 to place the sample on the sample stage 201. The sample can be detachably fixed on the sample stage 201 through a square sample holder. The focus of the present invention is on the reactor itself that realizes the high temperature and high pressure reaction. The user can select a suitable sample placement and holding method according to the type, shape, size and other parameters of the sample.

[0028] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the heating device 3 is a laser heater, the vacuum chamber 1 is provided with a heating window 11, the reaction pool chamber 202 includes a light-transmitting cavity 2021 and a cavity bracket 2022; the light-transmitting cavity 2021 is sealed and connected to the cavity bracket 2022, the cavity bracket 2022 includes a fixed end 2023 and a sealing end 2024, the fixed end 2023 is fixed to the feeding device 6, when the feeding device 6 is completely fed into the vacuum chamber 1, the sealing end 2024 is sealed and connected to the sample stage 201, and the laser heater, the heating window 11, the light-transmitting cavity 2021 and the sample are located on the same optical path.

[0029] Before the laser heater works, the user needs to put the sample on the sample stage 201, and then feed the feeding device 6 into the vacuum chamber 1. The reaction pool 2 is completely sealed, the laser heater, the heating window 11, the light-transmitting cavity 2021 and the sample are located on the same optical path, and the laser emitted by the laser heater is irradiated on the sample through the heating window 11 and the light-transmitting cavity 2021 to perform laser heating on the sample. In this specific embodiment, the light-transmitting cavity 2021 is configured to be annular, and the fixed end 2023 and the sealing end 2024 are connected by a plurality of connecting columns 2025 to fix the position of the light-transmitting cavity 2021. The user can set a plurality of heating windows 11 on the vacuum chamber 1 to facilitate the laser irradiation of the sample from different angles, which is suitable for samples of different shapes and sizes, and can improve the compatibility of the device.

[0030] When the feeding device 6 is fully fed into the vacuum chamber 1, the sample stage 201, the sealing end 2024, the light-transmitting cavity 2021 and the fixed end 2023 are sealed in sequence to form a first sealed cavity inside. The sample stage 201 and the sealing end 2024 are under great pressure in the axial direction of the annular light-transmitting cavity 2021, so that the sealing end 2024 and the light-transmitting cavity 2021, and the light-transmitting cavity 2021 and the fixed end 2023 are all under great pressure, thereby preventing degassing between the cavity bracket 2022 and the light-transmitting cavity 2021.

[0031] Heating by laser heating is conducive to simplifying the structure of the reaction pool 2. There is no need to set heating elements such as electric heating wires in the reaction pool 2, which is conducive to reducing the manufacturing difficulty of the reaction pool 2. The user can adjust the heating rate by setting the power of the laser to achieve slow and uniform heating, or instant heating. The maximum temperature can reach more than 1000°C, using more reaction types and improving the compatibility of the device.

[0032] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the sealing end 2024 is provided with a blade 2026 which fits the shape of the sample stage 201. When the feeding device 6 is fully fed into the vacuum chamber 1, the blade 2026 presses an indentation on the sample stage 201, and the sealing end 2024 and the sample stage 201 are sealed by relying on the elastic force between the blade 2026 and the sample stage 201. The structure is simple and the operation is convenient, which can reduce the production difficulty of the device and change the feeding degree of the feeding device 6. By adjusting the elastic force between the blade 2026 and the sample stage 201, the first sealing chamber can be applied to a higher pressure, thereby improving the compatibility of the device.

[0033] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the material of the light-transmitting cavity 2021 is sapphire or quartz.

[0034] The light-transmitting cavity 2021 bears the pressure from the sealing end 2024 and the fixed end 2023 in the axial direction, and bears the pressure under the high pressure difference between the first sealing cavity and the second sealing cavity in the radial direction, so the strength of the material of the light-transmitting cavity 2021 has high requirements.

[0035] In this specific embodiment, the material of the light-transmitting cavity 2021 is sapphire. On the one hand, sapphire has high structural strength and can withstand high pressure in both radial and axial directions, so that the pressure inside the first sealed cavity can reach more than 10 bar. On the other hand, the laser has good light transmittance, which can make most of the laser energy pass through the light-transmitting cavity and concentrate on the sample, which is conducive to the instantaneous ultra-high temperature heating of the sample by the device. At the same time, it can prevent the light-transmitting cavity from absorbing too much energy, causing excessive temperature to damage the reaction pool 2 structure, and improve the reliability of the device. In addition, sapphire has a low thermal expansion and contraction coefficient, which can increase the applicable reaction temperature and improve the compatibility and reliability of the device. Users can also use other high-strength light-transmitting materials such as quartz.

[0036] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3As shown, the feeding device 6 includes a screw 601 and a bellows 602 . The bellows 602 is mechanically sealed with the vacuum chamber 1 , and the screw 601 is arranged on the axis of the bellows 602 . The bellows 602 is sealed and connected to the reaction pool chamber 202 , and the screw 601 is connected to the reaction pool chamber 202 .

[0037] In this specific embodiment, the feed opening 9 of the vacuum chamber 1 can be provided with corrugations that match the bellows 602. After the bellows 602 is screwed into the vacuum chamber 1, the bellows 602 fits the feed opening 9, isolating the second sealed cavity from the external atmosphere, and realizing the sealing of the feed device 6 and the vacuum chamber 1. The screw 601 is connected to the reaction pool chamber 202, and the external driving mechanism can drive the screw 601 through a turbine or other device to realize the automatic feeding of the feed device 6. The bellows 602 and the screw 601 can be made of high-strength materials such as stainless steel to increase the pressure on the reaction pool chamber 202 and realize the sealing of the reaction pool chamber 202 and the sample stage 201.

[0038] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the feeding device 6 also includes a corrugated guide rod 603 , which is fixed inside the vacuum chamber 1 and connected to the bellows 602 .

[0039] In this specific embodiment, the corrugated guide rod 603 can be made of high-strength materials such as stainless steel and is fixed inside the vacuum chamber 1 by a detachable method such as bolts. The end of the corrugated guide rod 603 is arranged to fit the corrugations of the bellows 602 and is connected to the bellows 602 to stabilize the direction of the bellows 602 during the feeding process of the bellows 602, thereby facilitating the sealing of the reaction pool chamber 202 and the sample stage 201, thereby improving the reliability of the device.

[0040] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the refrigeration device 4 includes a cold head 401 and a coolant channel 402 ; the sample stage 201 is fixed to the cold head 401 .

[0041] The main body of the cooling device can be made of stainless steel, and the coolant can be liquid nitrogen, liquid helium or other coolants. The coolant exchanges heat with the sample stage 201 through the cold head 401 to achieve cooling of the sample. The cold head 401 and the coolant channel 402 can be fixed by non-detachable means such as welding, or by detachable means such as bolt fixing and clamping fixing.

[0042] In a preferred embodiment, Figure 1 As shown, the material of the cold head 401 includes copper, silver or aluminum.

[0043] In this specific embodiment, the cold head 401 uses copper as the material, which has good thermal conductivity, and is conducive to the device to quickly cool the sample through heat exchange on the sample stage 201, and can cool the sample to a low temperature below 77K or an ultra-low temperature below 4.2K.

[0044] In a preferred embodiment, Figure 1 As shown, the vacuum chamber 1 is provided with a window 10, and the number of the windows 10 is greater than or equal to one. The user can set the window 10 on the vacuum chamber 1 as needed to facilitate real-time monitoring and recording of the reaction situation. The window 10 can be made of a material with a specific wavelength filtering property, which is conducive to the user's research on the luminescent properties of the sample.

[0045] In a preferred embodiment, Figure 1 , Figure 2 and Figure 3 As shown, the pressurized gas circuit 5 is an air guide tube 501 , and the air guide tube 501 is arranged in the bellows 602 and connected to the reaction pool cavity 202 .

[0046] In this specific embodiment, the air pipe 501 is connected to the external exhaust channel and the high-pressure gas source, so the reaction pool 2 only needs to be provided with one air path opening, which can improve the sealing reliability of the device. The air pipe 501 is provided in the bellows 602 and wound on the screw 601, which is convenient for disassembly and replacement, and can reduce the maintenance cost of the device. The user can also choose to use other installation methods for the air pipe 501.

[0047] It should be pointed out that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. An in-situ high temperature and high pressure reaction device, characterized in that: include: Vacuum chamber, reaction pool, heating device, refrigeration device, pressurized gas circuit and feeding device; wherein, The vacuum chamber is provided with a cooling opening, a feeding opening and a vacuum chamber air hole; The refrigeration device extends into the vacuum chamber and is sealed and connected to the cooling opening; The reaction pool comprises a sample stage and a reaction pool cavity, and the sample stage is fixed to the refrigeration device; The feeding device is sealed and connected to the vacuum chamber, and the reaction pool chamber is fixed to the feeding device. When the feeding device is completely fed into the vacuum chamber, the reaction pool chamber is sealed and connected to the sample stage; The sample is fixed on the sample stage, and the heating device heats the sample; The vacuum chamber air hole is connected to an external vacuum system, and the pressurized gas circuit is connected to the reaction pool and an external high-pressure gas source; The heating device is a laser heater, the vacuum cavity is provided with a heating window, and the reaction pool cavity comprises a light-transmitting cavity and a cavity support; The light-transmitting cavity is sealed and connected to the cavity support, the cavity support includes a fixed end and a sealed end, the fixed end is fixed to the feeding device, when the feeding device is fully fed into the vacuum cavity, the sealed end is sealed and connected to the sample stage, the laser heater, the heating window, the light-transmitting cavity and the sample are located on the same optical path; The sealing end is provided with a knife edge that fits the shape of the sample stage. When the feeding device is completely fed into the vacuum chamber, the sealing end is metal-sealed with the sample stage.

2. The in-situ high temperature and high pressure reaction device according to claim 1, characterized in that: The material of the light-transmitting cavity is sapphire or quartz.

3. The in-situ high temperature and high pressure reaction device according to claim 1, characterized in that: The feeding device comprises a screw and a bellows, the bellows is mechanically sealed with the vacuum chamber, and the screw is arranged on the axis of the bellows; The bellows is sealed and connected to the reaction tank chamber, and the screw is connected to the reaction tank chamber.

4. The in-situ high temperature and high pressure reaction device according to claim 3, characterized in that: The feeding device also includes a corrugated guide rod, which is fixed inside the vacuum chamber and connected to the bellows.

5. The in-situ high temperature and high pressure reaction device according to claim 1, characterized in that: The refrigeration device includes a cold head and a coolant channel; the sample stage is fixed to the cold head.

6. The in-situ high temperature and high pressure reaction device according to claim 5, characterized in that: The cold head is made of copper, silver or aluminum.

7. The in-situ high temperature and high pressure reaction device according to claim 1, characterized in that: The vacuum chamber is provided with windows, and the number of the windows is greater than or equal to one.

8. The in-situ high temperature and high pressure reaction device according to claim 4, characterized in that: The pressurized gas circuit is an air guide pipe, which is arranged inside the corrugated pipe and connected to the reaction pool cavity.

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