An ultrahigh and ultralow temperature and high pressure in-situ reaction cell test device

Abstract

The application relates to the field of Mossbauer spectrum devices, and discloses an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device, which comprises a detection chamber used for detecting a sample and comprising a sample cavity used for containing the sample; a vacuum system used for ensuring vacuum isolation heat conduction and comprising a vacuum chamber arranged outside the detection chamber and a vacuum pump group used for keeping the vacuum degree in the vacuum chamber; and a temperature control system used for controlling the temperature at the sample cavity, so as to realize sample detection under an ultrahigh-temperature and ultralow-temperature high-pressure environment and comprising a refrigeration module and a heating module. The three functional systems are integrated together by arranging a high-temperature furnace system, a sample ultralow-temperature system and a high-pressure system into the device, the switching among the three single systems in the previous test process can be omitted, the contact between the sample and air is avoided, and the temperature control change is more continuous and stable.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of Mossbauer spectrum equipment, in particular to an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device. BACKGROUND

[0002] The Mossbauer spectrometer is a set of instruments made according to the principle of recoilless atomic nuclear resonance absorption of gamma rays. It is a uniform acceleration Mossbauer spectrometer that measures resonance absorption spectra. It can also study the internal relationship between the microscopic magnetism of magnetic materials and the macroscopic magnetism under an applied magnetic field, increase the research functions of spin structure and spin dynamics, and be used to study the electric or magnetic interaction between atomic nuclei and their surrounding environment in solid materials such as magnetic materials and high-temperature superconductors. Further research on the microscopic magnetism of surrounding atoms, electronic structure, valence state and distribution, and the properties of lattice dynamics and lattice relaxation. The Mossbauer spectrometer has the advantage of extremely high energy resolution (the highest energy resolution is 10-13eV), and is one of the powerful means for studying the hyperfine interaction and microstructure properties of matter.

[0003] At present, the measurable samples of the Mossbauer spectrometer need to be placed under high-temperature or low-temperature conditions according to different scientific research requirements, or high-pressure reaction gas is added to the sample chamber, so that the samples can be tested under different environments to measure the Mossbauer spectrum under different conditions. The influence of environmental temperature and other factors on the sample can be analyzed, or the Mossbauer spectrum can be tested under different application reaction conditions of the sample to analyze the structural properties, physical properties and chemical properties of the sample. It is most widely used in the field of catalyst research for catalytic cracking of petroleum.

[0004] However, switching between three separate systems is required in the traditional testing process, which is easy to cause the sample to come into contact with air, resulting in an impact on the results. SUMMARY

[0005] In view of the shortcomings of the prior art, the present application provides an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device, which solves the problem that switching between three separate systems is required in the traditional testing process, which is easy to cause the sample to come into contact with air, resulting in an impact on the results.

[0006] To achieve the above purpose, the present application is implemented by the following technical scheme: an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device, comprising:

[0007] a detection chamber for detecting the sample, comprising a sample chamber for containing the sample;

[0008] a vacuum system for ensuring vacuum isolation of heat conduction, comprising a vacuum chamber arranged outside the detection chamber and a vacuum pump group for maintaining the vacuum degree in the vacuum chamber;

[0009] A temperature control system for controlling the temperature at a sample chamber to achieve sample detection under ultra-high temperature and ultra-low temperature high-pressure environment, comprising a refrigeration module and a heating module.

[0010] Preferably, the refrigeration module comprises a primary cold head and a secondary cold head, the primary cold head and the secondary cold head are connected, the primary cold head is connected with a cooling device, the secondary cold head is connected with a cold copper braid, the cold copper braid is connected with a brass cold finger, the brass cold finger extends into a detection chamber, and the sample chamber is arranged on one side of the brass cold finger.

[0011] Preferably, the cooling device comprises a water-cooled unit, the water-cooled unit is connected with a helium compressor, the helium compressor is connected with a helium exchange chamber, the inlet and outlet of the helium compressor are connected on one side of the helium exchange chamber, and the helium exchange chamber is connected with the primary cold head.

[0012] Preferably, the water-cooled unit comprises a water-cooled indoor unit and a water-cooled outdoor unit, the water-cooled indoor unit is connected with the helium compressor, and the water-cooled indoor unit is used to provide water circulation cooling for the helium compressor.

[0013] Preferably, the brass cold finger is fixedly connected in the detection chamber through a boron nitride support, the heating module is arranged on one side of the boron nitride support, and the heating module comprises a heating wire arranged on one side of the boron nitride support.

[0014] Preferably, the temperature control system further comprises a control module and a detection module.

[0015] The control module is used to control the refrigeration module and the heating module to change the temperature of the sample detection environment.

[0016] The detection module is used to detect the current temperature at the sample chamber and output to the control module, and the detection module comprises a temperature sensor arranged on one side of the sample chamber.

[0017] Preferably, the vacuum chamber is connected with a fixed base, the vacuum pump group is connected on one side of the fixed base through a first corrugated pipe, the fixed base is connected with the vacuum chamber through a second corrugated pipe, and the fixed base and the vacuum chamber are connected in communication.

[0018] Preferably, the detection chamber and the vacuum chamber are both made of titanium alloy material.

[0019] Preferably, two diamond windows are arranged on the detection chamber and the vacuum chamber respectively.

[0020] Preferably, the plurality of diamond windows and the sample chamber are arranged on a straight line.

[0021] The application provides an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device.

[0022] 1、The application integrates the high-temperature furnace system, the sample ultralow-temperature system and the high-pressure system into the device, so that the switching between the three separate systems in the previous test process can be omitted, the contact between the sample and air is avoided, and the temperature control is more continuous and stable.

[0023] 2、The application isolates the vibration of the cold head through the corrugated pipe, simultaneously isolates the vacuum cavity, simultaneously utilizes the soft characteristics of the red copper braid to connect the sample chamber, guides the cold and isolates the vibration of the cold head, so that the vibration of the sample chamber can be reduced to below 1nm, even no vibration, the influence of the cold head vibration is completely removed, and it is guaranteed that the spectrum line spread difference of the Mossbauer spectrum test can meet the requirement of <0.05mm / s.

[0024] 3、The application can realize continuous conversion of different sample test conditions to measure the Mossbauer spectrum of the sample, and can also simulate an application scene to measure the Mossbauer spectrum of a sample alone. DETAILED DESCRIPTION

[0025] Figure 1 It is a schematic diagram of the overall structure of the application;

[0026] Figure 2 It is a schematic diagram of the internal structure of the detection chamber of the application.

[0027] 1, detection chamber; 11, sample cavity; 2, vacuum chamber; 21, vacuum pump set; 22, first corrugated pipe; 3, primary cold head; 31, secondary cold head; 32, cold copper braid; 33, brass cold finger; 4, helium compressor; 41, helium exchange cavity; 42, water chiller indoor unit; 43, water chiller outdoor unit; 5, boron nitride support; 6, heating wire; 7, fixed base; 71, second corrugated pipe; 8, diamond window. DETAILED DESCRIPTION

[0028] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.

[0029] Embodiment:

[0030] Please refer to the accompanying Figure 1 - the accompanying Figure 2 The embodiment of the application provides an ultrahigh-temperature and ultralow-temperature high-pressure in-situ reaction cell test device, which comprises:

[0031] a detection chamber 1 for detecting a sample, comprising a sample cavity 11 for containing the sample;

[0032] a vacuum system for ensuring vacuum isolation heat conduction, comprising a vacuum chamber 2 arranged outside the detection chamber 1 and a vacuum pump set 21 for maintaining the vacuum degree in the vacuum chamber 2;

[0033] a temperature control system for controlling the temperature at the sample cavity 11 to realize sample detection under the environment of ultrahigh temperature and ultralow temperature and high pressure, comprising a refrigeration module and a heating module.

[0034] In the embodiment, the vacuum system ensures vacuum isolation heat conduction in the sample cavity 11 by maintaining the vacuum degree outside the detection chamber 1, avoiding the influence of the external environment on the sample temperature; the temperature control system controls the temperature at the sample cavity 11 by the refrigeration module and the heating module to realize sample detection under the environment of ultrahigh temperature and ultralow temperature and high pressure; by integrating the high-temperature furnace system, the sample ultralow-temperature system and the high-pressure system into the device, the switching among the three separate systems in the previous test process can be omitted, the contact between the sample and the air is avoided, and the temperature control is more continuous and stable.

[0035] It should be noted that the device also includes some necessary components for sample detection, as follows:

[0036] 1) Host part, produced by Sidolim Company, the main function is to collect Mossbauer spectrum data;

[0037] 2) Detector Si-Pin and preamplifier, main amplifier from American company. The main function is to detect the signal of the spectrum;

[0038] 3) Spectrum analysis software, from Czech, the main function is to analyze Mossbauer spectrum data;

[0039] 4) Mossbauer radiation source from Russian RITVERC Company, the main function of this component is to excite iron atoms to produce Mossbauer spectrum effect, and then the detector can detect the Mossbauer spectrum;

[0040] 5) Multifunctional radiation dosimeter 950 from German Gamma-Scout Company. The main function is to provide radiation detection to avoid radiation damage.

[0041] In one embodiment, the refrigeration module comprises a primary cold head 3 and a secondary cold head 31, the primary cold head 3 and the secondary cold head 31 are connected, the primary cold head 3 is connected with the cooling device, the secondary cold head 31 is connected with a copper braided belt 32 for heat conduction, the copper braided belt 32 is connected with a brass cold finger 33, the brass cold finger 33 extends into the detection chamber 1, and the sample cavity 11 is arranged on one side of the brass cold finger 33;

[0042] In this embodiment, the structure of the primary cold head 3 and the secondary cold head 31 is adopted, and by connecting the two, more efficient refrigeration is achieved to ensure rapid cooling of the sample cavity 11. The primary cold head 3 is connected with the cooling device, and by means of water circulation cooling, the cooling water in the circulation is cooled and transmitted to the secondary cold head 31, further improving the cooling effect of the sample cavity 11. The copper braided belt 32 for heat conduction and the brass cold finger 33 connected with the secondary cold head 31 are used to transmit and contact the temperature inside the sample cavity 11 to achieve accurate cooling of the sample cavity 11. The brass cold finger 33 extends into the detection chamber 1 and is arranged on the side of the sample cavity 11 to ensure more accurate temperature control of the sample cavity 11. The structure design of the refrigeration module is scientific, which can maintain accurate control of the sample temperature in an ultra-low temperature environment, thereby improving the reliability and repeatability of the experiment.

[0043] On the other hand, by utilizing the soft characteristics of the copper braided belt 32 for heat conduction to connect the sample cavity 11, the vibration of the cold head can be isolated while conducting heat, and the vibration of the sample chamber can be reduced to below 1 nm or even no vibration, completely removing the influence of cold head vibration, ensuring that the mu spectrum test can meet the requirement of spectrum line broadening difference <0.05mm / s.

[0044] In one embodiment, the cooling device comprises a water chiller unit, the water chiller unit is connected with a helium compressor 4, the helium compressor 4 is connected with a helium exchange chamber 41, the inlet and outlet of the helium compressor 4 are connected on one side of the helium exchange chamber 41, and the helium exchange chamber 41 is connected with the primary cold head 3;

[0045] In this embodiment, the cooling device adopts a water chiller unit as a cold source, by connecting the primary cold head 3 in the refrigeration module with the cooling device, the cooling water is cooled and transmitted to the secondary cold head 31 to achieve rapid cooling of the sample. The water chiller unit is connected with a helium compressor 4, and the inlet and outlet of the helium compressor 4 are connected on one side of the helium exchange chamber 41. This design can convert helium into high-temperature and high-pressure gas by compressing it, and then transfer the heat in the high-temperature gas to the cooling water through the helium exchange chamber 41, thereby achieving cooling of the helium. Finally, the helium exchange chamber 41 is connected with the primary cold head 3, further realizing the cooling of the heat in the refrigeration module.

[0046] In one embodiment, the water chiller unit comprises a water chiller indoor unit 42 and a water chiller outdoor unit 43, the water chiller indoor unit 42 is connected with the helium compressor 4 to provide water circulation cooling for the helium compressor 4;

[0047] In this embodiment, the water chiller is a device that uses the evaporation of refrigerant to absorb heat in the air to cool. In the water chiller indoor unit 42, by circulating water into the water chiller condenser, the temperature is lowered by using the heat transfer between the refrigerant and the water, and the cooling water is sent back to the cooling device for use by the refrigeration module. At the same time, the water chiller outdoor unit 43 maintains the circulation of the refrigerant by discharging waste heat. In this way, the water chiller unit can stably and continuously provide cooling water, and through the water chiller cooling, it ensures that the temperature of the cooling water is stable, thereby improving the accuracy and reliability of the experimental data.

[0048] In one embodiment, the brass cold finger 33 is fixedly connected in the detection chamber 1 by the boron nitride bracket 5, and the heating module is arranged on one side of the boron nitride bracket 5. The heating module includes a heating wire 6 wound on one side of the boron nitride bracket 5.

[0049] In this embodiment, the heating wire 6 is a wire that generates heat energy by conducting current, mainly composed of high-resistance alloy wire. When current flows through, the high-resistance alloy wire generates heat, thereby increasing the temperature. In this embodiment, by winding the heating wire 6 on one side of the boron nitride bracket 5, the heating effect of the heating wire 6 can be accurately conducted to the brass cold finger 33 and the inside of the sample cavity 11.

[0050] Further, by using a bracket made of boron nitride material, the sample chamber can be fixed and the heat transfer can be isolated.

[0051] In one embodiment, the temperature control system further comprises a control module and a detection module.

[0052] The control module is used to control the refrigeration module and the heating module to change the temperature of the sample detection environment.

[0053] The detection module is used to detect the current temperature at the sample cavity 11 and output to the control module, including a temperature sensor arranged on one side of the sample cavity 11.

[0054] In this embodiment, the control module is used to control the refrigeration module and the heating module to change the temperature of the sample. Through the program in the control module, the refrigeration and heating operation can be accurately controlled according to the experimental requirements, so as to realize the accurate adjustment and control of the temperature of the sample environment.

[0055] The detection module is used to detect the current temperature at the sample cavity 11 and output to the control module. In this embodiment, the detection module includes a temperature sensor arranged on one side of the sample cavity 11. By monitoring the temperature change of the sample cavity 11 in real time, the detection module can feed back the current temperature information to the control module and make corresponding adjustment and control according to the preset program.

[0056] In one embodiment, the vacuum chamber 2 is connected with a fixed base 7, and the vacuum pump group 21 is connected with the fixed base 7 through a first bellows 22. The fixed base 7 is connected with the vacuum chamber 2 through a second bellows 71, and the fixed base 7 is in communication with the vacuum chamber 2;

[0057] In this embodiment, the fixed base 7 is a device that is in communication with the vacuum chamber 2 through the second bellows 71, and it plays a supporting and connecting role in the experiment. At the same time, the fixed base 7 is connected with the vacuum pump group 21 through the first bellows 22, which is used to extract the gas inside the vacuum chamber 2. The vacuum pump group 21 is a device that uses mechanical or physical methods to extract gas, and it usually extracts gas into the vacuum pump through the pipeline, and continuously reduces the pressure of the gas through continuous compression and expansion;

[0058] In this embodiment, the first bellows 22 and the second bellows 71 are both vacuum bellows;

[0059] On the other hand, the fixed base 7 and the vacuum chamber 2 are connected through the second bellows 71, which isolates the vibration of the cold head and also isolates the vacuum cavity.

[0060] In one embodiment, the detection chamber 1 and the vacuum chamber 2 are both made of titanium alloy material;

[0061] In this embodiment, titanium alloy is a metal material with high strength and good corrosion resistance, and it has high physical properties and chemical stability, so it is widely used in laboratory equipment. The detection chamber 1 and the vacuum chamber 2 are both important experimental environment components, so titanium alloy material is used to improve its corrosion resistance and high temperature resistance.

[0062] In the laboratory environment, common gases such as oxygen and nitrogen can cause serious corrosion and pollution to experimental equipment. Titanium alloy has low oxidation and occlusion ability, which can effectively resist gas corrosion and protect the stability and durability of experimental equipment.

[0063] In addition, titanium alloy also has good high temperature resistance, which can maintain its high strength and stability at high temperature. This feature is very important for applications that need to be tested in high temperature environment.

[0064] In one embodiment, two diamond windows 8 are arranged on the detection chamber 1 and the vacuum chamber 2 respectively;

[0065] In this embodiment, diamond is an extremely hard and corrosion resistant material, and is a good choice for manufacturing the diamond window 8. In the experiment, by processing the diamond into a thin sheet or a semi-spherical shape, and then fixing it on the vacuum chamber 2 or the detection chamber, reliable sealing and interface connection of the experimental environment can be achieved, while allowing the signal to penetrate and transmit. Two diamond windows 8 are arranged on the detection chamber 1 and the vacuum chamber 2 respectively, through which the signal can be transmitted inside the detection chamber and the vacuum chamber 2, so as to monitor and test the sample inside the sample cavity 11.

[0066] In one embodiment, the plurality of diamond windows 8 and the sample cavity 11 are arranged in a straight line.

[0067] In this embodiment, the diamond windows 8 of the detection chamber and the vacuum chamber 2 are automatically aligned in a straight line, which is very conducive to the combination with the Mossbauer spectrometer.

[0068] In one embodiment, in use, the method is to place the catalyst powder on the sample tablet press, press the sample into a sheet with a diameter of 10 mm and a thickness of 0.5-2 mm, place it into the sample cavity 11 and fix it, introduce the redox gas to cause in-situ reaction, control the temperature in the set range and the pressure in the set range, then start testing and collecting Mossbauer spectrum data, complete a sample test, then change the temperature and pressure test conditions, measure and collect the Mossbauer spectrum again, and finally complete the measurement of the Mossbauer spectrum of a sample.

[0069] Although embodiments of the present application have been shown and described, it is to be understood that various modifications, substitutions, replacements and variations can be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. An ultrahigh temperature and ultralow temperature high pressure in-situ reaction cell test apparatus, characterized in that, The utility model relates to a high pressure vacuum cryogenic sample detection device, including: a detection chamber (1) for detecting a sample, comprising a sample cavity (11) for containing the sample; a vacuum system for ensuring vacuum isolation heat conduction, comprising a vacuum chamber (2) arranged outside the detection chamber (1) and a vacuum pump set (21) for maintaining the vacuum degree in the vacuum chamber (2); a temperature control system for controlling the temperature at the sample cavity (11) to realize sample detection under ultra-high temperature and ultra-low temperature high pressure environment, comprising a refrigeration module and a heating module; the refrigeration module comprises a primary cold head (3) and a secondary cold head (31), the primary cold head (3) and the secondary cold head (31) are connected, the primary cold head (3) is connected with a cooling device, the secondary cold head (31) is connected with a cold copper braid (32), the cold copper braid (32) is connected with a brass cold finger (33), the brass cold finger (33) extends into the detection chamber (1), and the sample cavity (11) is arranged on one side of the brass cold finger (33); the brass cold finger (33) is fixedly connected in the detection chamber (1) through a boron nitride support (5), the heating module is arranged on one side of the boron nitride support (5), and the heating module comprises a heating wire (6) arranged on one side of the boron nitride support (5); the vacuum chamber (2) is connected with a fixed base (7), the vacuum pump set (21) is connected on one side of the fixed base (7) through a first bellows (22), the fixed base (7) is connected with the vacuum chamber (2) through a second bellows (71), and the fixed base (7) is communicated with the vacuum chamber (2).

2. The apparatus of claim 1, wherein, the cooling device comprises a water-cooled unit, the water-cooled unit is connected with a helium compressor (4), the helium compressor (4) is connected with a helium exchange cavity (41), the inlet and outlet of the helium compressor (4) are connected on one side of the helium exchange cavity (41), and the helium exchange cavity (41) is connected with the primary cold head (3).

3. The apparatus of claim 2, wherein the apparatus is configured to perform a high pressure in-situ reaction cell test at ultra-high temperature and ultra-low temperature. the water-cooled unit comprises a water-cooled indoor unit (42) and a water-cooled outdoor unit (43), the water-cooled indoor unit (42) is connected with the helium compressor (4) and is used to provide water circulation cooling for the helium compressor (4).

4. An ultrahigh and ultra-low temperature high pressure in-situ reaction cell test apparatus according to any one of claims 1-3, characterized in that, the temperature control system further comprises a control module and a detection module; the control module is used for controlling the refrigeration module and the heating module to change the temperature of the sample detection environment; the detection module is used for detecting the current temperature at the sample cavity (11) and outputting to the control module, comprising a temperature sensor arranged on one side of the sample cavity (11).

5. The apparatus of claim 1, wherein the apparatus is configured to perform in-situ reaction cell testing of ultra-high temperature and ultra-low temperature high pressure fluids. The detection chamber (1) and the vacuum chamber (2) are both made of titanium alloy material.

6. The ultra-high and cryogenic high-pressure in-situ reaction cell test apparatus of claim 5, wherein, Two diamond windows (8) are oppositely arranged on the detection chamber (1) and the vacuum chamber (2).

7. An ultrahigh and ultra-low temperature high pressure in-situ reaction cell test apparatus according to claim 6, wherein, The plurality of diamond windows (8) and the sample cavity (11) are arranged on a straight line.

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