Low-temperature packaging device for low-boiling-point substances in diamond anvil cell

Abstract

The invention belongs to the technical field of condensation packaging, and provides a low-temperature packaging device for low-boiling-point substances in diamond anvil cells, which comprises a refrigerant storage container, a press placing cylinder is detachably mounted at the inner top of the refrigerant storage container, and a press body is placed in the press placing cylinder. A sealing cover body is hermetically connected to the top end of the pressing machine placing cylinder and is positioned right above the pressing machine body; the sealing cover body is matched with the pressing machine body for use; in the packaging process, the temperature measuring point of the refrigerant storage container is controlled to be at the boiling point temperature of the refrigerant all the time to ensure the refrigeration efficiency, and if the temperature measuring point at the position of the corresponding height of the sample cavity just reaches the liquefaction temperature of the low-boiling-point substance, the liquid level of the target sample just reaches the height of the sample cavity of the diamond anvil cell press; in addition, a second temperature measuring point of the pressing machine placing barrel monitors whether the liquid level of the sample is too high or not, and standard pressure substances and other solid samples which are loaded in the sample cavity in advance and needed by the experiment are prevented from being washed away.

Description

Technical Field

[0001] The invention belongs to the technical field of condensation packaging, in particular to a low-temperature condensation packaging device based on a diamond anvil cell experiment. Background Art

[0002] The commonly used method for loading low-boiling-point material samples in diamond anvil press is the high-pressure gas filling method. However, the limitation of the high-pressure gas filling device is that some high-risk gases are flammable and explosive or toxic and volatile in high concentrations, which cannot meet the sample packaging requirements of all low-boiling-point materials in the high-pressure experiment of diamond anvil press.

[0003] In conventional low-temperature packaging operations, the refrigerant is constantly consumed and vaporized at room temperature, and the liquid level of the refrigerant also needs to be controlled. If the refrigerant is too little, the refrigeration efficiency will be compromised and the liquefied sample will boil and vaporize, washing away the solid sample and standard pressure material in the sample cavity. If the refrigerant is excessive, the screws and lid connections on the sealed container may be frozen, making it difficult to perform packaging operations. In addition, the following problems may occur: if there are pre-loaded solid samples or standard pressure material rubies in the sample cavity, they can easily be washed away by the target packaged sample in a liquefied state that cannot be observed and controlled, or in a sealed state, the liquid level of the unobservable target sample has not reached the height of the sample cavity before the packaging operation is performed. There is no integrated equipment to ensure that these problems can be effectively controlled when they are observed, which seriously affects the packaging success rate and experimental efficiency.

[0004] To this end, those skilled in the art have proposed a low-boiling point material low-temperature packaging device in a diamond anvil to solve the problems raised in the background art. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a low-temperature condensation packaging device based on a diamond anvil cell experiment to solve the problems in the prior art that the amount of refrigerant cannot be effectively controlled, resulting in the boiling and vaporization of the liquefied sample, washing away the solid sample and standard pressure material in the sample cavity, or freezing the connection between the screws and the lid on the sealed container, making it difficult to perform the packaging operation; and the problem that the degree of liquefaction of the target low-boiling point substance sample cannot be observed and controlled, resulting in packaging failure.

[0006] A low-boiling point material low-temperature packaging device in a diamond anvil comprises a refrigerant storage container, a press placement cylinder is detachably mounted on the inner top of the refrigerant storage container, a press body is placed inside the press placement cylinder, a sealing cover body is sealedly connected to the top of the press placement cylinder and located directly above the press body, and the sealing cover body is used in conjunction with the press body.

[0007] Preferably, it also includes a vacuum compressor, to which a delivery pipe is fixedly connected, an air valve is installed on the delivery pipe, and one end of the delivery pipe away from the vacuum compressor is fixedly connected to the center position of the sealing cover body.

[0008] Preferably, it also includes a sample gas cylinder, which is fixedly connected to an air pipe, and the end of the air pipe away from the sample gas cylinder passes through the refrigerant storage container and extends to the interior of the refrigerant storage container. The end of the air pipe away from the sample gas cylinder is fixedly connected to a mosquito coil, and the mosquito coil is located on the inner bottom surface of the refrigerant storage container. The end of the mosquito coil away from the air pipe is inserted into the interior of the corresponding compressor body, and the shape of the mosquito coil is designed to increase contact with the refrigerant.

[0009] Preferably, it also includes a first temperature measuring connecting line, a second temperature measuring connecting line and a third temperature measuring connecting line, and the ends of the first temperature measuring connecting line, the second temperature measuring connecting line and the third temperature measuring connecting line are correspondingly connected with temperature measuring points.

[0010] Preferably, four hexagonal screw columns are installed at the bottom of the sealing cover body, which are just aligned with the four screw holes on the press body, so as to seal the sample cavity conveniently during sealing.

[0011] Preferably, four hexagonal screw columns are installed at the bottom of the sealing cover body, which are just aligned with the four screw holes on the press body, so as to seal the sample cavity conveniently during sealing.

[0012] Preferably, a refrigerant inlet is provided on the top of the refrigerant storage container, and a circular hole is also provided on the top of the refrigerant storage container.

[0013] Preferably, the press body includes an upper press, a lower press is arranged directly below the upper press and cooperates with the upper press, a first pad is installed inside the upper press, a second pad is installed inside the lower press, an anvil diamond a is arranged at the middle position of the bottom of the first pad, and an anvil diamond b is arranged at the middle position of the top of the second pad.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] The present invention can realize multiple gas washing operations by setting a vacuum compressor, a sample gas connection and a gas valve to ensure the purity of the target low-boiling point material sample. Through three thermocouple probes, two temperature measuring points are placed in the press placement cylinder at the position corresponding to the height of the diamond anvil press sample chamber of standard specifications and at a fixed position above it, and one temperature measuring point is placed at the corresponding height of the refrigerant storage container. During the packaging process, the temperature measuring point of the refrigerant storage container is controlled to always be at the boiling point of the refrigerant to ensure the refrigeration efficiency. If the temperature measuring point at the position corresponding to the height of the sample chamber just reaches the liquefaction temperature of the low-boiling point material, it means that the liquid level of the target sample just reaches the height of the sample chamber of the diamond anvil press, and the packaging operation can be performed. In addition, the second temperature measuring point of the press placement cylinder monitors whether the sample liquid level is too high to prevent the standard pressure material and other solid samples required for the experiment loaded in advance in the sample chamber from being washed away. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic structural diagram of a low-temperature condensation packaging device based on a diamond anvil cell experiment of the present invention;

[0017] Figure 2 It is a schematic diagram of the structure of the press placement cylinder and the sealing cover body of the present invention;

[0018] Figure 3 It is a schematic structural diagram of the press body and the sealing cover body of the present invention;

[0019] Figure 4 It is a structural schematic diagram of the press body of the present invention;

[0020] Figure 5 This is a schematic diagram of observing the sample of the present invention through an optical microscope and taking pictures and recording them by CCD.

[0021] In the figure: 1. refrigerant storage container; 2. press placement cylinder; 3. press body; 301. upper press; 302. lower press; 303. first cushion block; 304. second cushion block; 305. diamond anvil a; 306. diamond anvil b; 4. sealing cover; 5. vacuum compressor; 6. delivery pipe; 7. sample gas cylinder; 8. gas delivery pipe; 9. mosquito coil; 10. first temperature measurement connecting line; 11. second temperature measurement connecting line; 12. third temperature measurement connecting line. DETAILED DESCRIPTION

[0022] The following embodiments of the present invention are described in further detail in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0023] As attached Figure 1 To Attachment Figure 5 As shown:

[0024] Embodiment 1:

[0025] The present invention provides a low-boiling-point substance low-temperature packaging device in a diamond anvil, comprising: a low-boiling-point substance low-temperature packaging device in a diamond anvil, the device comprising a refrigerant storage container 1, a press placement cylinder 2 is detachably mounted on the inner top of the refrigerant storage container 1, a press body 3 is placed inside the press placement cylinder 2, a sealing cover 4 is sealed and connected to the top of the press placement cylinder 2 and located directly above the press body 3, and the sealing cover 4 is used in conjunction with the press body 3;

[0026] It also includes a vacuum compressor 5, to which a delivery pipe 6 is fixedly connected, and an air valve is installed on the delivery pipe 6, and one end of the delivery pipe 6 away from the vacuum compressor 5 is fixedly connected to the center of the sealing cover 4;

[0027] It also includes a sample gas cylinder 7, the sample gas cylinder 7 is fixedly connected to an air pipe 8, the end of the air pipe 8 away from the sample gas cylinder 7 passes through the refrigerant storage container 1 and extends to the inside of the refrigerant storage container 1, the end of the air pipe 8 away from the sample gas cylinder 7 is fixedly connected to a mosquito coil 9, the mosquito coil 9 is located on the inner bottom surface of the refrigerant storage container 1, the end of the mosquito coil 9 away from the air pipe 8 is plugged into the corresponding compressor body 3, and the shape of the mosquito coil 9 is designed to increase contact with the refrigerant;

[0028] Four hexagonal screw columns are installed at the bottom of the sealing cover 4, which are aligned with the four screw holes on the press body 3, so as to seal the sample cavity conveniently;

[0029] A refrigerant inlet is provided on the top of the refrigerant storage container 1 , and a round hole is also provided on the top of the refrigerant storage container 1 . The purpose of providing the round hole is to vaporize the refrigerant and facilitate gas discharge.

[0030] The press body 3 includes an upper press 301, a lower press 302 cooperating with the upper press 301 is arranged directly below the upper press 301, a first cushion block 303 is installed inside the upper press 301, a second cushion block 304 is installed inside the lower press 302, a diamond anvil a305 is arranged at the middle position of the bottom of the first cushion block 303, and a diamond anvil b306 is arranged at the middle position of the top of the second cushion block 304;

[0031] Through pre-pressing with two pairs of diamond anvils, the gasket produces an indentation in the shape of a diamond side edge and becomes thinner in the center. The thinner area in the center has the same shape and area as the diamond anvil surface. A micron-sized hole is punched in this area through laser drilling. This small hole is the sample cavity of the experiment. The two diamond anvil surfaces are the upper and lower surfaces of the sample cavity. After pre-pressing, the thickness of the gasket is the height of the sample cavity, and the diameter of the sample cavity is only 100 to 500μm.

[0032] Working principle: The present invention can perform a vacuum operation on the interior of the compressor cylinder 2 by setting a vacuum compressor 5. By installing a temperature measuring point just above the sample cavity, if the temperature measuring probe just reaches the liquefaction temperature of oxygen, it means that it just passes. Another temperature measuring point is installed around the temperature measuring point, indicating that the liquid level is not too high, otherwise it is easy to be washed away. Temperature measuring points are installed at the same liquid level height to monitor the amount of refrigerant.

[0033] Embodiment 2: In this embodiment, the low boiling point substance of the present invention is used to perform oxygen packaging operation on the sleeve diamond anvil in the low temperature packaging device in the diamond anvil. A ruby ​​is placed in the sample cavity on the diamond 306 anvil surface of the lower press 302 part in the sample cavity of the diamond anvil press. The ruby ​​pressure calibration method is used to monitor the pressure in the sample cavity for subsequent experiments. The specific operation process is as follows:

[0034] In this embodiment, the anvil surface diameter of the diamond anvil press device 3 used is 400 μm, a rhenium foil with a thickness of 250 μm is pre-pressed to 40 μm, a hole with a diameter of 200 μm is punched in the center of the indentation with a laser beam as a sample cavity, a ruby ​​microsphere with a diameter of 10 μm is loaded into the sample cavity to calibrate the pressure in the sample cavity, and then the diamond anvil press 3 is closed and placed in the press placement tube 2, and the four hexagonal screw columns at the bottom of the sealing cover 4 are aligned with the four screw holes on the press device 3 and the press placement tube is sealed. Connect the vacuum compressor 7 and the high-purity oxygen cylinder 5 to Figure 1Position in the middle, close the valve, open the oxygen cylinder, and turn on the compressor. Open the compressor pipeline valve 6 to perform the vacuum operation in the compressor placement cylinder; close the compressor pipeline valve 6, open the oxygen cylinder pipeline valve 8, and fill the compressor placement cylinder with oxygen. Perform the above operations multiple times to wash the compressor placement cylinder 2 to achieve high purity of the target sample. Turn the four hexagonal screws on the sealing cover body according to the loosening direction of the four screws that control the pressure of the diamond anvil press 3 to open the sample cavity in the press cavity; place an appropriate amount of refrigerant into the refrigerant storage container 1 while monitoring whether the first temperature measuring point 10 reaches the boiling point of the refrigerant, and open the oxygen cylinder pipeline valve 8 to continue to fill the compressor placement cylinder 2 with oxygen to perform low-temperature condensation operations on the target sample. At this time, the temperature measuring point continues to decrease from room temperature, and observe whether the second temperature measuring point 11 reaches the oxygen boiling point. If it reaches the oxygen boiling point near -182.95°C, close the oxygen pipeline valve 8 before the third temperature measuring point 12 reaches the oxygen boiling point. Turn the four hexagonal screws on the sealing cover 4 in the tightening direction of the four screws that control the pressure of the diamond anvil press 3 to perform the packaging operation, so as to close the sample cavity in the press cavity and complete the packaging of the target sample. At this point, the sample packaging of the diamond anvil low-boiling point substance is completed. Observe through an optical microscope and record with CCD. Figure 5 It can be observed that the sample cavity is filled with light blue liquid, and there is a 10μm ruby ​​microsphere in the lower left corner of the sample cavity, accompanied by filamentous stripes. This is due to the partial solidification of oxygen under pressure conditions, which proves that the sample packaging operation of low-boiling-point materials on the diamond anvil press device with ruby ​​microspheres of standard pressure materials placed in advance was successful.

[0035] The embodiments of the present invention are provided for the purpose of illustration and description. Although the embodiments of the present invention have been shown and described above, it can be understood that the above embodiments are exemplary and cannot be understood as limitations of the present invention. Ordinary technicians in this field can change, modify, replace and modify the above embodiments within the scope of the present invention.

Claims

1. A low-boiling point material low-temperature packaging device in a diamond anvil cell, characterized in that: The invention comprises a refrigerant storage container (1), wherein a press placement cylinder (2) is detachably mounted on the inner top of the refrigerant storage container (1), a press body (3) is placed inside the press placement cylinder (2), and a sealing cover body (4) is sealedly connected to the top of the press placement cylinder (2) and located directly above the press body (3), and the sealing cover body (4) is used in conjunction with the press body (3).

2. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 1, characterized in that: It also comprises a vacuum compressor (5), to which a delivery pipe (6) is fixedly connected, and an air valve is installed on the delivery pipe (6), and one end of the delivery pipe (6) away from the vacuum compressor (5) is fixedly connected to the center position of the sealing cover body (4).

3. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 2, characterized in that: It also includes a sample gas cylinder (7), the sample gas cylinder (7) is fixedly connected to an air pipe (8), the end of the air pipe (8) away from the sample gas cylinder (7) passes through the refrigerant storage container (1) and extends to the interior of the refrigerant storage container (1), the end of the air pipe (8) away from the sample gas cylinder (7) is fixedly connected to a mosquito coil (9), the mosquito coil (9) is located on the inner bottom surface of the refrigerant storage container (1), the end of the mosquito coil (9) away from the air pipe (8) is inserted into the interior of the corresponding compressor body (3), and the shape of the mosquito coil (9) is designed to increase contact with the refrigerant.

4. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 3, characterized in that: It also comprises a first temperature measurement connecting line (10), a second temperature measurement connecting line (11) and a third temperature measurement connecting line (12), wherein the ends of the first temperature measurement connecting line (10), the second temperature measurement connecting line (11) and the third temperature measurement connecting line (12) are correspondingly connected with temperature measurement points.

5. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 4, characterized in that: Four hexagonal screw columns are installed at the bottom of the sealing cover (4), which are aligned with the four screw holes on the press body (3) to facilitate sealing the sample cavity during sealing.

6. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 5, characterized in that: A refrigerant inlet is provided on the top of the refrigerant storage container (1), and a circular hole is also provided on the top of the refrigerant storage container (1).

7. The low-boiling point material low-temperature packaging device in a diamond anvil as claimed in claim 6, characterized in that: The press body (3) comprises an upper press (301), a lower press (302) cooperating with the upper press (301) is arranged directly below the upper press (301), a first cushion block (303) is installed inside the upper press (301), a second cushion block (304) is installed inside the lower press (302), a diamond anvil a (305) is arranged at the middle position of the bottom of the first cushion block (303), and a diamond anvil b (306) is arranged at the middle position of the top of the second cushion block (304).

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