A visual and controllable pressurization system based on diamond anvil cell and a method of using the same

Abstract

The present application relates to the technical field of diamond anvil cell pressurization, and particularly discloses a visible and controllable pressurization system based on a diamond anvil cell and a use method thereof, which solves the problem that the pressurization process of the diamond anvil cell cannot be observed and controlled accurately in the prior art. The system comprises a diamond anvil cell, the diamond anvil cell is installed on a fixing device, and a pressure detection assembly for obtaining the pressure in a sample cavity of the diamond anvil cell and a pressurization detection assembly for obtaining the pressurization state of the diamond anvil cell are arranged above the diamond anvil cell. The present application has the advantages that the pressurization process is visualized and controllable, the phenomena such as sample cavity deviation, deformation and liquid leakage of the diamond anvil cell are avoided, the uncontrollable problem of target pressure and pressurization step length is solved, and the experimental precision and success rate are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of diamond anvil cell pressurization, in particular to a visible and controllable pressurization system based on diamond anvil cell and a method of using the same. BACKGROUND

[0002] Diamond anvil cell is an ultra-high pressure experimental device capable of generating pressure on the order of millions of atmospheres (GPa), with the advantages of small size, easy operation and high safety, and is one of the most important experimental instruments in the field of high pressure science. Diamond anvil cell combined with modern instrumental analysis technology can make in-situ measurements and research on the structure and properties of matter under ultra-high pressure conditions, and can observe new phenomena and laws that cannot be observed under normal pressure. Diamond anvil cell is a device that generates ultra-high pressure environment for the sample in the sample chamber by pressing two oppositely placed diamond anvils, thinning the metal sealing gasket with a small hole in the middle, and then obtaining an ultra-high pressure environment for the sample in the small hole (sample chamber).

[0003] Generally, the experimental personnel adopts the way of symmetric, step-by-step and multiple rotation of the pressurizing bolts to pressurize the diamond anvil cell, so that the sample chamber generates high pressure. However, the symmetric, step-by-step and multiple rotation of the pressurizing bolts has serious deficiencies. The specific deficiencies are as follows: it is difficult to keep the same rotation angle of the pair of pressurizing bolts when symmetrically pressurizing, which easily leads to the sample chamber to be offset; it is difficult to keep the same rotation angle of the two pairs of pressurizing bolts when step-by-step pressurizing, which easily leads to the sample chamber to be deformed; the rotation angle deviation of the four pressurizing bolts becomes larger and larger when multiple pressurizing, which easily leads to the sample chamber to leak. Most importantly, the diamond anvil cell is pressurized by the above-mentioned pressurizing method, which can only make the sample chamber close to the target pressure, but cannot accurately reach the target pressure.

[0004] In view of the above problems, the patent with publication number 201810304022.5 discloses a four-axis linkage pressurization equipment based on diamond anvil cell press, which uses four motors to link and rotate the pressurizing bolts at the same time, and realizes uniform pressurization of the diamond anvil cell by inputting the same torque. However, the device cannot observe the pressurization state in-situ when pressurizing the diamond anvil cell, so it cannot effectively avoid the sample chamber offset, deformation and leakage and other phenomena that may occur during the pressurization process. In addition, the device cannot real-time monitor and accurately control the pressurization process of the diamond anvil cell, and cannot effectively control the pressure in the sample chamber and the pressurization step length during the pressurization process. SUMMARY

[0005] The present application provides a visible and controllable pressurization system based on diamond anvil cell and a method of using the same, which solves the problem that the pressurization process of the diamond anvil cell cannot be real-time monitored and accurately controlled in the prior art.

[0006] The technical solution of the present application is implemented as follows:

[0007] A visible and controllable pressurization system based on a diamond anvil cell, comprising a diamond anvil cell, the diamond anvil cell is installed on a fixing device, an upper side of the diamond anvil cell is provided with a pressure detection assembly for obtaining the pressure in a sample cavity of the diamond anvil cell and a pressurization detection assembly for obtaining the pressurization state of the diamond anvil cell. The pressure detection assembly is a microscopic laser Raman spectrometer, which can realize real-time observation of the sample cavity in the diamond anvil cell and simultaneously collect the fluorescence spectrum of the ruby microsphere in the sample cavity, and the pressure in the sample cavity is determined according to the position of the characteristic fluorescence peak center wavelength of the ruby microsphere. The pressurization detection assembly is a Michelson interferometer, the movable mirror in the Michelson interferometer is connected with the diamond anvil cell, and the angle of the movable mirror is adjusted to make the Michelson interferometer generate a regular equal-inclination interference ring. During pressurization, the rotation angles of the four pressurization bolts are coordinated and controlled to keep the center position of the equal-inclination interference ring unchanged, so that the diamond anvil cell is uniformly pressurized; meanwhile, the number of the equal-inclination interference ring and the change amount of the position of the characteristic fluorescence peak center wavelength of the ruby microsphere are controlled to make the diamond anvil cell realize accurate pressurization and equal-step pressurization.

[0008] The pressure detection assembly comprises a microscope for focusing and imaging the sample cavity in the diamond anvil cell and a Raman spectrometer for collecting the fluorescence spectrum of the ruby microsphere in the sample cavity, the microscope is located directly above the diamond anvil cell, the microscope is connected with the Raman spectrometer, and the microscope and the Raman spectrometer are respectively connected with a computer. The microscope can present the image of the sample cavity on the display screen of the computer, so that the operator can realize real-time observation of the state of the sample cavity; the Raman spectrometer presents the collected fluorescence spectrum of the ruby microsphere on the display screen of the computer, so that the operator can realize real-time acquisition of the pressure in the sample cavity in the diamond anvil cell.

[0009] The diamond anvil cell comprises two parallel arranged upper and lower support blocks, the upper side of the upper support block is provided with an annular iron sheet, the lower side of the upper support block is provided with an upper supporting block, the upper side of the lower support block is provided with a lower supporting block, the upper and lower supporting blocks are arranged oppositely between the upper and lower supporting blocks, the upper and lower diamond anvils are arranged between the upper and lower supporting blocks, a metal sealing gasket is arranged between the upper and lower diamond anvils, a small hole is arranged on the metal sealing gasket, the space formed by the small hole, the upper diamond anvil and the lower diamond anvil is the sample cavity of the diamond anvil cell, and the upper and lower support blocks are connected through a plurality of pressurization bolts. Rotating the pressurization bolts can reduce the distance between the upper and lower support blocks, so as to compress the volume of the sample cavity to generate high pressure and realize the pressurization of the sample in the sample cavity.

[0010] A spring sheet is arranged on the pressurization bolt and located between the upper support block and the head of the pressurization bolt. The spring sheet can ensure that the pressurization bolt pressurizes the upper support block stably.

[0011] The pressurization detection assembly is a Michelson interferometer, which comprises a cross bracket and a movable mirror, the cross bracket is fixedly provided with a laser, a beam splitter, a compensation plate, a fixed mirror and a camera, the movable mirror is fixed on the diamond anvil cell through a connecting frame, the movable mirror is arranged in parallel with the upper surface of the upper support block of the diamond anvil cell, and the camera is connected with a computer. The laser is installed at the left end of the cross bracket, the fixed mirror is installed at the right end of the cross bracket, the camera is installed at the upper end of the cross bracket, the beam splitter is installed at the center of the cross bracket and is placed at an angle of 45 degrees, the compensation plate is installed between the beam splitter and the fixed mirror and is placed at an angle of 45 degrees, and the movable mirror is located at the lower end of the cross bracket. The camera can collect the isoclinal interference ring after the laser emits the laser, and the isoclinal interference ring can be displayed on the display screen of the computer.

[0012] The connecting frame comprises a ring magnet and a connecting rod, the ring magnet is adsorbed on the ring-shaped iron sheet on the upper side of the upper support block of the diamond anvil cell, one end of the connecting rod is connected with the ring magnet, and the other end of the connecting rod is connected with the movable mirror.

[0013] The fixing device comprises a support frame, the upper part of the support frame is provided with a working cavity for placing the diamond anvil cell, the side wall of the working cavity is provided with a fastening screw, and the fastening screw extends into the working cavity to lock the lower support block of the diamond anvil cell. The length of the fastening screw extending into the working cavity can be adjusted by rotating the fastening screw, so that the relative position of the diamond anvil cell in the working cavity can be adjusted.

[0014] The bottom of the working cavity is provided with an illumination hole, and the lower part of the support frame is provided with an illumination device facing the illumination hole. The illumination device can shoot the light source from directly below the working cavity, which is convenient for the microscope to observe the sample cavity.

[0015] The lower end of the support frame is provided with an ear seat, and the ear seat is provided with a fixing screw. The support frame is fixed on the optical platform through the fixing screw and the ear seat, so that the fixing device remains stable, and the diamond anvil cell remains stable during the pressurization process.

[0016] A use method of a visible and controllable pressurization system based on a diamond anvil cell, comprising the following steps:

[0017] Step S1: placing the diamond anvil cell, which is previously provided with a ruby microsphere, a pressure transmission medium and a sample, into the working cavity of the fixing device; the pressure transmission medium is silicone oil, which provides a hydrostatic pressure environment for the sample cavity, and the ruby microsphere is used to calibrate the pressure of the sample cavity;

[0018] Step S2: fixing the diamond anvil cell by using the fastening screw on the side of the working cavity and adjusting the position of the diamond anvil cell in the working cavity, so that the sample cavity is located in the field of view of the microscope and is aligned with the ruby microsphere in the sample cavity;

[0019] Step S3: observing and focusing the sample cavity in the diamond anvil cell by using the microscope, and displaying the image on the display screen of the computer;

[0020] Step S4: collecting the fluorescence spectrum of the ruby microsphere in real time by using the continuous spectrum collection function of the Raman spectrometer, displaying the fluorescence spectrum on the display screen of the computer, and determining the initial pressure of the sample cavity according to the position of the characteristic fluorescence peak center wavelength;

[0021] Step S5: adsorbing the annular magnet on the annular iron sheet, connecting the connecting frame with the upper support block of the diamond anvil cell, fixing the movable mirror in the Michelson interferometer on the connecting frame, adjusting the angle of the movable mirror to make the Michelson interferometer generate a regular isoclinal interference ring, and displaying it on the computer display screen;

[0022] Step S6: rotating the pressure screw to pressurize the diamond anvil cell, during the pressurization process, the rotation angles of the four pressure screws are coordinated and controlled to keep the center position of the isoclinal interference ring unchanged; at the same time, the fluorescence spectrum of the ruby microsphere is collected by using the continuous spectrum collection function of the Raman spectrometer to obtain the pressure in the sample cavity in real time until the target pressure is reached;

[0023] Step S7: during the pressurization process, the angle increment of the pressure screw is controlled, and then the throughput of the isoclinal interference ring and the position change amount of the characteristic fluorescence peak center wavelength of the ruby microsphere are controlled, so as to realize the incremental control of the pressure of the sample cavity, and finally complete the pressurization experiment with equal step length.

[0024] The beneficial effects of the present application are:

[0025] 1. The present application realizes the visualization and controllability of the pressurization process, avoids the possible offset, deformation and liquid leakage of the sample cavity in the diamond anvil cell, solves the uncontrollable problem of target pressure and pressurization step length, and improves the precision and success rate of the experiment. The microscope can observe the sample cavity in real time, the Raman spectrometer can measure the pressure in the sample cavity in real time, and the Michelson interferometer can monitor the pressurization state in real time. During pressurization, the use of the microscope to observe the sample cavity can avoid the offset, deformation and liquid leakage of the sample cavity in the diamond anvil cell; the use of the Raman spectrometer to collect the fluorescence spectrum of the ruby can monitor the position of the characteristic fluorescence peak center wavelength of the ruby, and the pressure in the sample cavity in the diamond anvil cell can be obtained; the use of the Michelson interferometer to generate the isoclinal interference ring can coordinate and control the rotation angles of the four pressure screws to keep the center position of the isoclinal interference ring unchanged, and the uniform pressurization of the diamond anvil cell can be realized; by controlling the rotation angle of the pressure screw, the throughput of the isoclinal interference ring and the position change amount of the characteristic fluorescence peak center wavelength of the ruby can be controlled, and then the pressurization step length in the pressurization process can be controlled.

[0026] 2. The present application can observe the sample cavity during the rotation of the pressurizing bolt, realize the visualization of the pressurizing process, and effectively avoid the sample cavity from being offset, deformed and leaking.

[0027] 3. The present application can judge whether the diamond anvil cell is uniformly pressurized during the pressurizing process by observing whether the center position of the isogyric interference ring changes, and effectively solve the problems of the sample cavity being offset, deformed and leaking.

[0028] 4. The present application can accurately control the pressure of the sample cavity by controlling the rotation angle of the pressurizing bolt, observing the number of the isogyric interference ring and monitoring the position of the center wavelength of the ruby characteristic fluorescence peak, and then can achieve the target pressure.

[0029] 5. The present application can accurately control the pressure increment of the sample cavity by controlling the rotation angle of the pressurizing bolt, observing the number of the isogyric interference ring and monitoring the position change of the center wavelength of the ruby characteristic fluorescence peak, and then can achieve the equal step pressurization. BRIEF DESCRIPTION OF DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description only some embodiments of the present application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of these drawings.

[0031] Figure 1 It is a structure schematic diagram of the present application based on the diamond anvil cell visual controllable pressurizing system.

[0032] Figure 2 It is a vertical sectional view of the fixing device.

[0033] Figure 3 It is a horizontal sectional view of the fixing device.

[0034] Figure 4 It is a structure schematic diagram of the diamond anvil cell.

[0035] Figure 5 It is a structure schematic diagram of the Michelson interferometer.

[0036] Figure 6 It is the fluorescence spectrum of the ruby.

[0037] Figure 7 It is a schematic diagram of the isogyric interference ring.

[0038] In the diagram: 1-Fixing device, 11-Support frame, 12-Ear seat, 13-Fixing screw, 14-Lighting device, 15-Working chamber, 16-Fastening screw, 17-Lighting hole, 2-Diamond anvil, 21-Pressure bolt, 22-Spring plate, 23-Upper support block, 24-Upper support block, 25-Upper diamond anvil, 26-Metal sealing gasket, 27-Lower diamond anvil, 28-Lower support block, 29-Lower support block, 3-Connecting frame, 31-Ring magnet, 32-Connecting rod, 4-Michelson interferometer, 41-Laser, 42-Beam splitter, 43-Compensation plate, 44-Fixed reflector, 45-Modible reflector, 46-Camera, 5-Microscope, 6-Raman spectrometer, 7-Computer. Detailed Implementation

[0039] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0040] Example 1, as Figure 1 As shown, a visually controllable pressurization system based on a diamond anvil cell includes a diamond anvil cell 2, which is mounted on a fixing device 1. Above the diamond anvil cell 2, there is a pressure detection component for acquiring the pressure of the sample cavity within the diamond anvil cell 2, and a pressurization detection component for acquiring the pressurization state of the diamond anvil cell 2. The pressure detection components can acquire images of the sample cavity and the fluorescence spectra of the ruby ​​microspheres inside the sample cavity. The image of the sample cavity allows the operator to understand the shape of the sample cavity and the morphology of the sample inside, achieving visualization during the pressurization process; the fluorescence spectrum of the ruby ​​microspheres allows the operator to understand the pressure inside the sample cavity. The pressurization detection components can generate equal-inclination interference rings. By controlling the center position of the equal-inclination interference rings to remain constant, uniform pressurization is achieved, thereby avoiding phenomena such as sample cavity displacement, deformation, and leakage. By controlling the number of equal-inclination interference rings and monitoring the positional change of the center wavelength of the characteristic fluorescence peak of the ruby ​​microspheres, the pressurization step size during the pressurization process is controlled, thereby achieving equal-step pressurization.

[0041] Furthermore, the pressure detection assembly includes a microscope 5 for focusing and imaging the sample cavity within the diamond anvil cell 2, and a Raman spectrometer 6 for acquiring the fluorescence spectrum of the ruby ​​microspheres within the sample cavity. The microscope 5 is located directly above the diamond anvil cell 2 and is connected to the Raman spectrometer 6. Both the microscope 5 and the Raman spectrometer 6 are connected to a computer 7. The microscope 5 displays the image of the sample cavity on the screen of the computer 7, allowing the operator to monitor the status of the sample cavity in real time. The Raman spectrometer 6 displays the acquired fluorescence spectrum of the ruby ​​microspheres on the screen of the computer 7, thus obtaining the pressure within the sample cavity.

[0042] Example 2 differs from Example 1 in that, as Figure 4 As shown, the diamond anvil cell 2 includes two parallel upper support blocks 23 and lower support blocks 29. An annular iron plate is provided on the upper side of the upper support block 23, and an upper support block 24 is provided on the lower side of the upper support block 23. A lower support block 28 is provided on the upper side of the lower support block 29. An upper diamond anvil cell 25 and a lower diamond anvil cell 27 are arranged opposite to each other between the upper support block 24 and the lower support block 28. A metal sealing gasket 26 is provided between the upper diamond anvil cell 25 and the lower diamond anvil cell 27. The metal sealing gasket 26 has a small hole. The space formed by the small hole and the upper diamond anvil cell 25 and the lower diamond anvil cell 27 is the sample chamber of the diamond anvil cell 2. The upper support blocks 23 and the lower support blocks 29 are connected by multiple pressure bolts 21. The sample chamber contains a pressure transmitting medium, a pressure standardizing substance, and a sample. The pressure transmitting medium is silicone oil, and the pressure standardizing substance is ruby ​​microspheres. The pressure transmitting medium provides a hydrostatic environment for the sample chamber, and the pressure standardizing substance calibrates the pressure of the sample chamber. When pressurizing, rotating the pressurizing bolt 21 reduces the distance between the upper support block 23 and the lower support block 29, thereby compressing the volume of the sample chamber to generate high pressure and pressurizing the sample.

[0043] Furthermore, a spring plate 22 is provided on the pressure bolt 21, and the spring plate 22 is located between the upper support block 23 and the head of the pressure bolt 21. The spring plate 22 can ensure that the pressure bolt 21 applies stable pressure to the upper support block 23. In this embodiment, there are four pressure bolts 21, and the four pressure bolts 21 are arranged in a circular array with the sample chamber as the center. The rotation of the four pressure bolts 21 can apply pressure to the upper support block 23.

[0044] Example 3 differs from Example 2 in that, as Figure 5As shown, the pressure detection component is a Michelson interferometer 4, which includes a cross-shaped support and a movable mirror 45. A laser 41, a beam splitter 42, a compensation plate 43, a fixed mirror 44, and a camera 46 are fixedly mounted on the cross-shaped support. The movable mirror 45 is fixed to the diamond anvil 2 via a connecting bracket 3. The movable mirror 45 is arranged parallel to the upper surface of the upper support block 23 of the diamond anvil 2. The camera 46 is connected to a computer 7. The laser 41 is installed at the left end of the cross-shaped support, the fixed mirror 44 at the right end, and the camera 46 at the top. The beam splitter 42 is installed at the center of the cross-shaped support at a 45-degree angle. A compensation plate 43 is placed between the beam splitter 42 and the fixed mirror 44, and the compensation plate 43 is arranged parallel to the beam splitter 42. The movable mirror 45 is horizontally positioned by adjusting the screws on its back, which causes the Michelson interferometer 4 to produce equal-inclination interference rings. The camera 46 captures these equal-inclination interference rings and displays them on the screen of the computer 7. Specifically, during the pressurization process, when the center position of the equal-inclination interference ring remains unchanged, it indicates that the movable reflector 45 remains horizontally arranged, which in turn indicates that the upper support block 23 translates relative to the lower support block 29, thus indicating that the diamond anvil 2 is undergoing a uniform pressurization process. Conversely, when the center position of the equal-inclination interference ring changes, it indicates that the movable reflector 45 deviates from its horizontal arrangement and tilts, which in turn indicates that the upper support block 23 performs a non-translational movement relative to the lower support block 29, thus indicating that the diamond anvil 2 is undergoing a non-uniform pressurization process.

[0045] Furthermore, the connecting frame 3 includes a ring magnet 31 and a connecting rod 32. The ring magnet 31 is attached to the ring-shaped iron sheet on the upper side of the upper support block 23. One end of the connecting rod 32 is connected to the ring magnet 31, and the other end of the connecting rod 32 is connected to the movable reflector 45. The ring magnet 31 is attached to the upper surface of the support block 23, and the ring magnet 31 avoids obstructing the line of sight of the microscope 5, allowing the microscope 5 to directly observe the sample chamber.

[0046] Example 4 differs from Example 2 or Example 3 in that, as Figure 2 , Figure 3As shown, the fixing device 1 includes a support frame 11. The upper part of the support frame 11 is provided with a working cavity 15 for placing the diamond anvil cell 2. The side wall of the working cavity 15 is provided with fastening screws 16. The fastening screws 16 extend into the working cavity 15 and lock the lower support block 29 of the diamond anvil cell 2. In this embodiment, there are four fastening screws 16, and the fastening screws 16 are arranged in a circumferential array on the side wall of the working cavity 15. By adjusting the length of the fastening screws 16 extending into the working cavity 15, the diamond anvil cell 2 can be locked and fixed. At the same time, the fastening screws 16 at different positions extend to different lengths, which can adjust the horizontal position of the diamond anvil cell 2 in the working cavity 15, so that the sample cavity of the diamond anvil cell 2 is located within the field of view of the microscope 5, which is convenient for observation by the microscope 5.

[0047] Furthermore, the bottom of the working chamber 15 is provided with an illumination hole 17, and the lower part of the support frame 11 is provided with an illumination device 14 facing the illumination hole 17. The illumination device 14 allows light to pass through the illumination hole 17 and illuminate the sample chamber of the diamond anvil cell 2, which facilitates the observation of the sample chamber by the microscope 5.

[0048] Furthermore, the lower end of the support frame 11 is provided with an ear seat 12, and a fixing screw 13 is provided on the ear seat 12. The support frame 11 is fixed to the optical platform by the fixing screw 13 and the ear seat 12, so that the fixing device 1 remains stable and the diamond anvil 2 remains stable during use.

[0049] Example 5, based on Example 4, provides a method for using a diamond anvil cell visual and controllable pressurization system, comprising the following steps:

[0050] Step S1: Place the diamond anvil cell 2, pre-loaded with ruby ​​microspheres, pressure-transmitting medium, and sample, into the working chamber 15 of the fixing device 1. Silicone oil serves as the pressure-transmitting medium, providing a hydrostatic environment for the sample chamber. The ruby ​​microspheres act as a pressure-calibrating material, calibrating the pressure in the sample chamber. At this point, the diamond anvil cell 2 acts as a leveling device, meaning the upper diamond anvil cell 25 and the lower diamond anvil cell 27 are parallel and aligned. Alternatively, when the sample is liquid, the sample itself can serve as the pressure-transmitting medium, eliminating the need for silicone oil.

[0051] Step S2: Use the fastening screws 16 on the side of the working chamber 15 to fix the diamond anvil 2 and roughly adjust the position of the diamond anvil 2 in the working chamber 15 so that the sample chamber is located within the field of view of the microscope 5.

[0052] Step S3: Use microscope 5 to observe and focus on the sample cavity of diamond anvil cell 2 and display the image on the screen of computer 7; and rotate the fastening screw 16 again to extend it into the working cavity 15 by different lengths, finely adjust the horizontal position of diamond anvil cell 2 in the working cavity 15, so that microscope 5 is aligned with ruby ​​microspheres in the sample cavity.

[0053] Step S4: Utilize the continuous spectral acquisition function of the Raman spectrometer 6 to acquire the fluorescence spectrum of the ruby ​​microspheres in real time, and display the fluorescence spectrum on the screen of the computer 7. The fluorescence spectrum of the ruby ​​is as follows: Figure 6 As shown, the operator determines the initial pressure in the sample chamber based on the position of the center wavelength of its characteristic fluorescence peak.

[0054] Step S5: The annular magnet 31 is attracted to the annular iron sheet, connecting the connecting frame 3 to the upper support block 23 of the diamond anvil cell 2. The movable mirror 45 in the Michelson interferometer 4 is fixed to the connecting frame 3. By adjusting the screws on the back of the movable mirror 45, it is brought to a horizontal position, thereby causing the Michelson interferometer 4 to produce regularly shaped, equally inclined interference rings, such as... Figure 7 As shown, it is displayed on the computer screen.

[0055] Step S6: The pressure bolts 21 on the rotating diamond anvil 2 are used to apply pressure. During the pressure application process, the rotation angles of each pressure bolt 21 are coordinated and controlled to keep the center of the equal-inclination interference ring generated by the Michelson interferometer 4 in a constant position, thus achieving uniform pressure on the sample cavity. At the same time, the fluorescence spectrum of the ruby ​​microspheres is acquired using the continuous spectral acquisition function of the Raman spectrometer 6 to obtain the pressure in the sample cavity in real time until the target pressure is reached.

[0056] Step S7: During the pressurization process, the angle increment of the pressurizing bolt 21 is controlled, thereby controlling the number of passes through the equal-inclination interference rings and the positional change of the center wavelength of the characteristic fluorescence peak of the ruby ​​microspheres. This achieves precise control over the increase in sample chamber pressure, ultimately completing a high-pressure experiment with equal pressurization steps. Specifically, when the position of the center wavelength of the characteristic fluorescence peak of the ruby ​​microspheres moves by an equal distance, the increase in sample chamber pressure is equal.

[0057] The above description 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 within the protection scope of the present invention.

Claims

1. A visually controllable pressurization system based on a diamond anvil cell, comprising a diamond anvil cell (2), characterized in that, The diamond anvil (2) is mounted on the fixing device (1), and the fixing device (1) keeps the diamond anvil (2) in the test optical path during the pressurization process; Above the diamond anvil cell (2) is a pressure detection component for obtaining the pressure inside the sample chamber of the diamond anvil cell (2) and a pressure detection component for obtaining the pressurization state of the diamond anvil cell (2); during the pressurization process of the diamond anvil cell, the pressure detection component is used to observe the state of the sample chamber in real time and detect the pressure in real time until the target pressure is reached. At the same time, the pressure detection component is used to monitor the pressurization process in real time, so that the diamond anvil cell is pressurized uniformly and in equal steps. The pressure detection assembly includes a microscope (5) for focusing and imaging the sample cavity of the diamond anvil cell (2) and a Raman spectrometer (6) for collecting the fluorescence spectrum of the ruby ​​microspheres in the sample cavity. The microscope (5) is located directly above the sample cavity of the diamond anvil cell (2). The microscope (5) is connected to the Raman spectrometer (6). The microscope (5) and the Raman spectrometer (6) are respectively connected to a computer (7). The computer (7) receives and displays the imaging data of the microscope (5) in real time and receives and displays the fluorescence spectrum collected by the Raman spectrometer (6) in real time to determine the pressure in the sample cavity. The pressure detection component is a Michelson interferometer (4). The Michelson interferometer (4) includes a cross bracket and a movable reflector (45). A laser (41), a beam splitter (42), a compensation plate (43), a fixed reflector (44), and a camera (46) are fixed on the cross bracket. The movable reflector (45) is fixed on the diamond anvil (2) through a connecting frame (3). The movable reflector (45) is arranged parallel to the upper surface of the upper support block (23) of the diamond anvil (2). The camera (46) is connected to a computer (7). The computer (7) receives and displays the equal-inclination interference rings generated by the Michelson interferometer (4) in real time. The fixing device (1) includes a support frame (11), the upper part of which is provided with a working cavity (15) for placing a diamond anvil (2), and a fastening screw (16) is provided on the side wall of the working cavity (15). The fastening screw (16) extends into the working cavity (15) to lock the lower support block (29) of the diamond anvil (2).

2. The diamond anvil cell-based visual and controllable pressurization system according to claim 1, characterized in that, The diamond anvil cell (2) includes two parallel upper support blocks (23) and lower support blocks (29). The upper support block (23) has an annular iron plate on its upper side and an upper support block (24) on its lower side. The lower support block (29) has a lower support block (28) on its upper side. The upper support block (24) and the lower support block (28) are provided with an upper diamond anvil cell (25) and a lower diamond anvil cell (27) arranged opposite to each other. A metal sealing gasket (26) is provided between the upper diamond anvil cell (25) and the lower diamond anvil cell (27). The metal sealing gasket (26) has a small hole. The space formed by the small hole and the upper diamond anvil cell (25) and the lower diamond anvil cell (27) is the sample cavity of the diamond anvil cell (2). The upper support block (23) and the lower support block (29) are connected by multiple pressure bolts (21).

3. The diamond anvil cell-based visual and controllable pressurization system according to claim 2, characterized in that, A spring plate (22) is provided on the pressure bolt (21), and the spring plate (22) is located between the upper support block (23) and the head of the pressure bolt (21).

4. The diamond anvil cell-based visual and controllable pressurization system according to claim 1, characterized in that, The connecting frame (3) includes a ring magnet (31) and a connecting rod (32). The ring magnet (31) is attracted to the ring iron plate on the upper side of the upper support block (23). One end of the connecting rod (32) is connected to the ring magnet (31), and the other end of the connecting rod (32) is connected to the movable reflector (45).

5. The diamond anvil cell-based visual and controllable pressurization system according to claim 1, characterized in that, The bottom of the working chamber (15) is provided with a lighting hole (17), and the lower part of the support frame (11) is provided with a lighting device (14) facing the lighting hole (17).

6. The diamond anvil cell-based visual and controllable pressurization system according to claim 5, characterized in that, The lower end of the support frame (11) is provided with an ear seat (12), and a fixing screw (13) is provided on the ear seat (12).

7. A method of using the diamond anvil cell visual and controllable pressurization system as described in any one of claims 1 to 6, characterized in that, Includes the following steps: Step S1: Place the diamond anvil cell (2) pre-loaded with ruby ​​microspheres, pressure-transmitting medium and sample into the working chamber (15) of the fixing device (1); Step S2: Use the fastening screws (16) on the side of the working chamber (15) to fix the diamond anvil (2) and adjust the position of the diamond anvil (2) in the working chamber (15) so that the sample chamber in the diamond anvil (2) is located in the field of view of the microscope (5) and aligned with the ruby ​​microspheres in the sample chamber. Step S3: Use a microscope (5) to observe and focus the sample cavity of the diamond anvil cell (2) and display the image on the screen of the computer (7); Step S4: Use the continuous spectral acquisition function of the Raman spectrometer (6) to acquire the fluorescence spectrum of the ruby ​​microspheres in real time, display the fluorescence spectrum on the screen of the computer (7), and determine the pressure of the initial state in the sample cavity according to the position of the center wavelength of its characteristic fluorescence peak. Step S5: Attach the ring magnet (31) to the ring iron sheet, connect the connecting frame (3) to the upper support block (23) of the diamond anvil (2), fix the movable mirror (45) in the Michelson interferometer (4) on the connecting frame (3), and make the Michelson interferometer (4) generate a regularly shaped equal-inclination interference ring by adjusting the angle of the movable mirror (45), and display it on the computer (7) screen through the camera (46); Step S6: Apply pressure to the sample by rotating the pressure bolts (21) on the diamond anvil (2). During the pressure application process, coordinate and control the rotation angle of each pressure bolt (21) so that the center of the equal-inclination interference ring generated by the Michelson interferometer (4) remains unchanged. At the same time, use the continuous spectral acquisition function of the Raman spectrometer (6) to acquire the fluorescence spectrum of the ruby ​​microspheres and obtain the pressure in the sample cavity in real time until the target pressure is reached. Step S7: During the pressurization process, control the angle increment of the pressurizing bolt (21), thereby controlling the number of equal inclination interference rings and the position change of the center wavelength of the characteristic fluorescence peak of the ruby ​​microsphere, so as to control the pressure increment of the sample cavity in the diamond anvil (2), and finally complete the high pressure experiment with equal pressurization step size.

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