Wide-angle diamond high-pressure pressure cavity device

Abstract

The utility model discloses a wide-angle diamond high-pressure cavity device. The pressure cavity device has the advantages that the guide columns and the pressurizing bolts are arranged on the same horizontal line, a traditional cylinder structure is simplified into a simple linear structure, the operation difficulty of the pressure cavity device is reduced, the overall stability of the pressure cavity is not lost, meanwhile, the mass of the pressure cavity device is greatly reduced, and the production cost is reduced. In-situ measurement and use on optical devices such as a light source are facilitated; besides, the pressure cavity upper plate and the pressure cavity lower plate are provided with axially-penetrating conical holes, the pressure cavity upper plate and the pressure cavity lower plate are of linear strip structures, and larger symmetrical radial field angles are formed on the side walls of the pressure cavity upper plate and the pressure cavity lower plate, so that on one hand, the axial working distance and the radial working distance can be remarkably shortened, and on the other hand, the axial working distance and the radial working distance can be greatly reduced through the large axial field angles and the large radial field angles. And the short focusing characteristic of the X-ray light spot in the high-pressure nano imaging experiment process can be met, so that an in-situ high-pressure experiment can be conveniently carried out on a synchrotron radiation light source or a high-intensity X diffraction spectrometer.

Description

Technical Field

[0001] The utility model relates to the technical field of static high-pressure experimental devices, and particularly relates to a wide-angle diamond anvil cell device. Background Technique

[0002] Static high-pressure experiments mainly study the changes in the material structure and related properties of materials in a high-pressure induced environment under hydrostatic pressure conditions. Static high-pressure technology usually uses a diamond anvil cell as the main experimental device, and a mechanical loading method is used to push the anvils inside the diamond anvil cell. Pressure is slowly applied to the center of the anvils, creating a hydrostatic-like high-pressure environment inside the sample chamber.

[0003] So far, the diamond anvil cell is the simplest device that can achieve a GPa-level pressure environment for micron-sized samples and is widely used in the fields of geology, materials science, physics, chemistry, and more recently, the field of electronic devices. Initially, the diamond anvil cell was designed for application in the field of geology. Researchers designed a diamond anvil cell with a piston-cylinder structure, placed geological samples inside the pressure cell, and compressed the samples by tightening four pressure bolts to simulate the state of materials deep in the earth. At the same time, combined with synchrotron radiation light source technology, the structural and corresponding chemical characteristics of the materials in this state were characterized to explore the unique properties of new and conventional materials under high-pressure conditions. This piston-cylinder structure diamond anvil cell device was also redeveloped and combined with a laser heating device to simulate extreme high-temperature and high-pressure environments for exploration in the fields of deep earth and deep space.

[0004] The diamond anvil cell device only provides a high-pressure environment, and it also needs to be combined with characterization methods and equipment to achieve the development of static high-pressure technology. Therefore, in combination with different characterization methods and testing devices, the diamond anvil cell device needs to be continuously innovated and improved. In recent years, with the development of X-ray imaging technology, the CT imaging technology for nano-scale has gradually matured, and there is a corresponding technical requirement for the diamond anvil cell device used for high-pressure imaging. However, the existing diamond anvil cell devices have problems such as long axial and radial working distances, narrow radial imaging collection angles, and limited axial collection angles, and cannot meet the basic hardware requirements for high-resolution CT imaging. Content of the Utility Model

[0005] (1) Technical Problems to be Solved

[0006] The technical problem to be solved by the utility model is to provide a wide-angle diamond anvil cell device that is miniaturized, has large radial and axial opening angles, and short working distances, in view of the current situation of the prior art.

[0007] (2) Technical Solutions

[0008] The present utility model is realized through the following technical solutions: The present utility model provides a wide-angle diamond anvil cell device, which includes an upper anvil plate. A lower anvil plate is arranged on the lower side of the upper anvil plate. Two pressure bolts are symmetrically installed between the upper anvil plate and the lower anvil plate. Two guide posts are also symmetrically installed between the upper anvil plate and the lower anvil plate. A disc spring is installed under the end of each pressure bolt. Both the upper anvil plate and the lower anvil plate are in the shape of long strip-shaped plates. Conical holes are formed on the upper side of the upper anvil plate and the lower side of the lower anvil plate. A diamond anvil support block is installed in each conical hole. A diamond anvil is installed on the diamond anvil support block. A metal gasket is also arranged between the diamond anvils.

[0009] By adopting the above technical solutions, the guide posts and the pressure bolts are arranged on the same horizontal line, simplifying the traditional cylindrical structure into a simple one-word structure. This not only reduces the operation difficulty of the anvil cell device but also does not compromise the overall stability of the anvil cell. At the same time, it greatly reduces the mass of the anvil cell device, facilitating in-situ measurement and use on optical devices such as light sources. Additionally, by opening axially penetrating conical holes on the upper anvil plate and the lower anvil plate and making both the upper anvil plate and the lower anvil plate adopt a one-word long strip structure, a larger symmetric radial opening angle is formed on the side walls of the upper anvil plate and the lower anvil plate. On the one hand, it can significantly shorten the axial and radial working distances. On the other hand, the large opening angles in the axial and radial directions can meet the short-focus characteristics of the X-ray spot during the high-pressure nano-imaging experiment, thereby facilitating in-situ high-pressure experiments on synchrotron radiation light sources or high-intensity X-ray diffractometers.

[0010] Furthermore, both the upper anvil plate and the lower anvil plate are symmetrically distributed with through-type guide post holes and pressure bolt holes centered on the conical holes.

[0011] By adopting the above technical solutions, such a design can facilitate the reliable installation and fixation of the guide posts and the pressure bolts, and on the one hand, ensure the reliable assembly of the upper anvil plate and the lower anvil plate.

[0012] Furthermore, the cone angle of the conical hole on the upper anvil plate is 70°, and the cone angle of the conical hole on the lower anvil plate is 85°.

[0013] By adopting the above technical solutions, it can ensure convenient observation of the materials inside the device with the aid of external measuring instruments during the measurement process.

[0014] Furthermore, the guide posts are installed on the lower anvil plate with an interference fit and penetrate through the upper anvil plate.

[0015] By adopting the above technical solution, the guide post can ensure the reliable installation and fixation of the upper plate of the pressure chamber and the lower plate of the pressure chamber.

[0016] Furthermore, after the upper plate of the pressure chamber and the lower plate of the pressure chamber are positioned and assembled through the guide post, the assembly distance is 18 mm.

[0017] By adopting the above technical solution, the thickness of the device after assembly is smaller, and the operation is more convenient.

[0018] Furthermore, after the upper plate of the pressure chamber and the lower plate of the pressure chamber are assembled, the maximum radial opening angle is 145°, the radial working distance is 6.5 - 12 mm, and the total weight is less than 90 g.

[0019] By adopting the above technical solution, it is convenient for the device to be observed conveniently during the measurement process, and it is also convenient for the device to be used flexibly and moved.

[0020] Furthermore, the upper plate of the pressure chamber and the lower plate of the pressure chamber are made of any one of high-strength titanium alloy, non-magnetic alloy and high-strength structural steel.

[0021] By adopting the above technical solution, the structural strength of the upper plate of the pressure chamber and the lower plate of the pressure chamber can be effectively ensured.

[0022] Furthermore, the device has axial and radial optical measurement channel windows. The axial direction is the axial optical measurement channel formed by the conical hole on the upper plate of the pressure chamber - the diamond anvil - the conical hole on the lower plate of the pressure chamber; the radial measurement channel window is on the side walls after the upper plate of the pressure chamber and the lower plate of the pressure chamber are assembled, and is formed along the radial direction of the diamond anvil; and the radial measurement channel windows are located on both sides of the upper plate of the pressure chamber and the lower plate of the pressure chamber and are arranged axially symmetrically.

[0023] By adopting the above technical solution, the device can be observed from both the radial and vertical directions when in use after assembly.

[0024] (III) Beneficial effects

[0025] The present utility model has the following beneficial effects compared with the prior art:

[0026] To solve the problems existing in the existing diamond anvil cell device, such as long axial and radial working distances, narrow radial imaging collection angle, and limited axial collection angle, which cannot meet the basic hardware requirements for high-resolution CT imaging, the utility model simplifies the traditional cylindrical structure into a simple linear structure by arranging guide columns and pressure bolts on the same horizontal line. This not only reduces the operation difficulty of the anvil cell device but also does not compromise the overall stability of the anvil cell. At the same time, it greatly reduces the mass of the anvil cell device, facilitating in-situ measurement and use on optical devices such as light sources. Additionally, by opening axially penetrating conical holes on the upper and lower plates of the anvil cell and adopting a linear strip structure for both the upper and lower plates of the anvil cell, a larger symmetric radial opening angle is formed on the side walls of the upper and lower plates of the anvil cell. On the one hand, it can significantly shorten the axial and radial working distances. On the other hand, the large opening angles in the axial and radial directions can meet the short-focus characteristics of the X-ray spot during the high-pressure nanoimaging experiment, thereby facilitating in-situ high-pressure experiments on synchrotron radiation light sources or high-intensity X-ray diffractometers. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 FIG. is a partial sectional view of a wide-angle diamond anvil cell device according to the utility model;

[0028] Figure 2 FIG. is an isometric view of a wide-angle diamond anvil cell device according to the utility model;

[0029] Figure 3 FIG. is a top view of a wide-angle diamond anvil cell device according to the utility model;

[0030] Figure 4 FIG. is an exploded view of a wide-angle diamond anvil cell device according to the utility model;

[0031] Figure 5 FIG. is a right view of a wide-angle diamond anvil cell device according to the utility model.

[0032] The reference numerals are explained as follows:

[0033] 1. Upper plate of the anvil cell; 2. Lower plate of the anvil cell; 3. Diamond anvil support block; 4. Diamond anvil; 5. Pressure bolt; 6. Guide column; 7. Disc spring; 8. Metal gasket. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0034] In order to make the objectives, technical solutions, and advantages of the utility model more clear and understandable, the following further elaborates on the utility model in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the utility model and are not used to limit the utility model.

[0035] As Figures 1 - 5As shown in the figure, a wide-angle diamond anvil cell device in this embodiment includes an upper anvil plate 1. A lower anvil plate 2 is arranged on the lower side of the upper anvil plate 1. Two pressure bolts 5 are symmetrically installed between the upper anvil plate 1 and the lower anvil plate 2. Two guide columns 6 are also symmetrically installed between the upper anvil plate 1 and the lower anvil plate 2. A disc spring 7 is installed under the end of each pressure bolt 5. Both the upper anvil plate 1 and the lower anvil plate 2 are long strip-shaped plate structures. Conical holes are opened on the upper side of the upper anvil plate 1 and the lower side of the lower anvil plate 2. A diamond anvil support block 3 is installed in each conical hole. A diamond anvil 4 is installed on the diamond anvil support block 3. The diamond anvil 4 is a bottom cone structure and is fixedly installed on the diamond anvil support block 3 through an adhesive. The diamond anvil 4 bonded to the diamond anvil support block 3 needs to be fixed and adjusted with screws to the upper anvil plate 1. A metal gasket 8 is also arranged between the diamond anvils 4. The guide columns 6 and the pressure bolts 5 are arranged on the same horizontal line, simplifying the traditional cylindrical structure into a simple one-word structure, which not only reduces the operation difficulty of the anvil cell device but also does not lose the overall stability of the anvil cell. At the same time, it greatly reduces the mass of the anvil cell device, facilitating in-situ measurement and use on optical devices such as light sources. Additionally, by opening axially penetrating conical holes on the upper anvil plate 1 and the lower anvil plate 2 and making both the upper anvil plate 1 and the lower anvil plate 2 adopt a one-word long strip structure, a larger symmetric radial opening angle is formed on the side walls of the upper anvil plate 1 and the lower anvil plate 2. On the one hand, it can significantly shorten the axial and radial working distances. On the other hand, the large opening angles in the axial and radial directions can meet the short-focus characteristics of the X-ray spot during the high-pressure nano-imaging experiment, thereby facilitating in-situ high-pressure experiments on synchrotron radiation light sources or high-intensity X-ray diffractometers.

[0036] As Figures 1 - 5 shown in the figure, in this embodiment, both the upper anvil plate 1 and the lower anvil plate 2 are symmetrically distributed with through-type guide column holes and pressure bolt holes centered on the conical holes. Such a design can facilitate the reliable installation and fixation of the guide columns 6 and the pressure bolts 5. On the one hand, it ensures the reliable assembly of the upper anvil plate 1 and the lower anvil plate 2. The cone angle of the conical hole on the upper anvil plate 1 is 70°, and the cone angle of the conical hole on the lower anvil plate 2 is 85°, which can ensure convenient observation of the materials inside the device with the help of external measuring instruments during the measurement process.

[0037] As Figures 1 - 5As shown, in this embodiment, the guide post 6 is installed on the lower plate 2 of the pressure chamber by interference fit, and the guide post 6 penetrates through the upper plate 1 of the pressure chamber. The guide post 6 can ensure the reliable installation and fixation of the upper plate 1 and the lower plate 2 of the pressure chamber. After the upper plate 1 and the lower plate 2 of the pressure chamber are positioned and assembled through the guide post 6, the assembly distance is 18 mm, making the thickness of the device smaller after assembly and the operation more convenient. The maximum radial opening angle after the upper plate 1 and the lower plate 2 of the pressure chamber are assembled is 145°, the radial working distance is 6.5 - 12 mm, and the total weight is less than 90 g, which is convenient for convenient observation during the measurement process of the device and also convenient for flexible movement and use of the device. The upper plate 1 and the lower plate 2 of the pressure chamber are made of any one of high-strength titanium alloy, non-magnetic alloy, and high-strength structural steel, which can effectively ensure the structural strength of the upper plate 1 and the lower plate 2 of the pressure chamber.

[0038] As Figures 1 - 5 shown, in this embodiment, the device has axial and radial optical measurement channel windows. Axially, it is the axial optical measurement channel formed by the conical hole on the upper plate 1 of the pressure chamber - the diamond anvil 4 - the conical hole on the lower plate 2 of the pressure chamber; the radial measurement channel window is on the side walls after the upper plate 1 and the lower plate 2 of the pressure chamber are assembled, and the radial measurement channel window is formed along the radial direction of the diamond anvil 4; and the radial measurement channel windows are located on both sides of the upper plate 1 and the lower plate 2 of the pressure chamber and are axially symmetrically arranged, so that the device can be observed from both the radial and vertical directions when in use after assembly.

[0039] As Figures 1 - 5 shown, in this embodiment, after the device is assembled, an incident channel with an incident angle of 145° is formed in the radial direction, and an exit channel is formed on the back of the pressure chamber; when performing a radial diffraction or imaging experiment, the X incident light enters through the incident channel, irradiates the sample in the beryllium sample chamber, and then the exit light enters the radially arranged X-ray detectors through the exit channel to collect the diffraction data and imaging data of the sample.

[0040] As Figures 1 - 5As shown, in this embodiment, by rotating the pressure bolt 5, a stable static high-pressure environment is formed in the diamond anvil 4 and the center of the sample chamber, and the sample in the sample chamber is pressured using a ruby ​​pressure system, and it is found that a high pressure of 110GPa is formed on the diamond anvil 4 with a 150um table surface; the pressure-standardized diamond high-pressure pressure chamber is horizontally placed on the imaging line station of a micro-nano CT device or a high-energy X-ray synchrotron radiation device, so that the incident channel is coaxial with the X-ray incident light, and the imaging or diffraction data collection device is located at the same level in the direction of the exit channel. In the plane, the angles of the exit channel and the incident channel are both 145°, which enables the X-ray detector to effectively detect data in the range of 0-145° on the exit channel side; this is a significant increase over the 60° and 100° of conventional radial diffraction presses; it can be seen that the device can not only be used for conventional axial high-pressure diffraction experiments, but can also achieve ultra-high pressure and wider-angle diffraction angles in radial diffraction and imaging experiments, and is very suitable for use in desktop high-energy X-ray diffractometers, nanoprobe platforms and synchrotron radiation imaging beamlines.

[0041] The specific implementation process of this embodiment is as follows: when conducting an XRD diffraction experiment, first place a 0.25mm thick metal gasket 8 between two diamond anvils 4 with an anvil surface size of 300um. The metal gasket 8 can be a rhenium sheet, a beryllium sheet or a T301 stainless steel sheet. Here, a rhenium sheet is selected. The center of the metal gasket 8 is punched with a 150um hole. The test sample, ruby ​​microspheres and silicone oil pressure transmission medium are loaded into the center hole of the metal gasket 8. The upper and lower diamond anvils 4 are combined with the holes on the metal gasket 8 to form a hydrostatic high-pressure sample chamber. By tightening the left and right pressure bolts 5, the upper and lower diamond anvils 4 compress the sample in the metal sample chamber, so that the test sample in the sample chamber generates high pressure. In the process of calibrating the sample pressure, it is necessary to use laser to excite the ruby ​​microspheres in the sample chamber. Generate fluorescence, collect the excited fluorescence spectrum through the spectrum, and calculate the pressure in the sample chamber according to the fluorescence peak shift; after sample preparation and pressure loading calibration, the wide-angle diamond high-pressure pressure chamber device can be placed on a high-energy X-ray diffractometer or a synchrotron radiation line station, and keep how the X-ray is incident from the conical hole on the upper plate 1 of the pressure chamber, through the diamond anvil 4 and the sample chamber, and irradiate the test sample in the sample chamber, and then collect the diffraction peaks generated by the sample in the direction of the conical hole on the lower plate 2 of the pressure chamber; load the pressure through the pressure bolt 5, and after the ruby ​​is calibrated, a pressure of 56Gpa can be generated on the diamond anvil 4 with a table surface of 300um, and with the diamond anvil support block 3 at the conical hole on the lower plate 2 of the pressure chamber, the diffraction data in the range of 0-85° can be effectively collected on the back.

[0042] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present utility model. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present utility model. Therefore, the present utility model will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A wide-angle diamond anvil cell device, characterized in that: It includes an upper pressure chamber plate (1), a lower pressure chamber plate (2) is arranged on the lower side of the upper pressure chamber plate (1), two pressurizing bolts (5) are symmetrically installed between the upper pressure chamber plate (1) and the lower pressure chamber plate (2), two guiding columns (6) are also symmetrically installed between the upper pressure chamber plate (1) and the lower pressure chamber plate (2), a disc spring (7) is installed under the end of each pressurizing bolt (5), both the upper pressure chamber plate (1) and the lower pressure chamber plate (2) are long strip-shaped plate structures, tapered holes are formed on the upper side of the upper pressure chamber plate (1) and the lower side of the lower pressure chamber plate (2), a diamond anvil support block (3) is installed in each tapered hole, a diamond anvil (4) is installed on the diamond anvil support block (3), and a metal gasket (8) is arranged between the diamond anvils (4).

2. The wide-angle diamond anvil cell device according to claim 1, wherein: Both the upper pressure chamber plate (1) and the lower pressure chamber plate (2) are symmetrically distributed with through-type guiding column holes and pressurizing bolt holes on the left and right with the tapered hole as the central symmetry axis.

3. The wide-angle diamond anvil cell device according to claim 2, characterized in that: The taper angle of the tapered hole on the upper pressure chamber plate (1) is 70°, and the taper angle of the tapered hole on the lower pressure chamber plate (2) is 85°.

4. The wide-angle diamond anvil cell device according to claim 1, characterized in that: The guiding column (6) is installed on the lower pressure chamber plate (2) by interference fit, and the guiding column (6) penetrates through the upper pressure chamber plate (1).

5. A wide-angle diamond anvil cell device according to claim 1, characterized in that: After the upper pressure chamber plate (1) and the lower pressure chamber plate (2) are positioned and assembled through the guiding column (6), the assembly distance is 18 mm.

6. The wide-angle diamond anvil cell device according to claim 5, characterized in that: After the upper pressure chamber plate (1) and the lower pressure chamber plate (2) are assembled, the maximum radial opening angle is 145°, the radial working distance is 6.5 - 12 mm, and the total weight is less than 90 g.

7. A wide-angle diamond anvil cell device according to claim 1, characterized in that: The upper pressure chamber plate (1) and the lower pressure chamber plate (2) are made of any one of high-strength titanium alloy, non-magnetic alloy and high-strength structural steel.

8. The wide-angle diamond anvil cell device according to claim 1, wherein: This device has axial and radial optical measurement channel windows. Axially, it is the axial optical measurement channel formed by the tapered hole on the upper pressure chamber plate (1) - the diamond anvil (4) - the tapered hole on the lower pressure chamber plate (2); the radial measurement channel window is on the side walls after the upper pressure chamber plate (1) and the lower pressure chamber plate (2) are assembled, and is formed along the radial direction of the diamond anvil (4); and the radial measurement channel window is located on both sides of the upper pressure chamber plate (1) and the lower pressure chamber plate (2) and is arranged axially symmetrically.

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