Automated integrated high pressure press and method of controlling the same

Abstract

The application provides an automatic high-pressure press and a control method thereof, and belongs to the field of high pressure and materials. A supporting mechanism is used for fixing a counter-pressure anvil or a press component. A driving mechanism is connected with the counter-pressure anvil or the press component, and is used for pressurizing, pressure maintaining or pressure releasing. A feeding mechanism is arranged on one side of the supporting mechanism, and is used for feeding or moving out a gasket or a material to be pressed into a press anvil surface area. A monitoring module is used for acquiring pressure parameters of the driving mechanism and corresponding working parameters of the counter-pressure anvil or the press component, and transmitting the pressure parameters and the working parameters to a control module. According to the pressure parameters and the working parameters, the control module controls the feeding mechanism, the driving mechanism and the supporting mechanism to cooperate with each other to process the gasket or the material under high pressure and other conditions. The application adopts a small amount of multiple strategies, can realize low-cost batch preparation of materials under high pressure, is more suitable for the case that the size or volume requirement of a single sample is not high, and reduces the preparation cost of high-pressure equipment and the production cost of high-pressure materials.

Description

Technical Field

[0001] This invention relates to the fields of high pressure and materials, and in particular to an automated integrated high pressure press and its control method. Background Technology

[0002] Pressure, like temperature, is a fundamental state parameter of matter. High pressure (pressure exceeding one standard atmosphere, or simply high pressure) can significantly alter the structure and properties of matter, thereby obtaining new materials that are difficult to obtain under normal conditions, which is conducive to the discovery of new phenomena and laws.

[0003] Developing presses capable of generating higher pressures and more advanced in-situ high-pressure characterization methods are key to advancing high-pressure science. Furthermore, given the large demand for materials in some characterization and testing studies (e.g., electron paramagnetic resonance, neutron diffraction, performance testing), and the many excellent properties of high-pressure materials (including materials whose structure or properties are preserved or partially preserved at atmospheric pressure, or composite materials prepared under atmospheric and high pressure) that remain to be developed and applied, developing devices capable of inexpensively, massively, and controllably preparing high-pressure materials can effectively promote cutting-edge research in high-pressure science and the widespread application of high-pressure technology.

[0004] Existing high-pressure material preparation methods typically require high pressure and sample volume or sample chamber volume; however, it becomes difficult to increase pressure once the volume is large enough. To address this issue, current technologies generally use larger superhard materials as anvils or top hammers to increase the sample chamber volume and pressure. While this has advantages in synthesizing bulk single-crystal materials, it increases the fabrication and production costs of the high-pressure equipment. In particular, for cases where the size or volume requirements of individual samples (i.e., the products obtained by the high-pressure press) are not critical, such as micron or nanomaterials smaller than 1 mm, using a large-cavity press is not economical. Summary of the Invention

[0005] This invention provides an automated integrated high-pressure press and its control method to solve the problem that the existing technology uses a large superhard material as an anvil or top hammer to increase the sample chamber volume and pressure. Although this has advantages in synthesizing bulk single crystal materials, it is easy to damage the anvil and requires a large pressure driving force, which increases the manufacturing cost and production cost of high-pressure equipment.

[0006] This invention provides an automated integrated high-pressure press, comprising a support mechanism, a drive mechanism, a feeding mechanism, a monitoring module, and a control module, wherein the control module is connected to the drive mechanism, the feeding mechanism, and the monitoring module respectively. The support mechanism is equipped with components for fixing the top pressing anvil or press; The drive mechanism is connected to the counterweight anvil or the press component and is used to pressurize, maintain pressure or depressurize the counterweight anvil or the press component. The feeding mechanism is located on one side of the support mechanism and is used to feed the pad or material to be pressed into or remove the anvil surface area corresponding to the top pressing anvil or the press component. The monitoring module is used to acquire at least the pressure parameters of the drive mechanism and the working parameters corresponding to the anvil or the press component, and transmit the pressure parameters and the working parameters to the control module. The control module is used to control the feeding mechanism and the driving mechanism according to the pressure parameters and the working parameters, so that the feeding mechanism, the driving mechanism and the support mechanism cooperate to process the gasket or the material at least once.

[0007] According to the present invention, an automated integrated high pressure press is provided, wherein the top anvil or the press component includes at least a pair of anvil assemblies, the anvil assemblies are arranged in a linear or array shape, and the anvil assemblies pressurize, maintain pressure or depressurize the gasket or the material according to preset driving parameters under the pressure of the driving mechanism.

[0008] According to the present invention, an automated integrated high-pressure press is provided, wherein the material of the anvil is one or more of diamond, silicon carbide, boron nitride, tungsten carbide, carbon composite material, alumina, topaz, zircon, quartz, superhard metal steel, cemented carbide, chromium, and tungsten steel.

[0009] According to the present invention, an automated integrated high pressure press is provided, wherein the feeding mechanism includes a feeding base, a sliding member, a clamping member, and a feeding drive member; The sliding member is disposed on the feeding base and slides on the feeding base in at least two dimensions under the drive of the feeding drive member; The clamping member is connected at its bottom to the top of the sliding member and is used to clamp the pad or the material.

[0010] An automated integrated high-pressure press according to the present invention further includes a filling component; The filling component is connected to the feeding base, and the outlet of the filling component is located above the gasket or the material, for filling the gasket with the material to be pressed.

[0011] According to an automated integrated high-pressure press provided by the present invention, one end of the feeding base is connected to the driving mechanism, and under the drive of the driving mechanism, the sliding member, the clamping member and the feeding driving member move along the movement direction of the driving mechanism.

[0012] An automated integrated high-pressure press according to the present invention further includes a calibration mechanism, which is electrically connected to the control module. A verification mechanism is provided above the anvil or press component, and is used to detect the position information of the gasket or the material in the anvil surface area, and send the position information to the control module. The control module is also used to control the feeding mechanism to adjust the position of the pad or the material in the anvil surface area according to the position information.

[0013] An automated integrated high-pressure press according to the present invention further includes a temperature regulating mechanism, which is connected to the control module; The temperature regulating mechanism is used to adjust the temperature of the top pressure anvil or press components, support mechanism and drive mechanism.

[0014] According to the present invention, an automated integrated high-pressure press is provided, wherein the pressure range generated by the drive mechanism is 0.1 GPa - 500 GPa.

[0015] The present invention also provides a method for controlling the aforementioned automated integrated high-pressure press, comprising: Obtain monitoring data; Based on the monitoring data, the drive mechanism and the support mechanism are controlled to cooperate in performing steady-state pressurization or dynamic pressurization, and the pressure value of the drive mechanism is monitored during the pressurization process. If the pressure value reaches the preset value, the drive mechanism and the support mechanism are controlled to cooperate in performing pressure holding, steady state or dynamic pressure relief operations; After the pressure relief operation is completed, control the feeding mechanism to move the gasket or the material, and repeat the above steps.

[0016] The automated integrated high-pressure press and its control method provided by this invention include a support mechanism, a drive mechanism, a feeding mechanism, a monitoring module, and a control module. Based on the pressure parameters and operating parameters, the feeding mechanism and the drive mechanism are controlled so that they cooperate with the support mechanism to process the gasket or material at least once. This invention employs a small-batch, multiple-processing strategy, enabling low-cost batch preparation of materials under high pressure. It is more suitable for situations where the size or volume requirements of individual samples are not critical, and it does not increase the preparation and production costs of high-pressure equipment. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in this invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of the structure of the automated integrated high-pressure press provided by the present invention; Figure 2 This invention provides Figure 1 Enlarged cross-sectional diagram of the central support mechanism; Figure 3 This is a schematic diagram of the control flow of the control module provided by the present invention; Figure 4 This is a schematic diagram of the automated integrated high-pressure press provided by the present invention; Figure 5 This is a flowchart illustrating the method for controlling the automated integrated high-pressure press provided by the present invention. Figure 6 This is a schematic diagram of the T301 stainless steel gasket provided by the present invention before high-pressure treatment; Figure 7 This is a schematic diagram of the T301 stainless steel gasket provided by the present invention after high-pressure treatment; Figure 8 This is a schematic diagram of the WO3 sample provided by this invention before and after high-pressure treatment; Figure 9 This is a schematic diagram of the light absorption of the WO3 sample before and after high-pressure treatment provided by the present invention.

[0019] Figure label: 1-Support mechanism, 2-Drive mechanism, 3-Feeding mechanism, 310-Feeding base, 320-Sliding part, 330-Clamping part, 340-Feeding drive part, 4-Monitoring module, 5-Control module, 6-Verification mechanism, 7-Temperature regulation mechanism, 8-Top pressing anvil, 9-Pressure anvil surface area. Detailed Implementation

[0020] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0021] In the description of the embodiments of this application, it should be noted that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of this application. In addition, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0022] In the description of the embodiments of this application, it should be noted that, unless otherwise explicitly specified and limited, the terms "connected" and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this application based on the specific circumstances.

[0023] In the embodiments of this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0024] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the embodiments of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0025] Figure 1 This is a structural schematic diagram of the automated integrated high-pressure press provided by the present invention. Figure 2 This invention provides Figure 1 An enlarged cross-sectional diagram of the central support mechanism is shown below. Figure 1 and Figure 2 As shown, the present invention provides an automated integrated high-pressure press, including a support mechanism 1, a drive mechanism 2, a feeding mechanism 3, a monitoring module 4, and a control module 5. The control module 5 is connected to the drive mechanism 2, the feeding mechanism 3, and the monitoring module 4 respectively. The support mechanism 1 is used to fix the top pressure anvil 8 or the press component, wherein the press component is the remaining parts of a manually pressurized diamond press (including piston-cylinder type and column type) after removing the manual pressurization screw, and is connected to the support mechanism 1; wherein the types of diamond presses include, but are not limited to: Mao-Bell symmetrical press, Paris-Edinburgh type press, hydrothermal press, Cross type press, non-magnetic or low-magnetic press, and high-pressure torsion press.

[0026] The drive mechanism 2 is connected to the counter-pressing anvil 8 or the press component, and is used to pressurize, maintain pressure or depressurize the counter-pressing anvil 8 or the press component; The feeding mechanism 3 is located on one side of the support mechanism 1 and is used to feed the pad or material to be pressed into or remove the anvil surface area 9 corresponding to the top pressing anvil 8 or the press component. The monitoring module 4 is used to acquire at least the pressure parameters of the drive mechanism 2 and the corresponding operating parameters of the anvil 8 or the press component, and transmit the pressure parameters and operating parameters to the control module 5. The operating parameters include at least the external pressure, internal pressure, and temperature of the anvil 8 or the press component. For cases where pressure accuracy requirements are not high, external pressure can be used. However, for cases where high pressure is required in the anvil surface area 9, such as hydrostatic pressure testing and dynamic loading experiments, internal pressure must be used. The internal pressure is calibrated by fluorescence (PL), Raman, and other measurements using a ruby ​​or other pressure gauge near the sample (the sample and the anvil itself can sometimes also serve as pressure gauges). Temperature and other operating parameters are similar.

[0027] The control module 5 is used to control the feeding mechanism 3 and the driving mechanism 2 according to the pressure parameters and the working parameters, so that the feeding mechanism 3, the driving mechanism 2 and the support mechanism 1 cooperate to process the gasket or the material at least once to prepare at least one high-pressure material, or to apply it to dynamic loading research.

[0028] Controlling the feeding mechanism 3 and the driving mechanism 2 according to the pressure parameters and the working parameters includes: generating control commands corresponding to the feeding mechanism 3 and the driving mechanism 2 according to the set pressure parameter lifting rate or flow rate and maximum value, such as: increasing the pressure to a certain level, heating, maintaining the temperature, and then cooling, or heating first and then increasing the pressure.

[0029] Optionally, the automated integrated high-pressure press provided by this invention can also be used for dynamic loading or in-situ structural property measurement experiments. Dynamic loading is an emerging technology in the field of high-pressure science and technology. Because its loading rate is between that of traditional dynamic high pressure and static high pressure, its physical process differs from the isothermal process of static high pressure and also from the adiabatic process of dynamic high pressure. Instead, it is a special physical process that is neither isothermal nor adiabatic. Under appropriate dynamic loading rates, substances will break away from their conventional chemical equilibrium state, achieving the construction and reorganization of material structures to form some metastable phase structures.

[0030] Optionally, the support mechanism 1 can be a multi-faceted support mechanism 1. The present invention will be described in detail using an anvil as an example.

[0031] Optionally, the drive mechanism 2 is used to pressurize, maintain, or depressurize the anvil 8 or press component. The pressure applied to the anvil 8 or press component can generate a high pressure exceeding one atmosphere. Driven by the drive mechanism 2, the anvil 8 or press component applies pressure to the gasket or material, squeezing the gasket or material to obtain high-pressure material. The drive mechanism 2 can be selected from one or more of the following: a servo electric cylinder, a hydraulic cylinder, a pneumatic cylinder (or air film cylinder), a piezoelectric ceramic, or a stepper motor-based electric cylinder, with at least one type.

[0032] Optionally, the feeding mechanism 3 is located on one side of the top pressing anvil 8 or the press component, and feeds the pad or material to be pressed into or out of the pressing anvil surface area 9 through the feeding drive mechanism; the feeding mechanism 3 can be one or more of the following: servo electric cylinder, hydraulic cylinder, pneumatic cylinder, piezoelectric ceramic, stepper motor-based electric cylinder.

[0033] Optionally, the monitoring module 4 includes at least a pressure sensor and a temperature sensor. In other embodiments, the monitoring module 4 may also include a position sensor and a fluorescence or Raman pressure measurement system. The fluorescence or Raman pressure measurement system is used to detect the internal pressure parameters of the anvil 8 or the press component and to determine whether the pressure of the anvil 8 or the press component has reached a preset value. If it has not reached the preset value, the drive mechanism 2 is controlled to increase the pressure.

[0034] Optionally, the control module 5 includes a driver for controlling the drive mechanism 2, an encoder for controlling the feeding mechanism 3, and a processor for data processing. The processor can be a computer, PLC, microcontroller, or analog-digital circuit, used to process the acquired working parameters and issue control signals based on the processing results.

[0035] Figure 3 This is a schematic diagram of the control flow of the control module 5 provided by the present invention, as shown below. Figure 3 As shown, optionally, the feeding mechanism 3 and the driving mechanism 2 are controlled according to the pressure parameters and the temperature parameters, so that the feeding mechanism 3, the driving mechanism 2, and the support mechanism 1 cooperate to process the gasket or the material at least once to prepare at least one high-pressure material, specifically including: S1, System initialization, control the feeding mechanism 3 to put the pad or material into the anvil surface area 9; S2, acquire the various parameters collected by the monitoring module 4, including but not limited to the pressure parameter and the temperature parameter; S3, send a control command to the drive mechanism 2 to control the drive mechanism 2 to pressurize the support mechanism 1 and the gasket or material in the support mechanism 1, and monitor the pressure parameters during the pressurization process; S4. If the pressure parameters reach the set pressure range, determine whether it is necessary to maintain pressure or adjust various parameters such as temperature and field strength according to the preparation conditions of the gasket or material. If it is not necessary to maintain pressure or adjust the temperature, proceed to the next step. S5, send a control command to drive mechanism 2 to control drive mechanism 2 to start depressurization until support mechanism 1 is completely separated from gasket or material; S6, send a control command to the feeding mechanism 3 to control the feeding mechanism 3 to move the pad or material; S7. Determine whether the gasket or material has moved to the preset area or the number of moves has reached the preset value. If yes, the process ends; otherwise, repeat steps S2 to S6.

[0036] It is understood that the present invention includes a support mechanism 1, a drive mechanism 2, a feeding mechanism 3, a monitoring module 4, and a control module 5. Based on the pressure and temperature parameters, the feeding mechanism 3 and the drive mechanism 2 are controlled so that they cooperate with the support mechanism 1 to process the gasket or the material at least once, preparing at least one batch of high-pressure material. The present invention employs a small-batch, multiple-process strategy, enabling low-cost batch preparation of materials under higher pressure. This is more suitable for situations where single-crystal volume requirements are not high, and it does not increase the preparation and production costs of high-pressure equipment.

[0037] Based on the above embodiments, as an optional embodiment, the anvil 8 or the press component includes at least a pair of anvil assemblies. The anvil assemblies are arranged linearly or in an array. Under the pressure of the drive mechanism 2, the anvil assemblies pressurize, maintain pressure, or depressurize the gasket or the material according to preset drive parameters. The linear or array arrangement of the anvil assemblies can greatly improve the preparation efficiency.

[0038] Optionally, the anvil assembly can consist of two anvils arranged opposite each other, and the driving parameters include at least the driving speed and the target pressure. The number of driving mechanisms 2 can be one or two, with the driving mechanism 2 located at one of the anvils, pushing the anvil to move and generate high pressure to pressurize the gasket or material.

[0039] Optionally, the material of the anvil is one or more of the following: diamond, silicon carbide, boron nitride, tungsten carbide, carbon composite material, alumina (or corundum, including sapphire and ruby), topaz, zircon, quartz, superhard metal steel, cemented carbide, chromium, and tungsten steel.

[0040] It is understood that this invention, by setting up multiple anvil components and using superhard materials as anvils, such as a diamond anvil cell (DAC), can achieve the highest static pressure (>100GPa) and withstand high temperatures (~5000K). It can observe the mechanical, thermal, electrical, magnetic, and optical properties of materials in situ under high temperature and high pressure. It also has the advantages of being compact and lightweight, and having relatively low manufacturing and usage costs (in the low-pressure area). This invention uses a small diamond anvil to generate high pressure and performs multiple pressurization processes on gaskets or materials, realizing the mass production and widespread application of high-pressure materials.

[0041] Based on the above embodiments, as an optional embodiment, the gasket is elongated and has multiple recesses on its surface for filling the material. The gasket can also be square, allowing the sample to be directly placed on it, eliminating the arduous process of loading the material into the pressure chamber and improving efficiency. Alternatively, material (including the sample and necessary pressure-transmitting medium or pressure gauge, such as ruby) can be pre-placed in the pits or holes of the gasket before being placed into the anvil or the press component.

[0042] It is understandable that the present invention adjusts the shape of the gasket, which is beneficial to the mass production and widespread application of high-pressure materials.

[0043] Based on the above embodiments, as an optional embodiment, the feeding mechanism 3 includes a feeding base 310, a sliding member 320, a clamping member 330, and a feeding drive member 340; The sliding member 320 is disposed on the feeding base 310 and slides on the feeding base 310 in at least two dimensions under the drive of the feeding drive member 340. The clamping member 330 is connected at its bottom to the top of the sliding member 320 and is used to clamp the pad or the material.

[0044] The sliding member 320 and the clamping member 330 cooperate to allow the pad or material to move in two dimensions on the anvil plane, namely the x and y axes on the anvil plane. After the feeding mechanism 3 moves the pad or material into the anvil area 9, it makes fine adjustments on the x and y axes on the anvil plane so that the hole on the pad can be aligned with the center of the anvil of the top anvil.

[0045] Optionally, the feeding mechanism 3 further includes a filling component (not shown in the figure); the filling component is connected to the feeding base, and the outlet of the filling component is located above the gasket or the material, for filling the gasket with the material to be pressed. The surface of the gasket is provided with positions for pressurizing the anvil. These positions can be provided with holes or pits, and the material can be filled directly into the corresponding positions, or into the holes or pits at the positions.

[0046] Optionally, the feeding drive unit 340 can be one of a servo electric cylinder, hydraulic cylinder, pneumatic cylinder, piezoelectric ceramic, or electric cylinder based on a stepper motor. This invention uses a stepper motor as an example for illustration.

[0047] Optionally, the feeding base 310 can also be connected to the support mechanism 1.

[0048] Optionally, one end of the loading base 310 is connected to the driving mechanism 2. Under the drive of the driving mechanism 2, the sliding member 320, the clamping member 330, and the loading driving member 340 move along the movement direction of the driving mechanism 2. The loading base 310 can move accordingly with the movement direction and speed of the driving mechanism 2.

[0049] It is understandable that during the pressurization process, pressurizing the anvil 8 or the press component on the pad or material will cause displacement of the pad or material. In order to avoid the decrease in accuracy caused by displacement, the present invention connects one end of the feeding base 310 to the drive mechanism 2, so that the part of the pad or material that has not entered the anvil surface area can move with the movement of the anvil 8 or the press component, thereby improving the preparation accuracy of the pad or material.

[0050] Figure 4 This is a schematic diagram of the automated integrated high-pressure press provided by the present invention, as shown below. Figure 4 As shown, based on the above embodiments, as an optional embodiment, a verification mechanism 6 is also included, which is electrically connected to the control module 5; Verification mechanism 6 is located above the anvil or press component, and can see the pad or material through the anvil or press component. It is used to detect the position information of the pad or the material in the anvil surface area and send the position information to the control module 5. The control module 5 is also used to control the feeding mechanism 3 to adjust the position of the pad or the material in the anvil surface area according to the position information.

[0051] Optionally, the verification mechanism 6 may be composed of a microscope or a camera.

[0052] It is understood that by setting up a verification mechanism 6, which works in conjunction with the feeding mechanism 3, the present invention can achieve precise positioning of the gasket or material within the anvil surface area.

[0053] Based on the above embodiments, as an optional embodiment, a temperature regulating mechanism 7 is also included, which is connected to the control module; The temperature regulating mechanism 7 is used to adjust the temperature of the top pressing anvil or press components, support mechanism and drive mechanism.

[0054] Optionally, the temperature control mechanism 7 can be a temperature control system such as resistance heating, laser heating, or low-temperature cooling device.

[0055] It is understandable that the monitoring module 4, control module 5 and temperature regulation mechanism 7 can work together to achieve precise adjustment of the ambient temperature of the support mechanism 1, so as to meet the preparation conditions of various gaskets or materials.

[0056] Based on the above embodiments, as an optional embodiment, the pressure range generated by the driving mechanism 2 is 0.1 GPa - 500 GPa, preferably 5 GPa - 500 GPa. More preferably, the pressure range generated by the driving mechanism 2 can exceed 30 GPa, or even 100 GPa or more.

[0057] Understandably, the application of multiple integrated high-pressure presses in batch conversion or preparation of materials under normal temperature and high pressure, low temperature and high pressure, and high temperature and high pressure can meet the industrial demand for large-scale material preparation and contribute to applications in basic research such as dynamic loading.

[0058] The method for controlling the automated integrated high-pressure press provided by the present invention is described below. The method for controlling the automated integrated high-pressure press described below can be referred to in correspondence with the automated integrated high-pressure press described above.

[0059] Figure 5 This is a flowchart illustrating the method for controlling the automated integrated high-pressure press provided by the present invention, as shown below. Figure 5 As shown, the present invention also provides a method for controlling the aforementioned automated integrated high-pressure press, comprising: S510, acquire monitoring data; S520, based on the monitoring data, control the drive mechanism and the support mechanism to cooperate in performing steady-state pressurization or dynamic pressurization, and monitor the pressure value of the drive mechanism during the pressurization process; S530, if the pressure value reaches the preset value, control the drive mechanism and the support mechanism to cooperate in performing pressure holding, steady state or dynamic pressure relief operation; S540, after the depressurization operation is completed, control the feeding mechanism to move the gasket or the material, and repeat the above steps.

[0060] The following examples illustrate the process of preparing high-pressure materials using the high-pressure press provided by the present invention.

[0061] Figure 6 This is a schematic diagram of the T301 stainless steel gasket provided by this invention before high-pressure treatment. Figure 7 This is a schematic diagram of the T301 stainless steel gasket provided by this invention after high-pressure treatment, as shown below. Figure 6 and Figure 7 As shown.

[0062] Example 1: High-pressure treatment was performed using a T301 stainless steel gasket as a sample. The specific steps are as follows: A press component with a diamond anvil platen diameter of 500 micrometers (the remaining parts of a manually pressurized symmetrical DAC press after removing the manual pressurization screw) and a T301 stainless steel gasket with a thickness of 250 micrometers are fixed into a high-pressure press. The press and the gasket inside the press are pressurized by controlling an electric cylinder. When the pressure on the gasket reaches 15-18 GPa, depressurization begins until the gasket and the diamond anvil are completely separated. A stepper motor is then controlled to move the indentation of the gasket out of the anvil region. The above steps are then repeated to achieve automatic pressurization and depressurization of the gasket. In this embodiment, the pressure loading rate can reach over 100 GPa / s, indicating that the high-pressure press of this invention can be used for dynamic loading experimental research.

[0063] Figure 8 This is a schematic diagram of the WO3 sample provided by this invention before and after high-pressure treatment. Figure 9 This is a schematic diagram of the light absorption of the WO3 sample before and after high-pressure treatment, provided by the present invention. Figure 9 In the diagram, the horizontal axis represents the wavelength of light, and the vertical axis represents the absorption value.

[0064] Example 2: High-pressure preparation of blue WO3 (tungsten oxide) sample, the specific steps are as follows: A concentrated aqueous solution of tungsten oxide (analytical grade WO3) was applied to a T301 stainless steel gasket. After drying, a pale yellow WO3 film was formed on the stainless steel substrate. The gasket and a press component with a diamond anvil diameter of 500 micrometers (the remaining parts of a manually pressurized symmetrical DAC press after removing the manual pressurization screw) were fixed into a high-pressure press. The press and the gasket inside the press were pressurized by controlling an electric cylinder. When the pressure on the gasket reached 35-38 GPa, depressurization began until the gasket and diamond anvil were completely separated. A stepper motor was used to move the indentation of the gasket out of the anvil region. The above steps were then repeated to achieve automatic pressurization and depressurization of the WO3 film on the gasket. After more than 30 high-pressure compression processes, the prepared sample was separated and collected.

[0065] The high-pressure press can repeatedly achieve pressures exceeding 35 GPa, breaking through the pressure limit of commercial large-cavity presses (generally less than 30 GPa) without damaging the diamond anvil, thus significantly reducing operating costs. The high-pressure treated tungsten trioxide samples have cubic millimeter-scale dimensions, and their color irreversibly changes from pale yellow to blue (or dark blue), exhibiting strong light absorption in the near-red light band. Compared to manual preparation, the high-pressure press can rapidly obtain millimeter-scale high-pressure materials, which is beneficial for promoting basic research and the practical application of high-pressure materials.

[0066] Example 3: Ultra-high pressure treatment was performed using a rhenium metal gasket as a sample. The specific steps are as follows: A press component with a diamond mesa diameter of 200 micrometers (the remaining parts of a manually pressurized symmetrical DAC press after removing the manual pressurization screw) and a 250-micrometer-thick rhenium sheet are fixed into a high-pressure press. The press and the gasket inside are pressurized by a controlled electric cylinder. When the gasket pressure reaches 70-85 GPa, depressurization begins until the gasket and diamond anvil are completely separated. A stepper motor is then controlled to move the gasket indentation out of the anvil region. This process is repeated to achieve automatic pressurization and depressurization of the gasket, ultimately pressing a two-dimensional pit array onto the rhenium sheet. To achieve higher pressures, the diamond mesa can be reduced in size; for example, a 150 μm mesa can achieve pressures exceeding 100 GPa. If the cost of diamond is not a concern, or if synthetic diamonds become cheaper, the maximum pressure can exceed 500 GPa by improving the shape of the diamond anvil and the high-pressure press.

[0067] Example 4: High-temperature and high-pressure synthesis of black phosphorus sample, the specific steps are as follows: A moissanite (SiC, 500 μm diameter circular anvil) and a 250 μm thick T301 stainless steel gasket (with pre-drilled 300 μm holes) are fixed in a high-pressure press. The gasket is controlled by a feeding mechanism to align the holes with the anvil, and red phosphorus (analytical grade) and ruby ​​microparticles are filled into the pressure chamber. The sample is pressurized by a controlled electric cylinder, and the pressure at the sample is determined by the fluorescence peak position of the ruby. When the gasket pressure reaches 2-6 GPa, the anvil and sample are heated by resistance heating, and the sample temperature is measured using a thermocouple attached to the anvil. When the temperature reaches 400-600℃, it is held for 10-60 minutes and then cooled to room temperature. The pressure is then released until the gasket and moissanite anvil are completely separated. A stepper motor is controlled to move the gasket indentation out of the anvil region, and then the black phosphorus in the gasket holes is separated and collected. The above steps are repeated to achieve automatic sample filling, pressurization, holding, cooling, and depressurization. This embodiment illustrates that a high-pressure press can be used to prepare high-pressure phase materials under high temperature and high pressure.

[0068] The automated integrated high-pressure press and its control method provided by this invention include a support mechanism, a drive mechanism, a feeding mechanism, a monitoring module, and a control module. Based on the pressure and temperature parameters, the feeding mechanism and the drive mechanism are controlled so that they cooperate with the support mechanism to process the gasket or material at least once, producing at least one batch of high-pressure material. This invention employs a small-batch, multiple-processing strategy, enabling low-cost batch production of materials under high pressure. It is more suitable for applications where single-crystal volume requirements are not high, and does not increase the manufacturing and production costs of high-pressure equipment.

[0069] Through the above description of the embodiments, those skilled in the art can clearly understand that each embodiment can be implemented by means of software plus necessary general-purpose hardware platforms, and of course, it can also be implemented by hardware. Based on this understanding, the above technical solutions, in essence or the part that contributes to the prior art, can be embodied in the form of a software product. This computer software product can be stored in a computer-readable storage medium, such as ROM / RAM, magnetic disk, optical disk, etc., and includes several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute the methods described in the various embodiments or some parts of the embodiments.

[0070] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. An automated integrated high-pressure press, characterized in that, The press includes a support mechanism, a drive mechanism, a feeding mechanism, a monitoring module, and a control module. The control module is connected to the drive mechanism, the feeding mechanism, and the monitoring module, respectively. The press also includes a calibration mechanism, which is electrically connected to the control module. The support mechanism is used to fix the top anvil or press component; the top anvil or press component includes at least a pair of anvil assemblies, and the anvil is made of an ultra-hard material. The drive mechanism is connected to the counterweight anvil or the press component and is used to pressurize, maintain pressure or depressurize the counterweight anvil or the press component. The feeding mechanism is located on one side of the support mechanism and is used to feed the pad or material to be pressed into or remove the anvil surface area corresponding to the top pressing anvil or the press component. The feeding mechanism includes a feeding base, a sliding component, a clamping component, and a feeding drive component; the feeding mechanism is located on the side of the press; The sliding member is disposed on the feeding base and slides on the feeding base in at least two dimensions under the drive of the feeding drive member; The clamping member is connected at its bottom to the top of the sliding member, and is used to clamp the pad or the material; The gasket is elongated and has holes or pits on its surface for applying pressure to the anvil. When adding material, it can be added directly to the corresponding position or to the hole or pit at the position. The material includes samples and pressure transmission media or pressure gauges. After the feeding mechanism moves the gasket or material into the anvil surface area, it can be finely adjusted on the x and y axes of the anvil surface to align the holes on the gasket with the center of the anvil surface of the anvil. The monitoring module is used to acquire at least the pressure parameters of the drive mechanism and the corresponding operating parameters of the anvil or the press component, and transmit the pressure parameters and the operating parameters to the control module; the operating parameters include at least the external pressure, internal pressure and temperature of the anvil or the press component; and determine whether pressure holding or temperature adjustment is required based on the preparation conditions of the gasket or material. The control module is used to control the feeding mechanism and the driving mechanism according to the pressure parameters and the working parameters, so that the feeding mechanism, the driving mechanism and the support mechanism cooperate to process the gasket or the material at least once to prepare at least one high-pressure material, or to apply it to in-situ structural property measurement experiments; The calibration mechanism is located above the anvil or press component and is used to detect the position information of the pad or the material in the anvil surface area and send the position information to the control module. The calibration mechanism works in conjunction with the feeding mechanism to achieve accurate positioning of the pad or the material in the anvil surface area.

2. The automated integrated high-pressure press according to claim 1, characterized in that, The top anvil or the press component includes at least one pair of anvil assemblies, which are arranged in a linear or array-like manner. Under the pressure of the drive mechanism, the anvil assemblies pressurize, maintain pressure, or depressurize the gasket or the material according to preset drive parameters.

3. The automated integrated high-pressure press according to claim 2, characterized in that, The material of the anvil is one or more of the following: diamond, silicon carbide, boron nitride, tungsten carbide, alumina, topaz, zircon, quartz, superhard metal steel, chromium, and tungsten steel.

4. The automated integrated high-pressure press according to claim 1, characterized in that, It also includes filling parts; The filling component is connected to the feeding base, and the outlet of the filling component is located above the gasket or the material, for filling the gasket with the material to be pressed.

5. The automated integrated high-pressure press according to claim 1, characterized in that, One end of the feeding base is connected to the driving mechanism. Under the drive of the driving mechanism, the sliding member, the clamping member, and the feeding driving member move along the movement direction of the driving mechanism.

6. The automated integrated high-pressure press according to claim 1, characterized in that, It also includes a temperature regulating mechanism, which is connected to the control module; The temperature regulating mechanism is used to adjust the temperature of the top pressure anvil or press components, support mechanism and drive mechanism; The monitoring module, control module, and temperature regulation mechanism work together to achieve precise adjustment of the ambient temperature of the support structure, meeting the preparation conditions of various gaskets or materials.

7. The automated integrated high-pressure press according to claim 1, characterized in that, The pressure range generated by the drive mechanism is 0.1 GPa - 500 GPa.

8. A method for controlling the automated integrated high-pressure press according to any one of claims 1-7, characterized in that, include: Obtain monitoring data; Based on the monitoring data, the drive mechanism and the support mechanism are controlled to cooperate in performing steady-state pressurization or dynamic pressurization, and the pressure value of the drive mechanism is monitored during the pressurization process. If the pressure value reaches the preset value, the drive mechanism and the support mechanism are controlled to cooperate in performing pressure holding, steady state or dynamic pressure relief operations; After the pressure relief operation is completed, control the feeding mechanism to move the gasket or the material, and repeat the above steps.

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