High-temperature and high-pressure dynamic detection system for synchronous laser heating and rapid pressurization

Abstract

The invention provides a high-temperature and high-pressure dynamic detection system capable of synchronizing laser heating and rapid pressurization. The high-temperature and high-pressure dynamic detection system comprises a rapid pressurization control module, a laser heating module, a microscopic imaging module and a Raman spectrum characterization module, wherein the rapid pressurization control module comprises a clamp assembly and a pressurization assembly, the clamp assembly comprises a clamp, a gas diaphragm and a four-column type anvil cell used for loading a sample, the pressurization assembly comprises an electromagnetic valve, a pressure reducing valve and a high-pressure gas cylinder, and the gas diaphragm is connected with the high-pressure gas cylinder through a capillary tube; the device has the beneficial effects that under the synergistic effect of the integrated clamp structure, the gas film driving module, the laser heating module and the high-resolution Raman spectrum module, millisecond-level rapid pressure loading in a high-temperature and high-pressure environment is realized; the method has great significance on research of planet internal substance evolution, metastable state material synthesis under extreme conditions and other scientific problems, and the problem of compatibility of extreme temperature and pressure dynamic synthesis and characterization based on diamond anvil cells is solved.

Description

Technical Field

[0001] The present invention relates to the technical field of high-pressure physical chemistry and material synthesis, and in particular to a high-temperature and high-pressure dynamic detection system for synchronous laser heating and rapid pressurization. Background Art

[0002] Diamond anvil cells, a core instrument for high-pressure scientific research, have long been constrained by traditional mechanical drive systems for pressurization technology. Existing mechanical screw adjustment systems rely on stepper motors. While single-stroke precision can reach micrometers, pressurization rates are generally below 10 GPa / s, significantly below the critical phase transition rate (typically >50 GPa / s) required for the formation of metastable materials. In scientific research, key parameters for simulating planetary interior environments include high temperature, high pressure, and rapid pressurization rates. High-pressure simulations of Earth's core require loading millions of atmospheres of pressure within milliseconds at a few thousand Kelvin to replicate celestial collisions. When pressurization rates exceed the rate of metastable material formation, previously undiscovered new materials with novel properties can be synthesized. Precision control of pressure film deformation is widely used in industry. Incorporating this technology into diamond anvil cell rapid pressurization systems, using gas flow to control film expansion to achieve rapid pressurization in a short period of time, achieving pressurization rates exceeding 100 GPa / s and preserving samples for characterization, remains a pressing technical challenge in the field of rapid pressurization. Summary of the Invention

[0003] In view of the shortcomings of the prior art described above, the purpose of the present invention is to provide a high-temperature and high-pressure dynamic detection system with synchronous laser heating and rapid pressurization, which is used to solve the problem in the prior art of how to introduce the precise control achieved by the deformation of the gas pressure film into the diamond anvil rapid pressurization system, so that the gas flow rate can be used to control the expansion of the gas film to achieve rapid pressurization in a short time.

[0004] To achieve the above-mentioned and other related purposes, the present invention provides the following technical solutions:

[0005] A high-temperature and high-pressure dynamic detection system with synchronous laser heating and rapid pressurization includes a rapid pressurization control module for pressurizing the sample, a laser heating module for high-temperature heating of the sample, a microscopic imaging module and a Raman spectroscopy characterization module for real-time monitoring of the sample pressure; wherein, the rapid pressurization control module includes a clamp assembly and a pressurization assembly, the clamp assembly includes a clamp, an air film installed in the clamp in sequence, a first metal gasket and a four-column anvil for loading the sample, the pressurization assembly includes a solenoid valve, a pressure reducing valve and a high-pressure gas cylinder, the air film is connected to the high-pressure gas cylinder through a capillary, and the solenoid valve and the pressure reducing valve are arranged in sequence on the capillary between the air film and the high-pressure gas cylinder.

[0006] In one embodiment of the present invention, the four-pillar anvil includes a first support ring, a first diamond mounted on the first support ring, a second support ring, and a second diamond mounted on the second support ring, a second metal gasket is provided between the first diamond and the second diamond, and a sample cavity for placing a sample is formed between the first diamond, the second diamond, and the second metal gasket, and a ruby ball for calibrating pressure is provided in the sample cavity.

[0007] In one embodiment of the present invention, a first thread is provided on a circumferential side surface of the second support ring, and a second thread matching the first thread is provided on an inner side surface of the clamp corresponding to the first thread.

[0008] In one embodiment of the present invention, the four-column anvil also includes a pressure screw, a threaded hole is provided in the first support ring, and a through hole is provided in the second support ring. The pressure screw can pass through the through hole and be threadedly connected to the threaded hole. A guide column is also provided in the first support ring, and one end of the guide column passes through the first support ring and is slidably connected to the second support ring.

[0009] In one embodiment of the present invention, the laser heating module includes an infrared laser, a shutter switch, a polarization beam splitter cube, a first half-wave plate, a first polarization crystal, a first beam cutoff, a first half-reflective half-mirror, a first attenuation plate, and a first microscope objective lens located on the side of the fixture, which are arranged in sequence along the first heating light path. The laser heating module also includes a first plane reflector, a second half-wave plate, a second polarization crystal, a second beam cutoff, a second half-reflective half-mirror, a second attenuation plate, and a second microscope objective lens located on the side of the fixture away from the first microscope objective lens, which are arranged in sequence along the second heating light path.

[0010] In one embodiment of the present invention, the laser heating module also includes a fifth half-reflecting half-mirror, a temperature measuring spectrometer and a first CCD imager, which are arranged in sequence along the first radiation collection light path and located on the side of the first half-reflecting half-mirror away from the first attenuation plate. The laser heating module also includes a third half-reflecting half-mirror, a fourth half-reflecting half-mirror and a second plane reflector, which are arranged in sequence along the second radiation collection light path and located on the side of the second half-reflecting half-mirror away from the second attenuation plate.

[0011] In one embodiment of the present invention, the microscopic imaging module includes a first visible light source arranged in sequence along the first imaging light path and a sixth half-reflective half-mirror located directly below the first half-reflective half-mirror. The microscopic imaging module also includes a second visible light source arranged in sequence along the second imaging light path and a seventh half-reflective half-mirror located directly below the fourth half-reflective half-mirror.

[0012] In one embodiment of the present invention, the microscopic imaging module also includes a second CCD imager arranged along the first return light path and located directly below the sixth semi-reflective half-mirror, and the microscopic imaging module also includes a third CCD imager arranged along the second return light path and located directly below the seventh semi-reflective half-mirror.

[0013] In one embodiment of the present invention, the Raman spectrum characterization module includes a Raman laser, a third attenuation plate, a first plano-convex lens, and an eighth semi-reflective half-mirror located on the side of the third semi-reflective half-mirror away from the second semi-reflective half-mirror, which are arranged in sequence along the optical path for collecting Raman signals. The Raman spectrum characterization module also includes a second plano-convex lens, a third plano-convex lens, a first BNF, a second BNF, a Raman spectrometer, and a fourth CCD imager, which are arranged in sequence along the optical path for collecting Raman signals and located on the side of the eighth semi-reflective half-mirror away from the third semi-reflective half-mirror.

[0014] As described above, the present invention provides a high-temperature, high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization, which has the following beneficial effects: the present invention can enable / disable gas flow in an extremely short period of time through a solenoid valve, thereby achieving the purpose of increasing the anvil pressure in a short period of time. The air film will expand under the action of the high-pressure gas cylinder, thereby squeezing the first support ring so that the first support ring and the first diamond move, thereby achieving the purpose of rapidly pressurizing the sample between the diamonds; the high temperature is generated by utilizing an infrared laser, which can directly heat dark samples and can be built-in thermocouples for light samples. The blackbody radiation during heating is collected through the optical path, and the sample temperature is obtained by fitting the Planck formula; the present invention realizes millisecond-level rapid pressure loading under a high-temperature, high-pressure environment under the synergistic effect of the integrated fixture structure, air film drive module, laser heating module and high-resolution Raman spectroscopy module, and can transfer the loaded sample to other platforms for testing. This is of great significance for studying scientific issues such as the evolution of planetary interior matter and the synthesis of metastable materials under extreme conditions, and solves the compatibility problem of extreme temperature and pressure dynamic synthesis and characterization based on diamond anvils. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 Shown is a schematic diagram of the overall structure of a fixture assembly in a high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization disclosed in an embodiment of the present invention;

[0016] Figure 2 Shown is a schematic internal cross-sectional view of a four-pillar anvil in a high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization disclosed in an embodiment of the present invention;

[0017] Figure 3Shown is a schematic diagram of the overall structure of a high-temperature and high-pressure dynamic detection system for simultaneous laser heating and rapid pressurization disclosed in an embodiment of the present invention;

[0018] Figure 4 A schematic diagram showing the pressurization rates of anvils with different anvil surfaces under the same conditions in a high-temperature and high-pressure dynamic detection system for simultaneous laser heating and rapid pressurization disclosed in an embodiment of the present invention;

[0019] Figure 5 It shows a schematic diagram of the instantaneous temperature of 2870±19K fitted by Planck's formula when a 100um anvil diamond is rapidly pressurized in the high-temperature and high-pressure dynamic detection system of synchronous laser heating and rapid pressurization disclosed in an embodiment of the present invention.

[0020] Component number description

[0021] 1. Fixture; 2. Air film; 3. First metal gasket; 4. Four-post anvil; 401. Pressure screw; 402. First support ring; 403. First diamond; 404. Second support ring; 405. Second diamond; 406. Guide post; 5. Capillary; 6. Second metal gasket; 7. Sample chamber; 8. Ruby ball; 9. First thread; 10. Threaded hole; 11. Through hole; 12. Solenoid valve; 13. Pressure reducing valve; 14. High-pressure gas cylinder; 15. Infrared laser; 16. Shutter switch; 17. Polarization beam splitter cube; 18. First half-wave plate; 19. First polarization crystal; 20. First beam cutoff; 21. First half-reflecting mirror; 22. First attenuator; 23. First microscope objective; 24. First plane mirror; 25. Second half-wave plate; 26. Second polarization crystal Oscillator crystal; 27. Second beam cutoff; 28. Second semi-reflecting half-mirror lens; 29. Second attenuation plate; 30. Second microscope objective lens; 31. Temperature measurement spectrometer; 32. First CCD imager; 33. Third semi-reflecting half-mirror lens; 34. Fourth semi-reflecting half-mirror lens; 35. Second plane reflector; 36. Fifth semi-reflecting half-mirror lens; 37. First visible light source; 38. Sixth semi-reflecting half-mirror lens; 39. Second CCD imager; 40. Second visible light source; 41. Seventh semi-reflecting half-mirror lens; 42. Third CCD imager; 43. Raman laser; 44. Third attenuation plate; 45. First plano-convex lens; 46. Eighth semi-reflecting half-mirror lens; 47. Second plano-convex lens; 48. Third plano-convex lens; 49. First BNF; 50. Second BNF; 51. Raman spectrometer; 52. Fourth CCD imager. DETAILED DESCRIPTION

[0022] The following specific embodiments illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. It should be noted that the following embodiments and features in the embodiments can be combined with each other unless there is a conflict.

[0023] See also Figures 1 to 3 The present invention provides a high-temperature and high-pressure dynamic detection system with synchronous laser heating and rapid pressurization, specifically a gas film rapid pressurization device and control method for a diamond anvil cell (DAC), which is suitable for the synthesis and characterization of metastable materials under ultra-high pressure environments (>10GPa), and is particularly suitable for the rapid pressure loading requirements of scenarios such as synchrotron radiation and optical testing. The system includes a rapid pressurization control module for pressurizing the sample, a laser heating module for high-temperature heating of the sample, a microscopic imaging module, and a Raman spectroscopy characterization module for real-time monitoring of the sample pressure. The laser heating and accelerated pressurization processes need to be completed under the control of a synchronous trigger signal, and the time synchronization error is less than 0.1 second.

[0024] The rapid pressurization control module includes a fixture assembly and a pressurization assembly. The fixture assembly includes a fixture 1, an air film 2 sequentially installed in the fixture 1, a first metal gasket 3, and a four-post anvil 4 for loading the sample. The fixture 1 is a hollow cylindrical fixture made of 440C stainless steel. The outer diameters of the air film 2 and the first metal gasket 3 are slightly smaller than the inner diameter of the fixture 1. The material of the first metal gasket 3 is copper or titanium alloy. The four-post anvil 4 adopts a GG-Cell structure. The GG-Cell structure uses four guide pillars 406 instead of an integrated diamond anvil device to allow more operations around the diamond.

[0025] The four-column anvil 4 includes a first support ring 402, a first diamond 403 mounted on the first support ring 402, a second support ring 404 and a second diamond 405 mounted on the second support ring 404. A second metal gasket 6 is provided between the first diamond 403 and the second diamond 405. The second metal gasket 6 is made of stainless steel or rhenium. A sample cavity 7 for placing a sample is formed between the first diamond 403, the second diamond 405 and the second metal gasket 6. A ruby ball 8 for calibrating pressure is provided in the sample cavity 7. A first thread 9 is provided on the circumferential side surface of the second support ring 404. A second thread matching the first thread 9 is provided on the inner side surface of the fixture 1 corresponding to the first thread 9. In the embodiment, the second thread in the fixture 1 is threadedly connected to the first thread 9, so that the four-column anvil 4 can be installed in the fixture 1; the four-column anvil 4 also includes a pressure screw 401, a threaded hole 10 is provided in the first support ring 402, and a through hole 11 is provided in the second support ring 404. The pressure screw 401 can pass through the through hole 11 and be threadedly connected to the threaded hole 10. It should be noted that the initial pressure of the four-column anvil 4 is adjusted by the four pressure screws 401, and after the rapid pressurization is completed, the final pressure is maintained by manually tightening the pressure screws 401 while releasing air; a guide column 406 is also provided in the first support ring 402, and one end of the guide column 406 passes through the first support ring 402 and is slidably connected to the second support ring 404;

[0026] The pressurizing component includes a solenoid valve 12, a pressure reducing valve 13 and a high-pressure gas cylinder 14. The air film 2 is connected to the high-pressure gas cylinder 14 through a stainless steel capillary 5. The solenoid valve 12 and the pressure reducing valve 13 are sequentially arranged on the capillary 5 between the air film 2 and the high-pressure gas cylinder 14. The high-pressure gas cylinder 14 is filled with an inert gas with a pressure of 10-200 bar, which is used to drive the air film 2 to expand to achieve rapid pressurization. The gas filled in the high-pressure gas cylinder 14 is argon, nitrogen or helium. It should be noted that the rapid pressurization system: Figure 3 The dotted line portion is the capillary 5, which is used as the power for the expansion of the air film. It starts from the high-pressure gas cylinder 14, passes through the pressure reducing valve 13 and the solenoid valve 12, and reaches the air film sheet 2 in the fixture 1.

[0027] The laser heating module includes an infrared laser 15, a shutter switch 16, a polarization beam splitter cube 17, a first half-wave plate 18, a first polarization crystal 19, a first beam cutoff 20, a first half-reflecting half-mirror 21, a first attenuation plate 22, a first microscope objective 23, a first plane reflector 24, a second half-wave plate 25, a second polarization crystal 26, a second beam cutoff 27, a second half-reflecting half-mirror 28, a second attenuation plate 29, a second microscope objective 30, a third half-reflecting half-mirror 33, a fourth half-reflecting half-mirror 34, a second plane reflector 35, a fifth half-reflecting half-mirror 36, a temperature measurement spectrometer 31 and a first CCD imager 32. It should be noted that the optical path of the infrared heating system: it starts with the infrared laser 15, the shutter switch 16 is turned on during heating, the heating beam passes through the polarization beam splitter cube 17 and is divided into two beams, the first beam passes through the first half-wave plate 18, the first polarization crystal 19, the first beam cutoff 2 0, the first semi-reflecting half-mirror 21, the first attenuation plate 22, and the first microscope objective lens 23 reach the sample position in the four-column anvil 4 in the fixture 1, and the collected radiation light path passes through the first microscope objective lens 23, the first attenuation plate 22, the first semi-reflecting half-mirror 21, the fifth semi-reflecting half-mirror 36, the temperature measurement spectrometer 31, and the first CCD imager 32 in sequence; the second beam passes through the polarization beam splitter cube 17, the first plane mirror 24, the second half-wave plate 25, the second polarization crystal 26, the second beam cutoff 27, the second semi-reflecting half-mirror 28, the second attenuation plate 29, and the second microscope objective lens 30 to reach the sample position in the four-column anvil 4 in the fixture 1, and the collected radiation light path passes through the second microscope objective lens 30, the second attenuation plate 29, the second semi-reflecting half-mirror 28, the third semi-reflecting half-mirror 33, the fourth semi-reflecting half-mirror 34, the second plane mirror 35, the fifth semi-reflecting half-mirror 36, the temperature measurement spectrometer 31, and the first CCD imager 32 in sequence.

[0028] The microscopic imaging module includes a first visible light source 37, a sixth semi-reflecting half-mirror 38, a first semi-reflecting half-mirror 21 shared with the laser heating module, a first attenuation plate 22 and a first microscope objective 23, a second visible light source 40, a seventh semi-reflecting half-mirror 41, a second microscope objective 30 shared with the laser heating module, a second attenuation plate 29, a second semi-reflecting half-mirror 28, a third semi-reflecting half-mirror 33 and a fourth semi-reflecting half-mirror 34, a second CCD imager 39 and a third CCD imager 42; it should be noted that the optical path of the microscopic imaging system is divided into two-sided imaging: (1) starting from the first visible light source 37 through the sixth semi-reflecting half-mirror 38, the first semi-reflecting half-mirror 21, the first attenuation plate 22, the seventh semi-reflecting half-mirror 41, the second microscope objective 30 shared with the laser heating module, a second attenuation plate 29, the second semi-reflecting half-mirror 28, the third semi-reflecting half-mirror 33 and the fourth semi-reflecting half-mirror 34, the second CCD imager 39 and the third CCD imager 42. A microscope objective lens 23 reaches the sample plane of the four-column anvil 4, and the return light path is the first microscope objective lens 23, the first attenuation plate 22, the first semi-reflecting half-mirror 21, the sixth semi-reflecting half-mirror 38, and the second CCD imager 39; (2) starting from the second visible light source 40, passing through the seventh semi-reflecting half-mirror 41, the fourth semi-reflecting half-mirror 34, the third semi-reflecting half-mirror 33, the second semi-reflecting half-mirror 28, the second attenuation plate 29, and the second microscope objective lens 30 to reach the sample plane of the four-column anvil 4, and the return light path is the second microscope objective lens 30, the second attenuation plate 29, the second semi-reflecting half-mirror 28, the third semi-reflecting half-mirror 33, the fourth semi-reflecting half-mirror 34, the seventh semi-reflecting half-mirror 41, and the third CCD imager 42.

[0029] The Raman spectrum characterization module includes a Raman laser 43, a third attenuation plate 44, a first plano-convex lens 45, an eighth semi-reflecting half-mirror 46, a second microscope objective lens 30 shared with the laser heating module, a second attenuation plate 29, a second semi-reflecting half-mirror 28 and a third semi-reflecting half-mirror 33, a second plano-convex lens 47, a third plano-convex lens 48, a first BNF 49, a second BNF 50, a Raman spectrometer 51 and a fourth CCD imager 52; it should be noted that the Raman system optical path: emitted by the Raman laser 43, passing through the third attenuation plate 44, the first plano-convex lens 45. The eighth semi-reflecting mirror 46, the third semi-reflecting mirror 33, the second semi-reflecting mirror 28, the second attenuation plate 29, and the second microscope objective lens 30 arrive at the ruby ball 8 in the four-column anvil 4 in the fixture 1 (close to the sample), and the optical path for collecting Raman signals is the second microscope objective lens 30, the second attenuation plate 29, the second semi-reflecting mirror 28, the third semi-reflecting mirror 33, the eighth semi-reflecting mirror 46, the second plano-convex lens 47, the third plano-convex lens 48, the first BNF49, the second BNF50, the Raman spectrometer 51, and the fourth CCD imager 52.

[0030] Specifically, embodiment (high temperature rapid pressurization verification): The following will be combined with the drawings in the present invention to fully and clearly describe the technical solution in the implementation of the present invention: The specific operating steps are as follows:

[0031] Step 1: After the sample is pre-loaded in the four-post anvil 4 and maintained at the initial pressure, denoted as a GPa, it should be noted that the second metal gasket 6 is placed between the two diamonds and pre-pressed to about 20 GPa. The second metal gasket 6 is removed, and a sample cavity 7 is burned out in the pre-pressed pit using a laser according to actual experimental requirements; the second metal gasket 6 is ultrasonically cleaned and reset to the middle of the two diamonds according to the traces of the original pre-pressed pit; a ruby ball 8 is placed in the sample cavity for pressure detection. For gaseous, liquid, and solid samples, a gas loading device, a syringe, and a tungsten needle are used to place the sample into the sample cavity respectively. Initially, the four pressure screws 401 are slightly tightened to achieve the purpose of maintaining pressure;

[0032] Step 2: Assemble the integrated fixture: Place the air film 2 at the bottom of the fixture 1, followed by the first metal gasket 3 for pressure transmission, and finally the four-column anvil 4 with a threaded top and a pre-installed sample. Then, insert the capillary tube 5 into the air film 2 and connect it to the high-pressure gas cylinder 14.

[0033] Step 3: Place the integrated fixture on the high-precision three-dimensional translation stage of the optical platform, and locate the sample through the microscopic imaging module. It should be noted that the four-column anvil 4 with the sample loaded is first placed on the high-precision three-dimensional translation stage. By adjusting the operating levers in the high-precision three-dimensional translation stage except for the focal length adjustment direction, the visible light spot emitted from the microscopic imaging module is roughly in the middle of the diamond anvil; then, the operating lever in the focusing direction is fine-tuned to focus the microscopic image on the plane of the sample cavity 7; and the operating levers in each direction are fine-tuned again to align the laser heating spot with the sample and the Raman laser spot with the ruby ball 8. At this time, the sample positioning work is completed;

[0034] Step 4: Turn on the Raman laser 43 and use the high time resolution mode to monitor the pressure in the four-pillar anvil 4 in real time. It should be noted that after positioning the sample cavity 7, switch it to the run mode in the lightfield software equipped with the Raman system, and select the exposure time required for the experiment (such as 1ms, 0.1ms); then start rapid pressurization and start the run mode at the same time. Within the set single exposure time, the Raman system records the pressure at this time node. After the rapid pressurization is completed, the Raman system will sequentially record and save all pressures within the rapid pressurization time ts used; after the pressurization is completed, the data can be retrieved to accurately find the pressure at each time node, thereby achieving real-time monitoring of the pressure;

[0035] Step 5: Turn on the heating infrared laser 15, adjust the laser power and the attenuation plate to make the sample reach the target temperature, collect the blackbody radiation through the temperature spectrometer 31, and get the sample temperature TK (greater than 1000K) by fitting the Planck formula. It should be noted that the heating part of the steps is: turn on the infrared laser 15, locate the laser heating position as before, turn on the heating laser through the shutter switch 16, and split into two beams of light at the polarization beam splitter cube 17. The first beam of light goes along the first half-wave plate 18 and the first polarization crystal 19 to the first beam cutoff 20. When heating, the first beam cutoff 20 is turned on, and the light beam continues to pass through the first half-reflective half-mirror 21, the first attenuation plate 22, and the first microscope objective 23 to reach the sample. The focusing produced by the objective lens 23 causes the light beam to generate an extremely high temperature at the focal point; the same second light beam synchronously passes through the first plane reflector 24, the second half-wave plate 25, the second polarizing crystal 26, the second beam cutoff 27, the second half-reflecting mirror 28, the second attenuation plate 29, and the second microscope objective lens 30, and the focusing produced by the second microscope objective lens 30 causes the light beam to generate an extremely high temperature at the focal point; the laser power can be adjusted by the first attenuation plate 22 and the second attenuation plate 29 to make the sample reach the target temperature; the extremely high temperature of the sample will generate radiation due to the thermal effect, and this radiation will be collected through the optical path to the temperature measuring spectrometer 31 and the first CCD imager 32, and the relevant temperature is then calculated using the Planck formula. For details, please refer to Figure 5 ;

[0036] Step 6: Quickly open the solenoid valve 12 to connect the gas in the high-pressure gas cylinder 14 with the air diaphragm 2, achieving millisecond-level rapid pressurization. Record the pressurization time ts. The air diaphragm 2 will expand under the action of the high-pressure gas cylinder 14, thereby squeezing the first support ring 402, causing the first support ring 402 and the first diamond 403 to move. At the same time, the guide column 406 will slide in the second support ring 404, and the pressurizing screw 401 will also move in the through hole 11 of the second support ring 404, achieving the purpose of rapidly pressurizing the sample between the diamonds; then manually tighten the pressurizing screw 401 to maintain the final pressure, recorded as bGPa. The pressurization rate of this rapid pressurization is (b–a) / t GPa / s. For details, please refer to Figure 4 ;

[0037] Step 7: Turn off the laser and control system, and take out the four-pillar anvil 4 for subsequent optical testing.

[0038] More specifically, the present invention realizes millisecond-level rapid pressure loading (rate>100GPa / s) under high temperature (greater than 1000K) and high pressure environment through the strategy of integrated fixture structure design and composite multiple systems, and can transfer the loaded sample to other platforms for testing; the present invention independently designs an integrated fixture structure, and assists laser heating means to realize millisecond-level rapid pressure loading under high temperature and high pressure environment, and combines the high-resolution Raman spectroscopy system to detect the signal in real time during the process, which is of great significance for studying scientific problems such as the evolution of planetary interior matter and the synthesis of metastable materials under extreme conditions, and solves the compatibility problem of extreme temperature and pressure dynamic synthesis and characterization based on diamond anvil cells; experimentally verified, the pressurization rate can reach 500GP a / s (it takes about 18ms to increase the pressure from an initial pressure of 0.3GPa to 45GPa); it should be noted that the compatibility difficulty lies in the use of diamond anvils to generate an extremely high-pressure environment, and the use of infrared lasers 15 with a precision optical platform to focus the laser spot on the sample to generate an extremely high-temperature environment. The above two methods have high requirements for sample stability, and the introduction of the air film pressurization system will make the stability of the above systems worse. At the same time, it is also necessary to consider the Raman laser system focusing on the sample to achieve real-time monitoring of the pressure. The use of integrated rapid pressurization loading can keep the movement of the sample in three-dimensional space at the micron level, and the infrared laser and Raman laser spot size used are about 10 microns in size, so the instability problem during multi-module compatibility is solved.

[0039] In summary, the present invention aims to provide a high-temperature, air-film-driven diamond anvil rapid pressurization device. Through the synergistic effects of an integrated fixture design, an air-film drive system, and a laser heating module, this device achieves millisecond-level rapid pressurization (rates >100 GPa / s) under high-pressure (>10 GPa) and high-temperature (>1000 K) environments. The main innovations of this device include:

[0040] Integrated fixture design: A hollow cylindrical fixture 1 made of 440C stainless steel is used. The top is manually pressurized using a pressure screw 401, which allows for quick disassembly and transfer of the sample to the subsequent optical testing platform. The internal threads are equipped with a GG-Cell four-post anvil structure. A metal gasket is placed in the middle as a pressure transmission device to transmit the pressure generated by the air film. The bottom is equipped with an air film sheet 2 that generates the initial pressure. An external stainless steel air pipe is connected to the high-pressure gas cylinder 14 to control the pressure.

[0041] Multi-system organic composite: It integrates a gas film rapid pressurization system, a laser heating system, a microscopic imaging system and a high-time-resolution Raman system. It can control the gas pipe pressure through the solenoid valve 12 at high temperature to achieve the goal of rapid pressurization. The pressure on the diamond anvil depends on the size of the gas film thrust, the time required for the gas film and the high-pressure gas cylinder to balance and pressure, and the time it takes for the solenoid valve to open. The size of the gas film thrust depends on the pressure of the high-pressure gas cylinder 14 (10-200 bar), and the balance time is not affected by the cross-sectional area of the capillary gas pipe. By introducing the solenoid valve 12, the gas can be circulated / cut off in an extremely short time, thereby achieving the purpose of increasing the anvil pressure in a short time. The high temperature is generated by using an infrared laser 15. Dark samples can be directly heated, and light samples can be built-in thermocouples. The blackbody radiation during heating is collected through the optical path, and the sample temperature is obtained by fitting the Planck formula.

[0042] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Any equivalent modifications or variations made by persons skilled in the art without departing from the spirit and technical concepts disclosed herein shall be encompassed by the claims of the present invention.

Claims

1. A high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization, characterized by: It includes a rapid pressurization control module for pressurizing the sample, a laser heating module for high-temperature heating of the sample, a microscopic imaging module, and a Raman spectroscopy characterization module for real-time monitoring of the sample pressure; The rapid pressurization control module includes a fixture assembly and a pressurization assembly, wherein the fixture assembly includes a fixture (1), an air film (2) sequentially installed in the fixture (1), a first metal gasket (3) and a four-column anvil (4) for loading a sample, and the pressurization assembly includes a solenoid valve (12), a pressure reducing valve (13) and a high-pressure gas cylinder (14), wherein the air film (2) is connected to the high-pressure gas cylinder (14) through a capillary (5), and the solenoid valve (12) and the pressure reducing valve (13) are sequentially arranged on the capillary (5) between the air film (2) and the high-pressure gas cylinder (14).

2. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 1, characterized in that: The four-pillar anvil (4) comprises a first support ring (402), a first diamond (403) mounted on the first support ring (402), a second support ring (404), and a second diamond (405) mounted on the second support ring (404); a second metal gasket (6) is provided between the first diamond (403) and the second diamond (405); a sample cavity (7) for placing a sample is formed between the first diamond (403), the second diamond (405), and the second metal gasket (6); a ruby ball (8) for calibrating pressure is provided in the sample cavity (7).

3. The high-temperature and high-pressure dynamic detection system of synchronous laser heating and rapid pressurization according to claim 2 is characterized in that: A first thread (9) is provided on the circumferential side surface of the second support ring (404), and a second thread matching the first thread (9) is provided on the inner side surface of the clamp (1) corresponding to the first thread (9).

4. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 2, characterized in that: The four-column anvil (4) also includes a pressure screw (401), a threaded hole (10) is provided in the first support ring (402), and a through hole (11) is provided in the second support ring (404). The pressure screw (401) can pass through the through hole (11) and be threadedly connected to the threaded hole (10). A guide column (406) is also provided in the first support ring (402), and one end of the guide column (406) passes through the first support ring (402) and is slidably connected to the second support ring (404).

5. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 1 is characterized in that: The laser heating module comprises an infrared laser (15), a shutter switch (16), a polarization beam splitter (17), a first half-wave plate (18), a first polarization crystal (19), a first beam cutoff (20), a first half-reflective half-mirror (21), a first attenuation plate (22), and a first microscope objective lens (23) located on the side of the fixture (1), which are sequentially arranged along the first heating light path. The laser heating module also comprises a first plane reflector (24), a second half-wave plate (25), a second polarization crystal (26), a second beam cutoff (27), a second half-reflective half-mirror (28), a second attenuation plate (29), and a second microscope objective lens (30) located on the side of the fixture (1) away from the first microscope objective lens (23), which are sequentially arranged along the second heating light path.

6. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 5, characterized in that: The laser heating module further comprises a fifth half-reflecting half-mirror (36), a temperature measuring spectrometer (31) and a first CCD imager (32) which are sequentially arranged along the first radiation collecting optical path and located on the side of the first half-reflecting half-mirror (21) away from the first attenuation plate (22); the laser heating module further comprises a third half-reflecting half-mirror (33), a fourth half-reflecting half-mirror (34) and a second plane reflecting mirror (35) which are sequentially arranged along the second radiation collecting optical path and located on the side of the second half-reflecting half-mirror (28) away from the second attenuation plate (29).

7. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 1, characterized in that: The microscopic imaging module includes a first visible light source (37) arranged in sequence along the first imaging light path and a sixth semi-reflective half-mirror (38) located directly below the first semi-reflective half-mirror (21). The microscopic imaging module also includes a second visible light source (40) arranged in sequence along the second imaging light path and a seventh semi-reflective half-mirror (41) located directly below the fourth semi-reflective half-mirror (34).

8. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 7, characterized in that: The microscopic imaging module also includes a second CCD imager (39) arranged along the first return light path and located directly below the sixth semi-reflective half-mirror (38), and the microscopic imaging module also includes a third CCD imager (42) arranged along the second return light path and located directly below the seventh semi-reflective half-mirror (41).

9. The high-temperature and high-pressure dynamic detection system with simultaneous laser heating and rapid pressurization according to claim 1, characterized in that: The Raman spectrum characterization module includes a Raman laser (43), a third attenuation plate (44), a first plano-convex lens (45), and an eighth semi-reflective half-mirror (46) located on the side of the third semi-reflective half-mirror (33) away from the second semi-reflective half-mirror (28), which are sequentially arranged along the optical path for emitting the Raman signal. The Raman spectrum characterization module also includes a second plano-convex lens (47), a third plano-convex lens (48), a first BNF (49), a second BNF (50), a Raman spectrometer (51), and a fourth CCD imager (52), which are sequentially arranged along the optical path for collecting the Raman signal and located on the side of the eighth semi-reflective half-mirror (46) away from the third semi-reflective half-mirror (33).

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