CN111774102A

CN111774102A - Pressure disc and high-temperature high-pressure synthesis equipment

Info

Publication number: CN111774102A
Application number: CN202010575002.9A
Authority: CN
Inventors: 校文超; 岳�文; 孟德忠; 康嘉杰
Original assignee: China University of Geosciences Beijing
Current assignee: Zhengzhou Research Institute of China University of Geosciences (Beijing); China University of Geosciences Beijing
Priority date: 2020-06-22
Filing date: 2020-06-22
Publication date: 2020-10-16
Anticipated expiration: 2040-06-22
Also published as: CN111774102B

Abstract

The invention provides a pressure plate which comprises a cylinder assembly, wherein a sealed cavity is arranged in the cylinder assembly, a sample bin is arranged in the sealed cavity, the diameter of the sealed cavity is D, the diameter of the sample bin is D, and D is larger than or equal to 4D and larger than or equal to 3D. The invention also provides high-temperature high-pressure synthesis equipment which comprises the pressure disc, and the high-temperature high-pressure synthesis equipment can ensure the proper volume ratio of the sample bin to the closed containing cavity, further improve the uniformity and stability of a temperature field and a pressure field during experiments, and maintain the long-time accurate control of the temperature and the pressure of the sample bin in the device.

Description

Pressure disc and high-temperature high-pressure synthesis equipment

Technical Field

The invention relates to the field of geological experimental devices, in particular to a pressure disc and high-temperature high-pressure synthesis equipment.

Background

The high-temperature high-pressure synthesis press is a high-temperature high-pressure instrument widely applied in the field of international static high-pressure large-cavity experiments at present. The conditions such as temperature, pressure, components, oxygen fugacity and the like in the earth are simulated, the internal environment of the earth is simulated, a new material is prepared, and the unique physical properties under high pressure are explored.

In the prior art, the volume ratio of a sample bin and a closed cavity of a high-temperature and high-pressure synthesis press is not appropriate, the volume ratio of the sample bin and the closed cavity is overlarge, and due to the fact that the closed cavity has obvious gradient descending conditions of temperature and pressure at the edge part, a temperature field and a pressure field in the sample bin are greatly descended and distributed from the center to the periphery, and the requirement of accurate control of a synthesis experiment cannot be met; if the volume ratio of the sample bin to the closed cavity is too small, the loading equipment for realizing the secondary high pressure required by the closed cavity is extremely large, and the economical efficiency is not proper.

High-pressure equipment such as a press for synthesizing diamond and the like puts higher requirements on the uniformity and stability of a pressure field and a temperature field in a sample bin.

Therefore, the pressure plate needs to be invented, the volume ratio of the sample bin to the closed containing cavity is appropriate, the uniformity and stability of the temperature field and the pressure field of the sample bin can be improved, and the long-time accurate and stable work of a high-temperature high-pressure synthesis instrument is facilitated.

Disclosure of Invention

In view of this, the invention aims to provide a pressure disc, which solves the technical problems that the volume ratio of a sample bin to a closed cavity is not suitable, and the uniformity and stability of a temperature field and a pressure field are poor.

In order to achieve the purpose, the technical scheme of the invention is realized as follows:

the pressure plate comprises a cylinder assembly, wherein a sealed cavity is arranged inside the cylinder assembly, a sample bin is arranged inside the sealed cavity, the diameter of the sealed cavity is D, the diameter of the sample bin is D, D is larger than or equal to 3D, and the volume ratio of the sample bin to the sealed cavity is appropriate.

Further, the drum subassembly includes urceolus, inner tube, piston and supporting pad, the urceolus cover is established the inner tube is outside, the piston sets up inner tube upper portion, the supporting pad sets up the lower part of inner tube, the inner tube with the piston the supporting pad encloses out airtight chamber, airtight chamber linear motion is followed to the piston.

Further, sealed intracavity portion is provided with first pipe box and second pipe box, first pipe box cover is established the second pipe box is outside, the bottom is provided with a supporting bench in the second pipe box, second pipe box upper portion is provided with the support stopper, the second pipe box with a supporting bench the support stopper encloses out the sample storehouse.

Further, the pressure plate further comprises an upper cooling plate and a lower cooling plate, the upper portion of the cylinder assembly is fixedly provided with the upper cooling plate, the lower portion of the cylinder assembly is fixedly provided with the lower cooling plate, and the upper cooling plate and the lower cooling plate are respectively provided with a circulating water cooling pipeline. This setting can be respectively to two parts about the pressure disk carry out the temperature drop, regulation temperature that can be faster.

Furthermore, a plurality of thermocouples are arranged in the cylinder assembly along the radial direction, and the arrangement can accurately measure the temperature of the cylinder assembly in a plurality of directions so as to control the temperature of the pressure disc, so that the uniformity and stability of the temperature field in the experiment are better.

Furthermore, be provided with a plurality of pressure sensor in the pressure disk, can diversely detect the pressure of pressure disk to control pressure disk pressure, in order to realize the uniform stability in pressure field.

The technical scheme of the invention has the following advantages:

(1) according to the pressure plate, the diameter of the closed containing cavity is large, the volume ratio of the sample bin to the closed containing cavity is appropriate, the uniform stability of a temperature field and a pressure field can be effectively controlled, the experimental accuracy is good, and the reliability is good;

(2) the pressure disc has the advantages that the sample bin is large in size, and experiments of large-size samples or experiments of a plurality of small-size samples can be achieved simultaneously.

(3) According to the pressure disc, the upper cooling disc and the lower cooling disc can be respectively cooled by water, so that the temperature of the upper part and the lower part of the pressure disc can be conveniently adjusted, and the uniformity and the stability of a temperature field can be ensured.

The invention also provides high-temperature high-pressure synthesis equipment which comprises the pressure disc. The high-temperature high-pressure synthesis equipment has the beneficial effects as described above.

Drawings

The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:

FIG. 1 is a schematic structural diagram of a high-temperature high-pressure synthesizer according to an embodiment of the present invention;

FIG. 2 is an enlarged view taken at A of FIG. 1 in accordance with the present invention;

FIG. 3 is a schematic structural diagram of a synthesis apparatus according to an embodiment of the present invention;

FIG. 4 is a schematic structural diagram of a pressure plate according to an embodiment of the present invention;

FIG. 5 is an enlarged view of the invention at B in FIG. 4.

Description of reference numerals:

1. a main press; 11. a set top; 12. a pillar; 13. a sliding disk; 14. a base; 2. a synthesizing device; 21. an upper top loading module; 211. a first terminal post; 212. a top plate is arranged; 213. an upper base plate; 214. a support block; 22. a pressure disc; 221. an upper cooling plate; 2211. an upper water outlet; 2212. an upper water inlet; 2213. an upper tray body; 222. a cylinder assembly; 2220. a support pillar; 2221. a support cover; 2222. a piston; 2223. a support plug; 2224. a sample; 2225. a support pad; 2226. a closed cavity; 2227. an outer cylinder; 2228. an inner barrel; 2229. a sample bin; 223. a lower cooling pan; 2231. a lower water outlet; 2232. a lower water inlet; 2233. a lower tray body; 224. a thermocouple channel; 225. a strain gauge; 226. a support table; 227. a first pipe sleeve; 228. a second pipe sleeve; 2251. measuring a hole; 23. a chassis module; 231. a second terminal; 232. a lower support block; 233. a lower base plate; 234. a lower chassis; 24. a strut; 3. a control system; 4. a regulated power supply; 41. a first electrode; 42. a second electrode; 5. a water cooling machine; 51. a first water outlet; 52. a second water outlet 53 and a second water return port; 54. a first water return port; 6. a hydraulic system.

Detailed Description

It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.

The descriptions of "left", "right", "upper", "lower", etc. in this disclosure are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit indication of the number of technical features indicated and have been identified in the drawings. Thus, a feature defined as "left", "right", "upper", "lower" may explicitly or implicitly include at least one such feature. In addition, the technical solutions in the embodiments may be combined with each other, but it is necessary that a person skilled in the art can realize the combination, and the technical solutions in the embodiments are within the protection scope of the present invention.

The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.

Embodiment as shown in fig. 4 and 5, a pressure disk includes a cylinder assembly 222, the cylinder assembly 222 includes an outer cylinder 2227, an inner cylinder 2228 and a piston 2222, the outer cylinder 2227 is sleeved outside the inner cylinder 2228, and plays a role in protecting the inner cylinder 2228 and playing a role in heat insulation, heat preservation and pressure maintenance, a support pad 2225 is arranged at the lower part of the inner cylinder 2228, a support column 2220 is arranged at the lower part of the support pad 2225, the support column 2220 can support the support pad 2225 and ensure the sealing performance of the inner cylinder 2228, a piston 2222 is connected to the upper part of the inner cylinder 2228 in a reciprocating motion, a support cover 2221 is sleeved on the upper part of the piston 2222, the support cover 2221 plays a role in supporting and protecting the piston, the inner cylinder 2228, the piston 2222 and the support pad 2225 form a sealed cavity 2226, a sample chamber 2229 is arranged in the middle of the sealed cavity 2226, the sample chamber 2229 is used for placing a sample, the first pipe sleeve 227 is sleeved outside the second pipe sleeve 228, the bottom of the second pipe sleeve 228 is provided with a support table 226, the upper part of the second pipe sleeve 228 is provided with a support plug 2223, the first pipe sleeve 227, the second pipe sleeve 228 and the support plug 2223 play a role in transmitting pressure, the support plug 2223 plays a role in protecting a sample 2224 at the same time, the second pipe sleeve 228, the support table 226 and the support plug 2223 enclose a sample bin 2229, the diameter of the closed cavity is D, the diameter of the sample bin 2229 is D, 4D is more than or equal to D and more than or equal to 3D, the length of the closed cavity 2226 is H, H changes along with the position change of the piston 2222, the length of the sample bin 2229 is H, H changes along with the position change of the support plug 2223, when the positions of the piston 2222 and the support plug 2223 under the action of pressure are fixed, 0< H is less than or equal to H, the diameter D of the sample bin 2229 is equal to the diameter of the support plug 2223, equal to the diameter of the piston 2222, to ensure the tightness of the sealed cavity 2226 and the sample chamber 2229, the larger the space of the sealed cavity 2226 is, the easier it is to ensure the gradient uniformity and stability of the temperature and pressure of the experimental sample, but the higher the equipment cost is, the diameter D of the sealed cavity 2226 is related to the pressure provided by the external press, when the volume space of the sealed cavity 2226 is greatly increased, the tonnage of the external press is considered, and in consideration of the economy, the sample 2224 is arranged in the sample chamber 2229, the diameter of the sample 2224 is slightly smaller than that of the sample chamber 2229, preferably, in this embodiment, the diameter of the sample chamber 2229 is 15mm, the diameter of the sealed cavity 2226 is 50mm, the piston 2222 pushes the support plug 2223 by the pressure, after the positions of the piston 2222 and the support plug 2223 are fixed, the length of the sealed cavity 2226 is 150mm, the length of the sample chamber 2229 is 50mm, and this arrangement can be used to accurately, meanwhile, the economy can be considered, the cavity space of the sample bin 2229 is large, the experiment of samples with various specifications can be met, and a plurality of small-size samples can be placed for the experiment at the same time; preferably, the piston 2222, the inner cylinder 2228 and the support pad 2225 are all made of tungsten carbide materials, so that the piston can better bear high temperature and high pressure;

further, a plurality of pressure sensors are arranged in the pressure disc, in this embodiment, the pressure sensors are strain gauges 225, the strain gauges 225 have small volume, the structure of the pressure disc is not affected, and the pressure sensors can be flexibly arranged, a plurality of strain gauges 225 are arranged on the circumferential outer surfaces of the inner cylinder 2228, the outer cylinder 2227, the piston 2222 and the support column 2220 to measure the pressure in the experiment, a measurement hole 2251 needs to be formed when the strain gauge 225 is arranged in the pressure disc, a plurality of strain gauges 225 are arranged on the upper end surface and the lower end surface of the inner cylinder 2228 and the outer cylinder 2227, a measurement hole (not shown in the figure) needs to be formed, a plurality of thermocouple channels 224 are arranged on the periphery of the inner cylinder 2228 close to the sealed cavity 2226, the thermocouple channels 224 are arranged in the centers of the support pad 2225 and the support column 2220 until the support pad is close to the sample chamber 2229, the thermocouple is used for installing the thermocouple to monitor the temperature of different points of the inner, in the design, the lead-out holes are distributed along the circumferential direction, and the solid lines and the broken lines of the thermocouple channels 224 in fig. 4 indicate that thermocouples at different positions are in different circumferential directions. The real-time temperature and pressure monitoring of the multiple points of the pressure disc provides data guarantee for the reliable and stable operation of the pressure disc.

Further, as shown in fig. 4, the pressure plate further includes an upper cooling plate 221 and a lower cooling plate 223, the upper cooling plate 221 is fixed on the upper portion of the cylinder assembly 222 by bolts, the lower cooling plate 223 is fixed on the lower portion of the cylinder assembly 222 by bolts, the upper cooling plate 221 includes an upper water outlet 2211, an upper water inlet 2212 and an upper plate 2213, a circular hole is formed in the center of the upper plate 2213 for the cylinder assembly 222 to reciprocate axially through the hole, the upper water outlet 2211 and the upper water inlet 2212 are connected to the circumferential outer surface of the upper plate 2213, the lower cooling plate 223 includes a lower water outlet 2231, a lower water inlet 2232 and a lower plate 2233, a circular hole is formed in the center of the lower plate 2233 for the cylinder assembly 222 to pass through, the lower water outlet 2231 and the lower water inlet 2212 are connected to the circumferential outer surface of the lower plate 2233, the upper water outlet 2211, the upper water inlet 2, the lower water outlet 2231 and the lower water inlet 2232, water flows in the upper cooling plate 221 and the lower cooling plate 223 respectively, and the upper cooling plate 221 and the lower cooling plate 223 can be cooled separately, so that the cooling effect of the whole pressure plate 22 is better;

further, as shown in fig. 1 and fig. 2, a high-temperature and high-pressure synthesis apparatus applying the pressure plate includes a synthesis device 2, a main press 1, a water cooler 5, a regulated power supply 4, a control system 3 and a hydraulic system 6, where the synthesis device 2 is disposed in the main press 1, and is used to place an experimental sample and perform a high-temperature and high-pressure experiment on the sample 2224, the output pressure of the main press 1 acts on the synthesis device 2, the synthesis device 2 is connected to the water cooler 5 through a plurality of circulating water cooling pipelines, and is used to cool the synthesis device 2 and control the temperature drop of the synthesis device 2, the synthesis device 2 is connected to the regulated power supply 4 through a wire, so as to heat the synthesis device 2 and control the experimental temperature of the sample 2224 by matching with the circulating water cooling pipelines, and the hydraulic system 6 is a servo control secondary pressurization system, the main press machine 1 is connected with the main press machine and is used for stably providing the pressure required by the experiment; and the control system 3 is respectively connected with the hydraulic system 6, the stabilized voltage power supply 4, the water cooling machine 5, the main press 1 and the synthesis device 2 so as to control and display the running state of the synthesis device.

Further, main press 1 includes roof 11, pillar 12, sliding disc 13, base 14, roof 11 with base 14 is fixed respectively and sets up both ends about pillar 12, sliding disc 13 cover is established on pillar 12, sets up between roof 11 and base 14, slides from top to bottom along pillar 12, sliding disc 13 with be provided with synthesizer 2 between the base 14, sliding disc 13 with hydraulic system 6 connects, provides pressure by hydraulic system 6, makes sliding disc 13 move down extrusion synthesizer 2, synthesizer 2 bottom and base 14 fixed connection, synthesizer 2 top can be connected with sliding disc 13, and synthesizer 2 top can be extrudeed the downward movement by sliding disc 13.

Further, the synthesis device 2 comprises a base module 23, a pressure disc 22, an upper top loading module 21 and support rods 24, wherein the pressure disc 22 is arranged between the base module 23 and the upper top loading module 21 and is fixedly supported by the base module 23, the base module 23 and the upper top loading module 21 are connected through the plurality of support rods 24, the upper top loading module 21 can be connected with the sliding disc 13, the upper top loading module 21 can be pushed by the sliding disc 13 to move downwards and extrude the pressure disc 22 under the action of the sliding disc 13, so that the pressure disc 22 generates high pressure required by an experiment, the support rods 24 are rod pieces sleeved at the lower part and the upper part, when the upper top loading module 21 moves, the support rods 24 can be compressed, when the upper top loading module 21 resets, the support rods 24 reset, the upper top loading module 21 is provided with first binding posts 211, and the first binding posts 211 are connected to the regulated power supply 4 through conducting wires; the base module 23 is fixedly connected with the base 14, the second binding post 231 is arranged on the base module 23, the second binding post 231 is connected to the stabilized voltage power supply 4 through a lead, the first binding post 211 and the second binding post 231 are respectively connected with the positive electrode and the negative electrode of the stabilized voltage power supply 4, and after the power is turned on, the extruded pressure plate 22 can be in a high-temperature state.

Further, as shown in fig. 3, the upper top-loading module 21 further includes an upper top disk 212, an upper backing plate 213, and a supporting block 214, the upper top disk 212, the upper backing plate 213, and the supporting block 214 are sequentially and fixedly connected by bolts, the upper top disk 212 can be connected to the sliding disk 13 and can be pushed by the sliding disk 13 to drive the upper backing plate 213 and the supporting block 214 to move downward, the upper top disk 212 is sleeved on the upper portion of the supporting rod 24 and can move axially along the supporting rod 24, the supporting rod 24 plays a role in supporting and guiding, the upper backing plate 213 is used for fixing the supporting block 214, the supporting cover 2221 penetrates through a hole in the middle of the upper disk 2213 and can be connected to the supporting block 214, the supporting block 214 can play a role in buffering and supporting protection for components in contact with the supporting block 214 during the pressing process, the first terminal 211 is disposed on the circumferential outer surface of;

the base module 23 further comprises a lower supporting block 232, a lower supporting plate 233 and a lower chassis 234, the lower supporting block 232, the lower supporting plate 233 and the lower chassis 234 sequentially pass through the bolt fixed connection, the lower supporting block 232 penetrates through a hole in the middle of the lower disk 2233 to be connected with the supporting column 2220, the supporting and buffering effects on the pressure plate 22 are achieved, the lower supporting plate 233 is used for fixing the supporting block 232, the lower chassis 234 is fixedly connected with the base 14, a second binding post 231 is arranged on the circumferential outer surface of the lower supporting block 232, and the connection of the stabilized voltage power supply 4 is facilitated.

Further, as shown in fig. 1 and fig. 2, the regulated power supply 4 is provided with a first electrode 41 and a second electrode 42, the first electrode 41 is connected with the first terminal 211, the second electrode 42 is connected with the second terminal 231, one of the first electrode 41 and the second electrode 42 is a positive electrode, and the other is a negative electrode, and the regulated power supply 4 can heat the synthesis device 2 to meet the temperature required by the experiment; the water cooler 5 is provided with a first water outlet 51, a second water outlet 52, a second water return port 53 and a first water return port 54, the first water outlet 51 is communicated with the upper water inlet 2212, the first water return port 54 is communicated with the upper water outlet 2211, the second water outlet 52 is communicated with the lower water inlet 2232, the second water return port 53 is communicated with the lower water outlet 2231, the water cooler 5 and the upper cooling plate 221 form a circulating cooling water path, and the water cooler 5 and the lower cooling plate 223 form another circulating cooling water path, so that the cooling speed can be increased, and the temperature of the synthesis device 2 can be better reduced.

In the experiment, the control system 3 firstly controls the output pressure of the hydraulic system 6 to act on the sliding block 13, the sliding block 13 moves downwards along the support column 12 to drive the upper top loading module 21 to move downwards, the support rod 24 is shortened, the extrusion piston 2222 moves downwards along the sealed cavity 2226 after the support block 214 on the upper top loading module 21 contacts the piston cover 2221, so that the support plug 2223 extrudes the sample 2224 to generate pressure, the control system 3 controls the stabilized voltage power supply 4 to heat the synthesis device 2 while the piston 2222 moves downwards, the strain gauge 225 detects the pressure of each measurement point, the thermocouple measures the temperature of the corresponding measurement point, the measured pressure and temperature are fed back to the control system 3, the control system 3 controls the opening and closing of the water cooling machine 5, the water cooling machine 5 can adjust the flow rate of water flowing through the upper cooling disc 221 and the lower cooling disc 223 to effectively perform the operation, the action of the water cooling machine 5 and the stabilized voltage power supply 4 can ensure that the synthesis device 2 generates continuous and stable high, the hydraulic system 6 can ensure that the synthesizer 2 generates a continuous and stable high-pressure environment, signals fed back by the strain gauge 225 and the thermocouple are input to the control system 3 together with running state signals of the main press 1, the water cooler 5 and the stabilized voltage power supply 4, and after program processing, output signals are output to adjust the running states of the main press 1, the water cooler 5, the stabilized voltage power supply 4 and the hydraulic system 6.

After the experiment is finished, the control system 3 controls the hydraulic system 6 to release pressure, controls the water cooling machine 5 to cool the upper cooling disc 221 and the lower cooling disc 223, controls the stabilized voltage power supply 4 to stop heating, and uses the unloading device to take the sample 2224 out of the inner cylinder 2228.

Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims

1. The pressure plate is characterized by comprising a cylinder assembly, wherein a sealed cavity is arranged in the cylinder assembly, a sample bin is arranged in the sealed cavity, the diameter of the sealed cavity is D, the diameter of the sample bin is D, and D is larger than or equal to 4D and larger than or equal to 3D.

2. The pressure plate of claim 1, wherein the cylinder assembly comprises an outer cylinder, an inner cylinder, a piston and a support pad, the outer cylinder is sleeved outside the inner cylinder, the piston is arranged on the upper portion of the inner cylinder, the support pad is arranged on the lower portion of the inner cylinder, a sealed cavity is defined by the inner cylinder, the piston and the support pad, and the piston moves linearly along the sealed cavity.

3. The pressure plate as claimed in claim 2, wherein a first pipe sleeve and a second pipe sleeve are arranged inside the sealed cavity, the first pipe sleeve is sleeved outside the second pipe sleeve, a support platform is arranged at the bottom inside the second pipe sleeve, a support plug is arranged at the upper part of the second pipe sleeve, and a sample bin is enclosed by the second pipe sleeve, the support platform and the support plug.

4. The pressure disc of claim 2, further comprising an upper cooling disc and a lower cooling disc, wherein the upper cooling disc is fixedly arranged on the upper portion of the cylinder assembly, the lower cooling disc is fixedly arranged on the lower portion of the cylinder assembly, and the upper cooling disc and the lower cooling disc are respectively provided with a circulating water cooling pipeline.

5. A pressure disc according to claim 2, wherein a plurality of thermocouples are radially arranged inside the cylindrical assembly.

6. The pressure disk of claim 2, wherein a plurality of pressure sensors are disposed within the hts pressure disk.

7. A high temperature and high pressure synthesis apparatus comprising the pressure disk of any one of claims 1 to 6.