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Device for measuring high temperature and high pressure transport properties based on diamond opposed anvils

A diamond anvil, high temperature and high pressure technology, applied in the direction of material resistance, material thermal development, etc., can solve the problems of high experimental equipment requirements, complex experimental technology, large temperature measurement error, etc., to reduce the difficulty of experimental operation and widen the experiment. The effect of operating space and avoiding partial short circuit

Active Publication Date: 2018-07-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are huge technical difficulties in how to detect the changes of pressure and temperature on the transport properties of materials in real time. The main reason is that the relevant experimental techniques for in-situ testing under high temperature and high pressure are very complicated. Technological Breakthrough of Anvil Device Improvement
[0003] So far, the pressure generation and calibration technology under extreme conditions has been very mature, but due to high-temperature oxidation of the diamond anvil, high-temperature damage to the diamond anvil press, etc., the temperature range of the experiment is limited, resulting in the sample in the DAC. The heating problem has not been well resolved
However, the above three methods have their own defects that limit their use: the first method uses strong laser pulses to heat the sample, and the introduction of heat-insulating and pressure-transmitting media restricts part of the electrical and heat transport. Measurement of transport properties
In addition, because this method uses black body radiation to measure temperature, it not only has high requirements for experimental equipment, but also has a large temperature measurement error. The temperature measurement error of this method can reach about 50K above 1500K, and the temperature measurement error is even greater below 1500K.
In the second and third methods, the deformation caused by the high temperature of the press will cause damage to the press, the pressure disc spring will soften at high temperature, resulting in pressure loss, and the diamond anvil exposed to the air will face the problem of oxidation , thus limiting the temperature range of the experiment
[0004] In order to solve the damage to the press and the loss of pressure caused by the high temperature environment, the applicant's patent "Internal Cooling Diamond Counter Anvil Press" (Patent No.: 201510036364.X) discloses a diamond counter anvil press with built-in water cooling. During the high-temperature experiment, the press body can be guaranteed to be at room temperature, which basically solves the problems of high-temperature damage and pressure loss of the press. However, the experimental temperature is still limited due to the failure to solve the problem of diamond anvil oxidation.
The inner-cooled diamond-anvil press adopts a sleeve-type design, and the arrangement and operation of electrodes and thermocouples are relatively difficult; due to the remarkable cooling effect of the press, most of the heat is consumed, so the heating wire requires higher power, reducing However, the heating space is still limited; in order to solve the problem of temperature limitation, a mica sheet is placed between the support block and the press, which limits the accuracy of leveling and alignment; the heating wire is wound on the support On the upper surface of the block or the gasket, less effective heat is transferred to the sample, and more heat is dissipated in the form of air heat conduction, heat convection, and heat radiation

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  • Device for measuring high temperature and high pressure transport properties based on diamond opposed anvils
  • Device for measuring high temperature and high pressure transport properties based on diamond opposed anvils
  • Device for measuring high temperature and high pressure transport properties based on diamond opposed anvils

Examples

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Embodiment 1

[0032] Embodiment 1 illustrates the structure of the present invention in conjunction with the accompanying drawings.

[0033] exist Figure 1~6 Among them, 1 is the upper mold of the press, 2 is the diamond anvil, 3 is the ceramic mold of the bracket end, 4 is the bracket, 5 is the shaker, 6 is the metal gasket, 7 is the shaker base, and 8 is the shaker cover , 9 is the mica sheet, 10 is the sample, 11 is the lower mold of the press, 12 is the fixing screw, 13 is the ceramic mold at the shaker end, 14 is the centering screw, 26 is the leveling screw, 15 is the test electrode, 16 is the thermoelectric Even, 27 is a groove, and 28 is a flat bottom mold hole, and 29 is a circular step, and 30 is a trapezoidal mold hole.

[0034] The upper die 1 of the press and the lower die 11 of the press are constructed into a press with a four-column structure. Two diamond anvils 2 are placed in the internal space of the upper die 1 of the press and the lower die 11 of the press, and a met...

Embodiment 2

[0039] Example 2 combined figure 1 , 2 The assembly process of the high temperature and high pressure diamond-anvil press is illustrated.

[0040] Step 1: Remove the stains on the surface of the diamond anvil 2 by conventional methods. Put the diamond anvil 2 into a mixture of acetone and alcohol and ultrasonically remove the stains on the surface for 20 minutes. After taking it out, rinse it with deionized water.

[0041] Step 2: Fix the cleaned two diamond anvils 2 on the support block 4 and the shaker 5 respectively by using a public press, and adjust the position of the diamond anvil 2 so that the center of the anvil surface of the diamond anvil 2 and the support The central holes of the block 4 and the shaking table 5 coincide, and the pressurizing screw of the public press is rotated to make the diamond anvil 2 closely bond with the supporting block 4 and the shaking table 5.

[0042] Step 3: Mix the high-temperature repair agent A and B evenly according to the mass ra...

Embodiment 3

[0048] Example 3 combined figure 1 , Figure 3-6 Explain the winding method of the heating wire and the installation of the ceramic mold.

[0049]Step 1: According to the experimental requirements, determine the ceramic mold 3 at the bracket end and the ceramic mold 13 at the shaker end to select a flat-bottomed mold or a trapezoidal mold.

[0050] Step 2: Select a flat-bottomed mold, and cross-wind the upper and lower surfaces of the heating wire. During the winding process, pay attention to ensure that the heating wire is embedded in the groove of the mold to prevent the exposed part of the heating wire from contacting with the support block or shaking table during the experiment. Trapezoidal mould, wrap the heating wire radially inside and outside sequentially. During the winding process, care should be taken to ensure that the heating wire can be covered by the edge of the ladder, and also prevent the exposed part of the heating wire from contacting with the support block...

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Abstract

The invention discloses a device for measuring high temperature and high pressure transport properties based on diamond opposed anvils, and belongs to the technical field of physical quantity in-situmeasuring device under extreme conditions. The device comprises a press machine upper die (1), a press machine lower die (11), and diamond anvil cells (2); a metal gasket (6) is clamped between the two diamond anvil cells, and two diamond anvil cells are fixed on a support block (4) and a rocking bed (5) respectively; a rocking bed base (7) is placed at the bottom of the rocking bed, and a rockingbed cover (8) is placed at the upper part of the rocking bed; mica pieces (9) are placed between the support block and a press machine, and between the rocking bed base and the press machine respectively; a prepared ceramic die (3) is fixed in a step trough of the support block, and a ceramic die (13) sleeves the rocking bed. A sample (10) is guaranteed to be in a high temperature and high pressure environment, on the basis of easy operation and overcoming of the damage of high temperature on the press machine and the loss of pressure due to high temperature, the high temperature and high pressure transport properties of the sample are measured, and favorable conditions are provided for in-situ measurement of multiple physical quantities under the extreme conditions.

Description

technical field [0001] The invention belongs to the technical field of in-situ measuring devices for physical quantities under extreme conditions, and in particular relates to a device for measuring high-temperature and high-voltage electrical transport and heat transport properties in a diamond anvil. Background technique [0002] Diamond Anvil Cell (DAC for short) is currently the only scientific device that can generate a static pressure of one million atmospheres, and is the most important scientific instrument in the field of high-pressure science and technology research. Using two specially-made diamond anvils, the known pressure limit has exceeded 1TPa. If combined with high-temperature technology, the temperature and pressure environment simulated in the laboratory can completely study the physical and chemical properties of related substances in the earth's interior, which is the key to explain seismic wave data. , An important way to understand the internal structu...

Claims

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Application Information

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IPC IPC(8): G01N27/04G01N25/20
CPCG01N25/20G01N27/04
Inventor 高春晓岳冬辉韩永昊冀婷婷彭刚刘才龙
Owner JILIN UNIV
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