High-pressure synthesis device and working method thereof

Abstract

The invention discloses a high-pressure synthesis device and a working method thereof, and relates to the technical field of high-pressure devices, the high-pressure synthesis device comprises two diamond anvils, and the two diamond anvils are symmetrically arranged up and down; the sample chamber is arranged between the two diamond anvils, and a sample is placed in the sample chamber; the temperature measuring device is arranged on the diamond anvil and is used for measuring the temperature of the diamond anvil; manganese-copper alloy is attached to the end face of the end, close to the sample chamber, of the diamond anvil and externally connected with a voltmeter and an ampere meter through electrodes, and the intensity of pressure applied by the diamond anvil can be indirectly measured. The high-pressure synthesis device is matched with the working method of the high-pressure synthesis device, the pressure intensity can be measured in real time, and interference of temperature on a measurement result can be removed.

Description

Technical Field

[0001] The present invention relates to the technical field of high-pressure devices, and in particular to a high-pressure synthesis device and a working method thereof. Background Art

[0002] The high-pressure synthesis device is a device that can generate and maintain extremely high pressure under laboratory conditions. It includes a pair of diamond anvils and a metal gasket. When working, the sample and the pressure-measuring ruby ​​are placed in the metal gasket of the high-pressure synthesis device at the same time, and the anvil is tightened to realize the high-pressure experiment. The pressure needs to be measured during the experiment. The existing method of measuring pressure generally uses the method of detecting the change of ruby ​​fluorescence to obtain the pressure, and it is impossible to measure the pressure in real time. However, the high temperature generated by the laser will affect the temperature of the experimental device. The change in temperature will affect the fluorescence of the ruby, which will have a certain impact on the result of measuring pressure and reduce the accuracy of the measurement result. Summary of the invention

[0003] The purpose of the present invention is to provide a high-pressure synthesis device and a working method thereof to solve the problems existing in the above-mentioned prior art, and to be able to measure the pressure in real time and to remove the interference of temperature on the measurement result.

[0004] To achieve the above object, the present invention provides the following solutions:

[0005] The present invention provides a high pressure synthesis device, comprising:

[0006] Diamond anvils, two of which are symmetrically arranged up and down, and driven by a known pressurizing device to pressurize the sample;

[0007] A sample chamber, disposed between the two diamond anvils, and used for placing a sample therein;

[0008] A temperature measuring device, disposed on the diamond anvil, for measuring the temperature at the diamond anvil;

[0009] The manganese-copper alloy is attached to the end surface of the diamond anvil close to one end of the sample chamber, and is externally connected to a voltmeter and an ammeter through electrodes, so as to indirectly measure the pressure applied by the diamond anvil.

[0010] Preferably, the longitudinal section of the diamond anvil is a trapezoidal structure, and the dimension of the end face of the diamond anvil close to the sample chamber is smaller than the dimension of the end face away from the sample chamber.

[0011] Preferably, the sample chamber includes a sealing gasket, the sealing gasket is provided with a vertical through hole, and the aperture size of the vertical through hole is smaller than the width size of the end face of the diamond anvil close to one end of the sample chamber, and one end of the diamond anvil is pressed onto one end of the vertical through hole.

[0012] Preferably, the vertical through hole is filled with aluminum oxide powder, and a sample hole is provided after the vertical through hole is filled with aluminum oxide powder, and the sample hole is used for placing a sample.

[0013] Preferably, the surface of the sealing gasket is coated with an adhesive layer.

[0014] Preferably, the temperature measuring device is a thermocouple.

[0015] The present invention also provides a working method of a high pressure synthesis device, comprising the steps of:

[0016] Step 1: Install two diamond anvils and level them;

[0017] Step 2: Paste a thermocouple on the side edge of the diamond anvil to measure temperature changes in real time;

[0018] Step 3: pre-press the gasket and punch a hole, put the gasket between two diamond anvils, and press the end of the diamond anvil on the vertical through hole of the gasket, release the pressure after pressing for a set distance, apply a layer of adhesive on the surface of the gasket, press aluminum oxide powder into the vertical through hole after the adhesive layer is dried, and punch a sample hole after compaction;

[0019] Step 4: a sheet of manganese-copper alloy is placed on the end surface of the diamond anvil close to one end of the sample chamber, and the manganese-copper alloy is connected to four electrodes using four gold wires, two of which are connected to a voltmeter, and the other two electrodes are connected to an ammeter;

[0020] Step five: Start the diamond anvil pressurization, during which the temperature value and pressure magnitude are measured in real time.

[0021] Preferably, the inner diameter of the vertical through hole is 150 μm.

[0022] Preferably, the inner diameter of the sample hole is 100 μm.

[0023] Preferably, the resistivity of the manganese-copper alloy is ρ=ρ0(1+P / k), ρ0 is the resistivity when the pressure is zero, P is the pressure, k is the slope relationship between the pressure and the normalized resistance of the manganese-copper alloy, k=23.4GPa; the resistivity ρ of the manganese-copper alloy is determined according to the numerical changes of the voltmeter and the ammeter, and then the applied pressure can be measured by substituting it into the above formula; when the temperature changes during the experiment, based on ρ0=ρ0'+aT, after removing the influence of temperature on the resistivity, the applied pressure is measured by substituting it into the relationship between resistivity and pressure, wherein ρ0' is the resistivity of the manganese-copper alloy at 0°C, T is the temperature value, and a is the temperature coefficient of resistivity. The present invention uses Mn-14at.%Cu, "at%" is the "atomic percentage" unit (at is the abbreviation of atom), which is used to describe the atomic content (percentage) of various elements in a certain inorganic substance, that is, manganese accounts for 14% in the alloy; a=1.87×10-9 / ℃.

[0024] Compared with the prior art, the present invention has achieved the following technical effects:

[0025] The present invention arranges a manganese-copper alloy between diamond anvils, and measures the change in the resistivity of the manganese-copper alloy during the pressure application process, and then according to the relationship between the resistivity and the pressure, the pressure during the pressure application process can be measured in real time; at the same time, a temperature measuring device can measure the temperature at the diamond anvil in real time, and according to the relationship between the temperature and the resistivity of the manganese-copper alloy, after removing the interference of temperature, the magnitude of the applied pressure can be accurately measured without being affected by the temperature. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0027] Figure 1 It is a side view of the high pressure synthesis device of the present invention;

[0028] Figure 2 This is a schematic diagram of the interior of the high pressure synthesis device of the present invention.

[0029] In the figure: 1-diamond anvil, 2-thermocouple, 3-manganese-copper alloy, 4-electrode, 5-adhesive layer, 6-aluminum oxide powder, 7-sample, 8-gasket. DETAILED DESCRIPTION

[0030] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0031] The purpose of the present invention is to provide a high-pressure synthesis device and a working method thereof to solve the problems existing in the above-mentioned prior art, and to be able to measure the pressure in real time and to remove the interference of temperature on the measurement result.

[0032] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0033] refer to Figure 1 and Figure 2As shown, the present invention provides a high-pressure synthesis device, including diamond anvils 1, two diamond anvils 1 are symmetrically arranged on a pressure mechanism, and the pressure mechanism is a known structure, so it is not described in detail; the diamond anvils 1 are used to pressurize, and the diamond has high thermal conductivity and small temperature influence. At the same time, diamond has excellent pressure-induced phase change characteristics, has a wide pressure measurement range, and can withstand pressures up to hundreds of GPa, so that the pressure material does not need to be replaced during the experiment in most cases. The sample chamber is arranged between the two diamond anvils 1, and the sample 7 is placed therein; the temperature measuring device is arranged on the diamond anvil 1, and is used to measure the temperature at the diamond anvil 1. The temperature measuring device of this embodiment adopts a thermocouple 2, which can measure and display the temperature value; the manganese-copper alloy 3 is attached to the end surface of the diamond anvil 1 near one end of the sample chamber. When the pressure mechanism drives the diamond anvil 1, the manganese-copper alloy 3 is compressed, and its resistivity will change. The manganese-copper alloy 3 is externally connected to a voltmeter and an ammeter through an electrode 4. According to the changes in the values ​​of voltage and current, the pressure applied by the diamond anvil 1 can be indirectly measured.

[0034] In a preferred embodiment, the longitudinal section of the diamond anvil 1 is a trapezoidal structure, and the end face size of the diamond anvil 1 close to the sample chamber is smaller than the end face size away from the sample chamber. The sample chamber includes a seal 8, which is provided with a vertical through hole, and the aperture size of the vertical through hole is smaller than the width size of the end face of the diamond anvil 1 close to the sample chamber. One end of the diamond anvil 1 is pressed into one end of the vertical through hole. During the pressing process, the vertical through hole is expanded so that the side wall of the pressed area matches the end side of the diamond anvil 1. The surface of the seal 8 is coated with an adhesive layer 5, and the adhesive layer 5 adopts AB glue, which is a two-component epoxy resin adhesive, usually composed of component A (resin) and component B (hardener or curing agent). When in use, the two components need to be mixed in a certain proportion, and then applied to the surface of the object to be bonded. After a period of curing, a strong bonding effect is formed; after pressing to a set depth, the pressure is released, and then alumina powder 6 is filled in the vertical through hole. After the vertical through hole is filled with alumina powder 6, a sample hole is penetrated, and the sample hole is used to place the sample 7.

[0035] The present invention also provides a working method of a high pressure synthesis device, comprising the steps of:

[0036] Step 1: Install two diamond anvils 1 so that they are aligned and close to each other, and then observe the diffraction fringes on the upper end surface of the diamond anvil 1. If the number of fringes is within three, the leveling is completed.

[0037] Step 2: Paste a thermocouple 2 on the side edge of the diamond anvil 1 to measure the temperature change in real time;

[0038] Step three, pre-press the gasket 8 and punch a hole, keep the end face of the diamond anvil 1 clean, pay attention to the pressure balance during the pressing process to prevent excessive pressure on one side of the diamond anvil 1, and release the pressure after the set depth is pressed. At this time, the end of the diamond anvil 1 will expand the vertical through hole close to the opening, and the expansion structure matches the end face structure of the diamond anvil 1, and then release the pressure. The pressure should not be released too quickly, and the pressure is released in several stages until it reaches normal pressure. Apply a thin layer of AB glue on the gasket 8. The inner diameter of the vertical through hole of the gasket 8 is 150μm. No glue is applied in the hole. After the AB glue is dry, press alumina powder 6 in the vertical through hole. After compaction, punch a sample hole. The inner diameter of the sample hole is 100μm.

[0039] Step 4: a manganese-copper alloy 3 is placed on the end surface of the diamond anvil 1 close to one end of the sample chamber, and the manganese-copper alloy 3 is connected to four electrodes 4 using four gold wires, two of which are connected to a voltmeter, and the other two electrodes 4 are connected to an ammeter;

[0040] Step 5, start the diamond anvil 1 to apply pressure, during which the temperature value and pressure are measured in real time; the thermocouple 2 is used to measure the temperature, and the entire device is placed in a copper heating device to control the temperature of the device of the present invention, and the sample 7 is placed in the sample hole between the two diamonds. By adjusting the temperature and pressure, the properties of the sample 7 at different temperatures and pressures can be explored.

[0041] The resistivity of manganese-copper alloy 3 is ρ=ρ0(1+P / k), where ρ0 is the resistivity when the pressure is zero, P is the pressure, k is the slope relationship between the pressure and the resistance of manganese-copper alloy 3, and k=23.4GPa; the resistivity ρ of manganese-copper alloy 3 is determined according to the numerical changes of the voltmeter and the ammeter, and then the applied pressure can be measured by substituting it into the above formula; when the temperature changes during the experiment, based on ρ0=ρ0'+aT, after removing the influence of temperature on the resistivity, the applied pressure is measured by substituting it into the relationship between resistivity and pressure, where ρ0' is the resistivity of manganese-copper alloy 3 at 0°C, T is the temperature value, and a is the temperature coefficient of resistivity. The present invention uses Mn-14at.%Cu, a=1.87×10 -9 / ℃.

[0042] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A high pressure synthesis device, characterized in that: include: Diamond anvils, two diamond anvils are symmetrically arranged up and down; A sample chamber, disposed between the two diamond anvils, and used for placing a sample therein; A temperature measuring device, disposed on the diamond anvil, for measuring the temperature at the diamond anvil; The manganese-copper alloy is attached to the end surface of the diamond anvil close to one end of the sample chamber, and is externally connected to a voltmeter and an ammeter through electrodes, so as to indirectly measure the pressure applied by the diamond anvil.

2. The high pressure synthesis device according to claim 1, characterized in that: The longitudinal section of the diamond anvil is a trapezoidal structure, and the size of the end surface of the diamond anvil close to the sample chamber is smaller than the size of the end surface far from the sample chamber.

3. The high pressure synthesis device according to claim 1, characterized in that: The sample chamber comprises a sealing gasket, which is provided with a vertical through hole, and the aperture size of the vertical through hole is smaller than the width size of the end face of the diamond anvil close to one end of the sample chamber, and one end of the diamond anvil is pressed on one end of the vertical through hole.

4. The high pressure synthesis device according to claim 3, characterized in that: The vertical through hole is filled with aluminum oxide powder. After the vertical through hole is filled with aluminum oxide powder, a sample hole is drilled therein, and the sample hole is used for placing a sample.

5. The high pressure synthesis device according to claim 3, characterized in that: The surface of the sealing gasket is coated with an adhesive layer.

6. The high pressure synthesis device according to claim 1, characterized in that: The temperature measuring device is a thermocouple.

7. A method for operating a high pressure synthesis device, characterized in that: Includes steps: Step 1: Install two diamond anvils and level them; Step 2: Paste a thermocouple on the side edge of the diamond anvil to measure temperature changes in real time; Step 3: pre-press the gasket and punch a hole, put the gasket between two diamond anvils, and press the end of the diamond anvil on the vertical through hole of the gasket, release the pressure after pressing for a set distance, apply a layer of adhesive on the surface of the gasket, press aluminum oxide powder into the vertical through hole after the adhesive layer is dried, and punch a sample hole after compaction; Step 4: Place a manganese-copper alloy on the end surface of the diamond anvil close to one end of the sample chamber, and connect the manganese-copper alloy to four electrodes using four gold wires, two of which are connected to a voltmeter, and the other two electrodes are connected to an ammeter; Step five: Start the diamond anvil pressurization, during which the temperature value and pressure magnitude are measured in real time.

8. The operating method of the high pressure synthesis device according to claim 7, characterized in that: The inner diameter of the vertical through hole is 150 μm.

9. The operating method of the high pressure synthesis device according to claim 7, characterized in that: The inner diameter of the sample hole is 100 μm.

10. The operating method of the high pressure synthesis device according to claim 7, characterized in that: The resistivity of the manganese-copper alloy is ρ=ρ0(1+P / k), where ρ0 is the resistivity when the pressure is zero, P is the pressure, and k is the slope relationship between the pressure and the normalized resistance of the manganese-copper alloy, k=23.4 GPa; the resistivity ρ of the manganese-copper alloy is determined according to the numerical changes of the voltmeter and the ammeter, and then the magnitude of the applied pressure can be measured by substituting it into the above formula; When the temperature changes during the experiment, based on ρ0=ρ0' + aT, after removing the influence of temperature on resistivity, the applied pressure is measured by substituting the relation between resistivity and pressure, where ρ0' is the resistivity of manganese-copper alloy at 0°C, T is the temperature value, and a is the temperature coefficient of resistivity, a=1.87×10 -9 / ℃.

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