A large cavity press deformation pressure calibration method

Abstract

The present application belongs to the technical field of large cavity press, and particularly relates to a large cavity press deformation pressure calibration method. The present application provides a large cavity press deformation pressure calibration method, which comprises the following steps: depositing a conductive layer on the surface of the beveled plug to obtain a conductive beveled plug; and assembling the conductive beveled plug, molybdenum column, magnesium oxide tube, magnesium oxide sample bin, magnesium oxide octahedron and pressure calibration substance, and then placing them in the large cavity press to perform large cavity press pressure correction experiment. The present application innovatively improves the internal assembly of the large cavity press, deposits a conductive layer on the surface of the beveled insulating plug to obtain a good conductive shearing assembly, and further realizes the large cavity press deformation pressure calibration.

Description

Technical Field

[0001] This invention belongs to the field of large-cavity press technology, specifically relating to a method for calibrating the deformation pressure of a large-cavity press. Background Technology

[0002] Researchers have improved the internal assembly design of a press by introducing 45-degree angled alumina, enabling deformation stress loading in a large-cavity press. Using this technology, researchers have investigated the structural transformation mechanisms of materials such as olivine under high temperature and pressure, further revealing insights into issues in Earth sciences such as subducting plates, asthenospheric interactions, and the formation of the marine lithosphere.

[0003] Pressure calibration of large-cavity presses typically employs an indirect calibration method. This involves placing highly conductive copper or molybdenum pillars above and below the calibration material (Bi, ZnTe, ZnS, GaAs, etc.), and then measuring the resistance of the calibration material as a function of pressure using an external resistance meter. Based on the relationship between the phase transition pressure point and the abrupt change in resistance of the calibration material, the relationship between the pressure within the sample chamber and the magnitude of the hydraulic load in the large-cavity press is determined. However, the alumina-modified assembly used to generate deformation pressure loading has extremely poor conductivity, making pressure correction experiments difficult. Therefore, high-pressure deformation experiments are usually conducted by referencing hydrostatic pressure calibration data. This estimation method undoubtedly introduces errors in determining the true pressure value of the sample chamber. Therefore, the design and development of an assembly capable of accurately calibrating high-pressure deformation is an urgent need. Summary of the Invention

[0004] In view of this, the present invention provides a method for calibrating the deformation pressure of a large-cavity press. The method provided by the present invention can improve the accuracy of pressure calibration for assemblies formed by beveled plugs.

[0005] To solve the above-mentioned technical problems, the present invention provides a method for calibrating the deformation pressure of a large-cavity press, comprising the following steps:

[0006] A conductive layer is deposited on the surface of the beveled plug to obtain a conductive beveled plug;

[0007] The conductive beveled plug, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, magnesium oxide octahedron and standard pressure material were assembled and placed in a large-cavity press for a large-cavity press pressure correction experiment.

[0008] Preferably, the beveled plug is a diamond beveled plug or an alumina beveled plug.

[0009] Preferably, the angle of the beveled surface of the beveled plug is 45°.

[0010] Preferably, the conductive layer is made of copper or molybdenum.

[0011] Preferably, the thickness of the conductive layer is 1.62 to 1.65 μm.

[0012] Preferably, the standard pressure material is zinc telluride.

[0013] Preferably, the assembly process further includes: grinding and annealing zinc telluride.

[0014] Preferably, the annealing temperature is 98–102°C and the annealing time is 1.8–2.2 h.

[0015] Preferably, the heating rate to the annealing temperature is 4–6 °C / min.

[0016] The present invention also provides an angled plug, the angled plug being made of diamond and having an angle of 45° on its beveled surface.

[0017] This invention provides a method for calibrating the deformation pressure of a large-cavity press, comprising the following steps: depositing a conductive layer on the surface of an angled plug to obtain a conductive angled plug; assembling the conductive angled plug, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, magnesium oxide octahedron, and pressure calibration material, and then placing them in a large-cavity press for pressure correction experiments. This invention is the first to combine chemical vapor deposition with semiconductor plugs, depositing a layer of conductive copper or molybdenum on the surface of the alumina plug, which not only retains the angled features but also significantly improves the conductivity of the assembly, thereby enabling pressure calibration of the assembly formed by the angled plug. Attached Figure Description

[0018] Figure 1 The diagram shows the structure of the assembled assembly, where 5 is the molybdenum column electrode, 6 is the magnesium oxide sample chamber, 7 is the conductive beveled plug, 8 is the magnesium oxide octahedron, 9 is the standard pressure material, and 10 is the magnesium oxide tube.

[0019] Figure 2 This is a graph showing the resistance of the ZnTe standard pressure material as a function of oil pressure in Example 1;

[0020] Figure 3 The graph shows the actual pressure and the applied oil pressure inside the large-cavity press in Example 1.

[0021] Figure 4 The images show the actual magnesium oxide octahedron, magnesium oxide cylinder, molybdenum column electrode, magnesium oxide sample chamber, and metal-plated angled diamond plug used in Example 1.

[0022] Figure 5 Here is a scanning electron microscope image of the copper-plated beveled diamond plug from Example 1;

[0023] Figure 6 Here is a scanning electron microscope image of the silicon wafer with the metallized layer in Example 1;

[0024] Figure 7This is a graph showing the resistance of the ZnTe standard pressure material as a function of oil pressure in Example 2;

[0025] Figure 8 This is a graph showing the relationship between the hydraulic pressure and the chamber pressure when the large-cavity press is applied in Example 2. Detailed Implementation

[0026] This invention provides a method for calibrating the deformation pressure of a large-cavity press, comprising the following steps:

[0027] A conductive layer is deposited on the surface of the beveled plug to obtain a conductive beveled plug;

[0028] The conductive beveled plug, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, magnesium oxide octahedron and standard pressure material were assembled and placed in a large-cavity press for a large-cavity press pressure correction experiment.

[0029] This invention deposits a conductive layer on the surface of a beveled end cap to obtain a conductive beveled end cap. In this invention, the beveled end cap is a diamond beveled end cap or an alumina beveled end cap, more preferably an alumina beveled end cap. In this invention, the angle of the beveled surface of the beveled end cap is preferably 45°. This invention preferably obtains the beveled end cap by cutting a cylindrical end cap. In this invention, the diameter of the cylindrical end cap is preferably 0.8–2.5 mm, and the height is preferably 1–1.5 mm. This invention preferably cuts from the middle of the cylinder.

[0030] In this invention, the conductive layer is preferably made of copper or molybdenum, more preferably copper. The thickness of the conductive layer is preferably 1.62–1.65 μm, more preferably 1.632–1.647 μm. The deposition method preferably includes chemical vapor deposition or magnetron sputtering, more preferably magnetron sputtering; this invention does not specifically limit the magnetron sputtering method, and conventional methods in the art can be used.

[0031] This invention deposits a conductive metal layer on the surface of an angled insulating plug, which not only retains its angled characteristics but also significantly improves the conductivity of the assembly. This invention calibrates not only the deformation pressure loading of an alumina angled plug but also that of an insulating diamond angled plug. This method is not limited to alumina or diamond but can also be applied to other insulating angled plug systems, thus laying the foundation for accurately calibrating the internal pressure of high-voltage deformation assemblies.

[0032] After obtaining the conductive beveled plug, this invention assembles the conductive beveled plug, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, magnesium oxide octahedron, and standard pressure material, and places them in a large-cavity press for a large-cavity press pressure correction experiment. In this invention, the molybdenum column serves as the electrode. In this invention, the standard pressure material is preferably zinc telluride, but not limited to zinc telluride. In this invention, the assembly process preferably includes grinding and then annealing the zinc telluride. In this invention, the grinding is preferably wet grinding, and the dispersant used for wet grinding is preferably anhydrous ethanol. This invention reduces the particle size of zinc telluride through grinding.

[0033] In this invention, the annealing temperature is preferably 98–102°C, more preferably 100°C; the heating rate to the annealing temperature is preferably 4–6°C / min, more preferably 5°C / min; and the annealing time is preferably 1.8–2.2 h, more preferably 2 h. In this invention, the annealing is preferably performed under vacuum conditions. This invention does not impose any particular limitation on the vacuum degree of the vacuum conditions, as long as the vacuum condition can be achieved.

[0034] The present invention has no special requirements for the assembly, and conventional methods in the art can be used. Figure 1 The diagram shows the structure of the assembled assembly, where 5 is the molybdenum column electrode, 6 is the magnesium oxide sample chamber, 7 is the conductive beveled plug, 8 is the magnesium oxide octahedron, 9 is the standard pressure material, and 10 is the magnesium oxide tube.

[0035] The present invention does not have any special requirements for the method of pressure correction experiment of the large cavity press; conventional methods in the field can be used.

[0036] In this invention, the pressure ramp rate in the correction experiment is preferably 2-5 min / bar, more preferably 3-4 min / bar. During the correction experiment, this invention continuously records the change in sample resistance and plots the resistance curve of the ZnTe standard pressure material as a function of oil pressure. The internal pressure of the chamber is calibrated by the abrupt change in resistance caused by the phase transition of ZnTe under high pressure, thus establishing and determining the relationship between the oil pressure applied by the large-chamber press and the chamber pressure.

[0037] This invention also provides an angled plug, the angled plug being made of diamond, and the angle of the angled surface of the angled plug being 45°. Preferably, the angled diamond plug is obtained by cutting a cylindrical diamond plug. In this invention, the diameter of the cylindrical diamond plug is preferably 0.8–2.5 mm, and the height is preferably 1–1.5 mm. Preferably, the angled diamond plug is obtained by cutting from the middle of the cylindrical diamond plug.

[0038] To further illustrate the present invention, the technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0039] Example 1

[0040] 5 mg of zinc telluride was placed in an agate grinding medium, anhydrous ethanol was added and the mixture was manually ground for 2.5 h. The ground sample was then placed in a vacuum muffle furnace and heated to 100 °C at a heating rate of 5 °C / min under vacuum conditions. After holding the temperature for 2 h, the sample was cooled to room temperature with the furnace.

[0041] A diamond cylinder with a height of 1 mm and a diameter of 0.8 mm was cut in half from the middle using a laser cutting machine with an excitation wavelength of 532 nm. The cutting angle was 45° to the cross-section of the cylinder to obtain an angled diamond plug.

[0042] A copper layer with a thickness of 1.63 μm was deposited by magnetron sputtering on the surface of an angled diamond plug to obtain a metal-plated angled diamond plug; the thickness of the copper layer was controlled by sputtering using a silicon wafer as a substrate during the magnetron sputtering process.

[0043] The annealed zinc telluride, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, metal-plated beveled diamond plug, and magnesium oxide octahedron were arranged according to... Figure 1 The assembled structure was placed in a large-cavity press, and a pressure correction experiment was conducted by increasing the pressure at a rate of 3 min / bar. During the correction experiment, the change in sample resistance was recorded continuously, and a curve showing the change in ZnTe pressure gauge versus oil pressure was plotted. Figure 2 As shown. Based on the steep drop in resistance, the phase transition pressure points of ZnTe at standard pressure were determined to be 6.6 GPa (zinc blende), 8.9 GPa (cina bar), and 12.9 GPa (cm cm). The relationship between the hydraulic pressure and the pressure of the large-cavity press was plotted using the phase transition pressure points of ZnTe under high pressure, as shown below. Figure 3 As shown, the red dotted line graph represents the test results using the angled diamond plug with a metal coating from Example 1 as the plug, and the black dotted line graph represents the test results using a molybdenum column as the plug. The experimental pressure calibration used an HXR type tungsten carbide two-stage anvil, but the calibration pressure is not limited to the HXR type. Figure 3 As shown, comparing the pressure calibration curves of shear and non-shear pressures, it was found that under the same oil pressure, the pressure boosting efficiency of the shear assembly was significantly improved by nearly 40 Bar. Therefore, accurate pressure calibration of the high-pressure deformation assembly is necessary for conducting the corresponding experiments, and it is feasible to accurately calibrate the deformation assembly pressure using the method provided by this invention.

[0044] Figure 4 The image shows the actual components used in Example 1: a magnesium oxide octahedron, a magnesium oxide cylinder, a molybdenum column electrode, a magnesium oxide sample chamber, and a metal-plated angled diamond plug.

[0045] Figure 5 Scanning electron microscope image of a beveled diamond plug with a metal coating.

[0046] Figure 6 This is a SEM image of a copper layer deposited on a silicon wafer. Figure 6 The thickness of the deposited copper layer can be observed, thus allowing determination of the thickness of the copper layer deposited on the surface of the angled diamond plug.

[0047] Example 2

[0048] Pressure calibration was performed according to the method in Example 1, except that the diamond column was replaced with an alumina column.

[0049] The annealed zinc telluride, molybdenum column, magnesium oxide tube, magnesium oxide sample chamber, conductive angled alumina plug, and magnesium oxide octahedron were arranged according to... Figure 1 The assembled structure was placed in a large-cavity press, and a pressure correction experiment was conducted by increasing the pressure at a rate of 3 min / bar. During the pressure correction experiment, the change in sample resistance was recorded continuously, and a curve showing the change in ZnTe pressure gauge versus oil pressure was plotted. Figure 7 As shown. By Figure 7 The ZnTe phase transition pressure points can be determined to be 6.6 GPa (zinc blende), 8.9 GPa (cinabar), and 12.9 GPa (cmcm), corresponding to the abrupt change in resistance. The abrupt change in resistance caused by the ZnTe phase transition under high pressure is used to calibrate the internal pressure of the chamber and establish and determine the relationship between the oil pressure and the chamber pressure in a large-chamber compressor. Figure 8 As shown. Figure 8 The blue curve represents the precise pressure calibration curve based on the shear pressure generated by the alumina angled plug, while the black curve represents the pressure calibration curve based on the molybdenum column. Comparison reveals a significant difference between the non-shear pressure calibration curve and the shear pressure calibration curve, highlighting the necessity of calibrating the shear pressure curve.

[0050] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for calibrating the deformation pressure of a large-cavity press, comprising the following steps: A conductive beveled end is obtained by depositing a conductive layer on the surface of the beveled end; the beveled end is a diamond beveled end or an alumina beveled end, and the conductive layer is made of copper or molybdenum. A conductive beveled plug, a molybdenum column electrode, a magnesium oxide tube, a magnesium oxide sample chamber, a magnesium oxide octahedron, and a standard pressure material are assembled to obtain a shear assembly with good conductivity. The assembly is then placed in a large-cavity press for pressure correction experiments. The internal pressure of the cavity is calibrated by the sudden change in resistance caused by the phase transition of the standard pressure material under high pressure, and the relationship between the oil pressure applied to the large-cavity press and the cavity pressure is established and determined.

2. The method according to claim 1, characterized in that, The angle of the beveled end cap is 45°.

3. The method according to claim 1, characterized in that, The thickness of the conductive layer is 1.62~1.65μm.

4. The method according to claim 1, characterized in that, The standard pressure material is zinc telluride.

5. The method according to claim 4, characterized in that, The process before assembly includes grinding and annealing zinc telluride.

6. The method according to claim 5, characterized in that, The annealing temperature is 98~102℃, and the annealing time is 1.8~2.2h.

7. The method according to claim 6, characterized in that, The heating rate to the annealing temperature is 4~6℃ / min.

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