CN114323405A - Cadmium phosphide (Cd)3P2) Be applied to big cavity press high pressure means intracavity pressure and mark - Google Patents
Cadmium phosphide (Cd)3P2) Be applied to big cavity press high pressure means intracavity pressure and mark Download PDFInfo
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Abstract
The invention relates to the treatment of cadmium phosphide (Cd)3P2) Is applied to the calibration of the pressure in the cavity of a high-pressure device of a large-cavity press, and particularly relates to a method for newly adding cadmium phosphide (Cd) on the basis of traditional standard pressure substances such as bismuth (Bi), thallium (Tl), barium (Ba) and the like3P2) The phase-change pressure point is used as a pressure marking substance and is used for marking the pressure in the cavity of the high-pressure device of the large-cavity press under the high-pressure condition, and the phase-change pressure point belongs to the technical field of high-pressure scientific experiments. The invention uses a domestic hinge type cubic apparatus large cavity press as a high-pressure generating device to firstly convert cadmium phosphide (Cd)3P2) As a pressure calibration material of the high-pressure device of the large-cavity press, the result further calibrates a calibration curve, and is beneficial to improving the accuracy of the cavity pressure and oil pressure loading curve of the high-pressure device of the large-cavity press. The method provided by the invention has the characteristics of low cost, environmental friendliness, clear electrical signals, simplicity in operation, practicability and the like.
Description
Technical Field
The invention relates to the first time of Cd precipitation3P2The method is applied to pressure calibration of the high-pressure device of the large-cavity press. In particular to a new Cd added on the basis of the traditional standard pressure substances of bismuth (Bi), thallium (Tl), barium (Ba) and the like3P2The material is used as a standard pressure material, and the resistivity mutation is utilized to calibrate the cavity pressure when the material is subjected to phase change under high pressure, and the material belongs to the technical field of high-pressure experiments.
Background
As a fundamental thermodynamic parameter determining the state of existence and the structural change of a substance, the pressure (P) has a specific capacity to induce changes in the structure and properties of the substance, different from the temperature (T) and chemical composition. In 1935, high pressure technology was gradually emerging in the human vision with the Bridgman press. In the last hundred years, the rapid development of high-pressure experimental technology is the basis for deepening and expanding the application of high-pressure science and technology, and becomes a main method for processing materials under high-pressure extreme physical conditions. The high-pressure device of the multi-surface top large-cavity press is mainly divided into a pull rod type, a slide block type and a hinge type. The hinged cubic apparatus large cavity press is a high-pressure device which is independently researched and developed in China, and has the advantages of compact structure, low operation cost, good self-alignment property, easy maintenance, large sample size, relatively uniform pressure and temperature field and controllable pressure and temperature field. Because of the technical advantages, the domestic hinge type cubic press has been widely applied to scientific research in scientific research and production fields at home and abroad, and synthesis of superhard materials in other related fields, and has made a series of breakthrough progresses, becoming one of the mainstream high-pressure devices for scientific research and production.
In a high-voltage environment, the physical properties such as the structure, electrical properties, magnetic properties, and optical properties of a substance are generally changed. Therefore, in a high-pressure experiment, the pressure inside the high-pressure cavity is often calibrated by indirectly measuring the physical property change of a substance, and the commonly used pressure calibration methods include a substance phase-change pressure calibration method, a state equation pressure calibration method and a spectrum pressure calibration method. The pressure calibration is actually the pressure calibration in the high-pressure science and technology field, and aims to establish the corresponding relation between the oil pressure loading of a large-cavity press and the pressure in a cavity. This patent adopts the cubic hinge chain type press of making at home as high pressure to produce the device, to the demarcation of the one-level cavity pressure of the cubic hinge chain type press of making at home, often utilizes the phase transition point of material under the high pressure to mark. Generally, a substance with a known phase transition pressure is placed in a pressure chamber of a high-pressure device, and then an in-situ observation is performed on a certain physical property of the substance along with the change of the pressure to judge whether phase transition or other physical property changes. If the phase change occurs, the current pressure in the high-pressure cavity can be judged to be the phase change pressure value of the substance, and therefore the corresponding relation of the cavity pressure loaded along with the oil pressure is obtained. In 1952, the Bridgman reference proposed by Bridgman calibrates the pressure value of the environment where a substance is located by using the phenomenon of resistivity mutation when the substance is subjected to phase change under high-pressure extreme physical conditions, and the method is widely applied to calibration of the cavity pressure of a high-pressure device of a large-cavity press including a hexahedral-top hinge type press at normal temperature.
Disclosure of Invention
The invention aims to increase the standard pressure substance cadmium phosphide (Cd)3P2) The accuracy of a relation curve between the cavity pressure and the oil pressure loading is improved, and the cavity pressure in the high-pressure device can be calibrated more accurately. Cd was studied by F.S. Yel' kin et al in 20083P2Phase transition at high temperature and high pressure, this study showed Cd3P2The high-pressure Phase transition pressure point at normal temperature is 4.0GPa (F.S. Yel' kin, et al. "Phase transitions in Cd3P2 at high pressures and high temperatures." Journal of Alloys &Compounds 450.1-2(2008): 79-85.). Based on this study, we utilized Cd3P2The electrical characteristic that the resistivity of 4.0GPa is suddenly changed at normal temperature is applied to the pressure calibration of a high-pressure device of a large-cavity press, and the domestic chain hinge type cubic-anvil large-cavity press is used as a high-pressure generating device. In the invention, Cd is utilized for the first time3P2The primary pressure cavity pressure calibration of the domestic hinge type cubic press is carried out, and the accuracy of the corresponding relation between the cavity pressure and the oil pressure loading is further calibrated.
Cadmium phosphide (Cd) related to the invention3P2) The pressure calibration applied to the high-pressure device of the large-cavity press mainly comprises the following steps:
the first step is as follows: selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm) with high quality, wherein the mass is about 90.6 g;
the second step is that: cutting off the selected pyrophyllite by about 1/3 volumes, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
the third step: machining the cut pyrophyllite into two pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with smooth surfaces by using a lathe, namely combining the pyrophyllite blocks into cube pyrophyllite blocks with side length of 32.5 mm;
the fourth step: selecting a pyrophyllite block with a smooth surface, marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by a knife, and weighingCd in an amount of about 0.2g3P2Powder is filled into the groove;
the fifth step: cutting the bright copper sheet with good conductivity polished by abrasive paper into L shape, wherein the sharp part of the middle part is connected with Cd3P2Powder is contacted and conducted, copper sheets are fixed, then the copper sheets exceeding the pyrophyllite part are cut off, and a part of 2-3mm is reserved and is used for conducting a circuit of a hammer face after being folded;
and a sixth step: the other half of the pyrophyllite was covered and compacted by standing with a weight for 2 hours to ensure compactness of the packed powder. A four-wire method is adopted, a constant current source and a multi-channel recorder are introduced into a front top hammer, a rear top hammer, a left top hammer and a right top hammer of a press, an oil pressure signal is connected to the multi-channel recorder, and two ends of the constant current source are connected with a resistor with the resistance value of 1K omega in parallel. The boosting rate and the boosting time are set before the experiment begins, and on the premise that the constant current source current is stable after the experiment begins, the oil pressure curve is recorded, the range of voltage test is selected well, and the change of the voltage value is recorded.
The main component of the high-quality pyrophyllite solid block selected in the first step of the method is Al2Si4O10(OH)2And the final product of decomposition at high temperature is SiO2、Al2O3. The density of the selected pyrophyllite solid block is about 2.64g/cm3。
In the second step of the method, 1/3 of the pyrophyllite square block is cut off by a steel saw, so that the cut surface has no large inclination as much as possible, and the method is convenient to process.
When the pyrophyllite is machined by a lathe in the third step of the method, the flatness of the plane is ensured, and meanwhile, the height of the pyrophyllite is ensured to be 16.25 (+/-0.1) mm as far as possible, namely, the two blocks are combined to be machined into a cubic pyrophyllite block with the side length of 32.5 mm.
The purpose of scribing a groove at the center of the pyrophyllite in the fourth step of the method is to reduce the influence of the rheology generated in the process of compressing the powder on the detection of the electric signals. The depth and the length of the scratch groove and the powder taking amount are approximate range values, and the specific experiment can be flexibly implemented.
In the fifth step of the method, the copper sheet is polished to be bright, so that the oxidized copper oxide film is polished to improve the conductivity of the copper sheet. The sharp part of the L-shaped copper sheet is well attached to the powder so as to be conducted with a middle marking substance, and after the copper sheet is fixed along the diagonal direction, the connection of a circuit is ensured by using the gear of a measuring resistor of a multimeter. The top ends of the two L-shaped copper sheets are forbidden to be close to each other so as to avoid the problem of short circuit of the circuit.
In the sixth step of the method, the four-wire method is adopted to arrange the circuit, and is favorable for reducing the contact resistance, so that the electrical signals required to be acquired in the experiment can be clearer. The current value of the constant current source in the whole experiment process is stable, and the multichannel recorder records the oil pressure of the press and the voltage signal in the line in the in-situ pressure loading process.
Advantageous effects
(1) The invention firstly uses cadmium phosphide (Cd)3P2) As a new standard pressure substance, the invention adds a substance which can be used for calibrating the pressure of the high-pressure device of the large-cavity press on the basis of the traditional standard pressure substances such as bismuth (Bi), thallium (Tl), barium (Ba) and the like. The chemical property of the cadmium phosphide is stable, the resistance change is obvious during phase change, and the pressure measurement is accurate. Meanwhile, the pressure calibration material has no high toxicity like a thallium material and is extremely easy to oxidize like a barium material, and is an ideal pressure calibration material for pressure calibration of a large-cavity press.
(2) The invention leads cadmium phosphate (Cd) to3P2) The method is applied to pressure calibration of a high-pressure device of a large-cavity press, further calibrates a calibration curve, and is beneficial to improving the accuracy of a relation curve of cavity pressure and oil pressure loading.
(3) The invention is not only suitable for a six-side top hinge type press, but also can be used for pressure calibration of other large-cavity high-pressure devices with two sides, four sides, eight sides and the like, and the specific equipment has different electrical signal acquisition modes and needs specific device analysis. The invention only uses a domestic hexahedral top hinge type press as a high-pressure generating device and aims to increase the standard pressure substance cadmium phosphide (Cd)3P2) And can be used for calibrating the cavity pressure of the high-pressure equipment.
Drawings
FIG. 1: example a schematic diagram of an assembled high voltage in situ resistance measurement circuit.
FIG. 2: example two initial marking substance cadmium phosphide (Cd)3P2) XRD pattern of (a).
FIG. 3: third embodiment the voltage signal profile collected by the multichannel recorder.
FIG. 4: example three the phase change pressure points for the pressure calibration material of the high-pressure device of the large-cavity press are commonly used.
FIG. 5: EXAMPLE four novel addition of cadmium phosphide (Cd)3P2) And comparing the standard pressure curve with the traditional standard pressure curve.
Detailed Description
The first embodiment is as follows:
(1) selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm), cutting 1/3 of the selected pyrophyllite by using a steel saw, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
(2) processing the cut pyrophyllite into two pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with smooth surfaces by using a lathe, and controlling the blocks to be combined into cube pyrophyllite blocks with side length of 32.5mm, wherein the error range is within +/-0.1 mm;
(3) selecting a pyrophyllite block with a smooth surface, marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by a knife, and adding Cd with the weight of about 0.2g3P2Powder is filled into the groove; cutting the bright copper sheet with good conductivity polished by abrasive paper into L shape, wherein the sharp part of the middle part is connected with Cd3P2Powder is contacted and conducted, copper sheets are fixed, the copper sheets exceeding the pyrophyllite part are cut off, and a part of 2-3mm is reserved and is folded to be contacted with the hammer face, so that a circuit is conducted; then covering the other pyrophyllite block, and standing and compacting for 2 hours by using a weight; the constant current source and the multi-channel recorder are respectively introduced into a front anvil, a rear anvil, a left anvil and a right anvil of a cubic press by adopting a four-wire method, two ends of the constant current source are connected with a resistor with the resistance value of 1K omega in parallel, and an oil pressure signal is connected to the multi-channel recorder;
(4) setting the voltage increasing and decreasing rate to be 5-45MPa/20min before the start of the experiment, ensuring the current stability of the constant current source, and selecting the range of proper voltage test; when an experiment is started, filling liquid into six oil cylinders of the press, starting to record an oil pressure signal and a voltage signal when the oil pressure is increased to 5MPa, clicking pressure to jump and start pressure relief when the oil pressure is increased to 45MPa, and stopping recording and taking out a change curve of a card reader for analyzing the voltage signal when the oil pressure is released to 5 MPa;
(5) the file is converted into an Excel format by multichannel reading software, and then the Excel format is used for drawing by Origin, and the voltage signal, namely the sudden change of the resistance is observed. The experimental results are as follows: when the corresponding oil pressure loading is 28.2MPa, the voltage signal is obviously changed, and a curve inflection point appears, which shows that the oil pressure value corresponds to the cavity pressure of 4.0 GPa; finally, adding Bi, Tl and Cd3P2And the phase change pressure point of Ba is fitted by Origin to obtain a relation graph of oil pressure loading and cavity pressure, and a standard pressure curve is obtained.
Example two:
(1) selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm), cutting 1/3 of the selected pyrophyllite by using a steel saw, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
(2) processing the cut pyrophyllite into two pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with smooth surfaces by using a lathe, and controlling the blocks to be combined into cube pyrophyllite blocks with side length of 32.5mm, wherein the error range is within +/-0.1 mm;
(3) selecting a pyrophyllite block with a smooth surface, marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by a knife, and adding Cd with the weight of about 0.2g3P2Powder is filled into the groove; cutting the bright copper sheet with good conductivity polished by abrasive paper into L shape, wherein the sharp part of the middle part is connected with Cd3P2Powder is contacted and conducted, copper sheets are fixed, the copper sheets exceeding the pyrophyllite part are cut off, and a part of 2-3mm is reserved and is folded to be contacted with the hammer face, so that a circuit is conducted; then covering the other pyrophyllite block, and standing and compacting for 2 hours by using a weight; by adopting a four-wire method, the constant current source and the multi-channel recorder are respectively connectedThe hydraulic pressure signal is introduced into a front anvil, a rear anvil, a left anvil and a right anvil of a cubic press, a resistor with the resistance value of 1K omega is connected in parallel at two ends of a constant current source, and an oil pressure signal is connected to a multi-channel recorder;
(4) setting the voltage increasing and decreasing rate to be 5-45MPa/20min before the start of the experiment, ensuring the current stability of the constant current source, and selecting the range of proper voltage test; when an experiment is started, filling liquid into six oil cylinders of the press, starting to record an oil pressure signal and a voltage signal when the oil pressure is increased to 5MPa, clicking pressure to jump and start pressure relief when the oil pressure is increased to 45MPa, and stopping recording and taking out a change curve of a card reader for analyzing the voltage signal when the oil pressure is released to 5 MPa;
(5) the file is converted into an Excel format by multichannel reading software, and then the Excel format is used for drawing by Origin, and the voltage signal, namely the sudden change of the resistance is observed. The experimental results are as follows: when the corresponding oil pressure loading is 29.3MPa, the voltage signal changes obviously, and an inflection point appears on a voltage curve, which indicates that the oil pressure value corresponds to the cavity pressure of 4.0 GPa. Finally, adding Bi, Tl and Cd3P2And the phase change pressure point of Ba is fitted by Origin to obtain a relation graph of oil pressure loading and cavity pressure, and a standard pressure curve is obtained.
Example three:
(1) selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm), cutting 1/3 of the selected pyrophyllite by using a steel saw, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
(2) processing the cut pyrophyllite into two pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with smooth surfaces by using a lathe, and controlling the blocks to be combined into cube pyrophyllite blocks with side length of 32.5mm, wherein the error range is within +/-0.1 mm;
(3) selecting a pyrophyllite block with a smooth surface, marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by a knife, and adding Cd with the weight of about 0.2g3P2Powder is filled into the groove; cutting the bright copper sheet with good conductivity polished by abrasive paper into L shape, wherein the sharp part of the middle part is connected with Cd3P2Powder contact and conduction, fixing copper sheet, cutting off the copper sheet exceeding pyrophyllite part, and reserving 2-3mm partAfter being folded, the electric circuit is connected by contacting with the hammer surface; then covering the other pyrophyllite block, and standing and compacting for 2 hours by using a weight; the constant current source and the multi-channel recorder are respectively introduced into a front anvil, a rear anvil, a left anvil and a right anvil of a cubic press by adopting a four-wire method, two ends of the constant current source are connected with a resistor with the resistance value of 1K omega in parallel, and an oil pressure signal is connected to the multi-channel recorder;
(4) setting the voltage increasing and decreasing rate to be 5-45MPa/30min before the start of the experiment, ensuring the current stability of the constant current source, and selecting the range of proper voltage test; when an experiment is started, filling liquid into six oil cylinders of the press, starting to record an oil pressure signal and a voltage signal when the oil pressure is increased to 5MPa, jumping to start pressure relief when the oil pressure is increased to 45MPa, and stopping recording and taking out a change curve of a card reader for analyzing the voltage signal when the oil pressure is released to 5 MPa;
(5) the file is converted into an Excel format by multichannel reading software, and then the Excel format is used for drawing by Origin, and the voltage signal, namely the sudden change of the resistance is observed. The experimental results are as follows: when the corresponding oil pressure is 28.3MPa, the voltage signal changes obviously, and an inflection point appears on a voltage curve, which indicates that the oil pressure value corresponds to the cavity pressure of 4.0 GPa. Finally, adding Bi, Tl and Cd3P2And the phase change pressure point of Ba is fitted by Origin to obtain a relation graph of oil pressure loading and cavity pressure, and a standard pressure curve is obtained.
Example four:
(1) selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm), cutting 1/3 of the selected pyrophyllite by using a steel saw, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
(2) processing the cut pyrophyllite into two pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with smooth surfaces by using a lathe, and controlling the blocks to be combined into cube pyrophyllite blocks with side length of 32.5mm, wherein the error range is within +/-0.1 mm;
(3) selecting a pyrophyllite block with a smooth surface, marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by a knife, and adding Cd with the weight of about 0.2g3P2Powder is filled into the groove; the conductivity of the polished conductive filmThe good copper sheet is cut into an L shape, and the middle sharp part is connected with Cd3P2Powder is contacted and conducted, copper sheets are fixed, the copper sheets exceeding the pyrophyllite part are cut off, and a part of 2-3mm is reserved and is folded to be contacted with the hammer face, so that a circuit is conducted; then covering the other pyrophyllite block, and standing and compacting for 2 hours by using a weight; the constant current source and the multi-channel recorder are respectively introduced into a front anvil, a rear anvil, a left anvil and a right anvil of a cubic press by adopting a four-wire method, two ends of the constant current source are connected with a resistor with the resistance value of 1K omega in parallel, and an oil pressure signal is connected to the multi-channel recorder;
(4) setting the voltage increasing and decreasing rate to be 5-45MPa/30min before the start of the experiment, ensuring the current stability of the constant current source, and selecting the range of proper voltage test; when an experiment is started, filling liquid into six oil cylinders of the press, starting to record an oil pressure signal and a voltage signal when the oil pressure is increased to 5MPa, jumping to start pressure relief when the oil pressure is increased to 45MPa, and stopping recording and taking out a change curve of a card reader for analyzing the voltage signal when the oil pressure is released to 5 MPa;
(5) the file is converted into an Excel format by multichannel reading software, and then the Excel format is used for drawing by Origin, and the voltage signal, namely the sudden change of the resistance is observed. The experimental results are as follows: when the corresponding oil pressure is 29.5MPa, the voltage signal changes obviously, and an inflection point appears on a voltage curve, which indicates that the oil pressure value corresponds to the cavity pressure of 4.0 GPa. Finally, adding Bi, Tl and Cd3P2And the phase change pressure point of Ba is fitted by Origin to obtain a relation graph of oil pressure loading and cavity pressure, and a standard pressure curve is obtained.
The experimental result of the invention is that the oil pressure error corresponding to the voltage mutation point is within 1.3MPa due to the slight difference of each experimental assembly, which belongs to the allowable error range of oil pressure loading of the high-pressure device of the large-cavity press, and multiple repeated experiments prove that the cadmium phosphide (Cd)3P2) Feasibility as a pressure calibration material. The process parameters listed (such as pyrophyllite quality, standard pressure material usage, boosting rate, groove depth and length, parallel resistance value, copper sheet length, etc.) can all achieve the invention at upper and lower interval values, and this is not an example. The foregoing is only a preferred embodiment of the present invention and is provided to illustrate the technical spirit of the present inventionWhile the invention has been described with reference to specific embodiments, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, combinations and simplifications can be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. Cadmium phosphide (Cd)3P2) The method is applied to calibrating the pressure in the cavity of the high-pressure device of the large-cavity press, and is characterized by comprising the following steps:
(1) selecting a dense pyrophyllite solid block (32.5 mm multiplied by 32.5 mm) with high quality;
(2) cutting off the selected pyrophyllite in the step (1) by about 1/3 volumes, and simultaneously ensuring that the height of the residual pyrophyllite is more than 16.25 mm;
(3) machining the cut pyrophyllite in the step (2) into pyrophyllite blocks (32.5 mm multiplied by 16.25 mm) with two smooth surfaces by using a lathe, namely combining the pyrophyllite blocks into square pyrophyllite blocks with the side length of 32.5 mm;
(4) selecting a pyrophyllite block with a smooth surface from the pyrophyllite blocks processed in the step (3), marking a small groove with the depth of about 2mm and the length of about 8mm at the center along the direction of a diagonal line by using a knife, and adding 0.2g of Cd3P2Powder is filled into the groove;
(5) cutting the bright copper sheet with good conductivity polished by abrasive paper into L shape, wherein the sharp part of the copper sheet is connected with Cd3P2Powder is contacted and conducted, copper sheets are fixed, then the copper sheets exceeding the pyrophyllite part are cut off, and a part of 2-3mm is reserved and is used for conducting a circuit of a hammer face after being folded;
(6) covering the other half of the pyrophyllite in the step (3), and standing and compacting for 2 hours by using a heavy object to ensure the compactness of the filling powder; the method adopts a four-wire method to arrange a circuit, introduces a constant current source and a multi-channel recorder into a front anvil, a rear anvil, a left anvil and a right anvil of a cubic press, and connects an oil pressure signal to the multi-channel recorder; setting the boosting rate and time, recording an oil pressure curve and selecting the voltage test range of the multi-channel recorder and recording the change of a voltage value under the premise of ensuring the current of the constant current source to be stable after the experiment begins; this patent adopts the cubic hinge chain formula press of making at home as high pressure to produce the device, and other types's high-voltage apparatus circuit arrangement is as the circumstances decides.
2. The method according to claim 1, wherein in step (1), the high-quality pyrophyllite solid block is selected to have Al as a main component2Si4O10(OH)2And the final product of decomposition at high temperature is SiO2、Al2O3The density of the selected pyrophyllite solid block is about 2.64g/cm3。
3. The method of claim 1, wherein in step (2), 1/3 of the pyrophyllite square block is cut off by a steel saw to make the cut surface not greatly inclined as much as possible for convenient processing.
4. The method as claimed in claim 1, wherein in step (3), when the pyrophyllite is machined by a lathe, the height of the pyrophyllite is ensured to be 16.25 (+ -0.1) mm as much as possible while the flatness of the plane is ensured, namely, the two blocks are combined to be machined into a cubic pyrophyllite block with a side length of 32.5 mm.
5. The method according to claim 1, wherein in the step (4), the groove is scribed at the centre of the pyrophyllite for the purpose of reducing the influence of the rheology generated during the process of compressing the powder on the detection of the electric signal, the depth and the length of the groove and the powder taking amount are upper and lower interval values, and the specific experiment can be flexibly implemented.
6. The method as claimed in claim 1, wherein in the step (5), the copper sheet is polished to polish the oxidized copper oxide film, so as to improve the conductivity of the copper sheet, the sharp part of the L-shaped copper sheet must be better attached with the powder so as to be conductive with the middle marking substance, after the copper sheet is fixed along the diagonal direction, the position of the measuring resistor of the multimeter is used to ensure the circuit connection, and the top ends of the two L-shaped copper sheets are forbidden to be too close to each other so as to avoid the problem of circuit short circuit.
7. The method according to claim 1, wherein in the step (6), a four-wire method is adopted to arrange the circuit, the four-wire method is favorable for reducing contact resistance, electric signals required to be acquired by the experiment can be clearer, the current value of the constant current source in the whole experiment process is ensured to be stable, and the multichannel recorder records the oil pressure of the press and the voltage signals in the circuit in the in-situ pressure loading process.
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