CN112147414A - Method for measuring resistivity of metallic iron under ultrahigh pressure - Google Patents
Method for measuring resistivity of metallic iron under ultrahigh pressure Download PDFInfo
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- CN112147414A CN112147414A CN202011035505.3A CN202011035505A CN112147414A CN 112147414 A CN112147414 A CN 112147414A CN 202011035505 A CN202011035505 A CN 202011035505A CN 112147414 A CN112147414 A CN 112147414A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/08—Measuring resistance by measuring both voltage and current
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
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Abstract
The invention discloses a method for measuring the resistivity of metallic iron under ultrahigh pressure, which comprises the following steps: respectively processing a high-purity iron sheet and a rhenium sheet into a round sample and a rectangular component by using a laser cutting machine; the rhenium sheet is used as a heater, and the round iron sheet, three tungsten wires and one tungsten-rhenium alloy wire are put into an ultrahigh pressure testing device for assembly; placing the test assembly block in a six-sided-top large press, loading to specified pressure and temperature, and measuring and recording the resistivity of the sample by adopting a four-probe van der Waals principle; after the heating and data recording are finished, the pressure is unloaded; taking out a round iron sheet sample, fixing the round iron sheet sample by using epoxy resin, then cutting, grinding and polishing to obtain a longitudinal section of the round iron sheet, measuring the thickness, and calculating by using a van der Waals measurement formula to obtain the resistivity values of the metal iron sheet under different temperature and pressure conditions; the problems of large temperature gradient, inaccurate temperature measurement, mutual contact of measurement leads, excessive resistivity calculation parameters and large error in the prior art are solved.
Description
Technical Field
The invention belongs to the field of testing devices, and particularly relates to a method for measuring the resistivity of metallic iron under ultrahigh pressure.
Background
Common metals, such as iron, nickel, copper, aluminum, etc., have very low resistivity, all around minus eight and minus seven ohms per meter. It is particularly difficult to accurately measure the resistivity of these metals. There are many commercial metal resistivity measurement platforms and tools that are already in widespread use in laboratories and industry at atmospheric pressure. However, under ultra-high pressure and high temperature conditions, there is a lack of a method for measuring the resistivity of metals. Because the volume of the sample to be tested is limited in the high-temperature high-pressure generating device, the arrangement of the electrode lead is complicated, and the risk of high failure rate under the condition of extreme temperature and pressure is faced.
The conventional method for measuring the resistivity of a metal wire or a conductive film under normal pressure is: for linear samples, the kelvin four-wire method principle is used; for sheet or film samples, the four probe van der Pair principle was used. They can only obtain the resistivity of a high-conductivity sample at normal pressure, low temperature and normal pressure and high temperature, and cannot obtain the resistivity data under the conditions of high pressure and high temperature.
The existing resistivity measuring method of metal under high temperature and high pressure comprises a four-wire method aiming at a columnar sample, wherein the principle is a Kelvin four-wire method principle, but the temperature gradient caused by overhigh sample height is large; the measurement leads are in mutual contact, so that the influence of thermoelectric force cannot be avoided; the parameters for solving the resistivity comprise the diameter and the height of the columnar sample, and the problems of overlarge error (the error is between 7 and 15 percent) and the like caused by the overlarge parameters.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for measuring the resistivity of the metallic iron under the ultrahigh pressure is provided, so as to solve the technical problems that the resistivity measurement result of pure metal has large error and large temperature gradient, a flaky sample cannot be tested and the like under the ultrahigh pressure condition.
The technical scheme of the invention is as follows: a method for measuring the resistivity of metallic iron at ultra-high pressure, comprising the steps of:
step 1: a rhenium tube heater for processing the high-purity iron sheet and the rhenium sheet into a round sample and a rectangular component respectively by using a laser cutting machine, and rolling the rectangular component into a hollow cylindrical shape;
step 2: preparing three 99.9% high-purity tungsten wires with the diameter of 0.2mm and one tungsten-rhenium alloy wire containing 26 wt% of rhenium, flattening one end of each tungsten wire, and wrapping and protecting the flattened end by using a ceramic aluminum oxide tube and a copper wire coil;
and step 3: assembling an ultrahigh pressure test block;
and 4, step 4: placing the ultrahigh pressure test block in the step 3 in a cubic apparatus press, preheating, cooling to room temperature, and loading to a specified pressure and temperature range;
and 5: under different temperatures and pressures, measuring and recording the resistivity of the iron sheet sample by adopting a four-probe Van der Ware principle;
step 6: after the data recording is finished, unloading the pressure;
and 7: and taking out the round iron sheet sample, fixing the round iron sheet sample by using epoxy resin, then cutting, grinding and polishing to obtain a longitudinal section of the round iron sheet, measuring the thickness, and calculating by using a van der Waals measurement formula to obtain the resistivity values of the metal iron sheet under different temperature and pressure conditions.
Further, the round sample in the step 1 is 99.9% high-purity iron sheet with the thickness of 0.5mm and the diameter of 0.8-1.5 mm; the rectangular component is a 99.9% high purity rhenium sheet metal with a thickness of 0.2mm, a length of 8.5mm and a width of 7.5 mm.
Further, the method for assembling the ultra-high voltage test block in step 3 comprises:
3.1, selecting a chromium-containing magnesium oxide octahedron, drilling a cylindrical through hole in the center of the octahedron, sleeving a rhenium tube heater into the cylindrical through hole, reserving 4 through holes around the middle position of the rhenium tube heater, and reserving 4 through holes corresponding to the positions of the 4 through holes on the octahedron block and the heater;
3.2, sleeving a boron nitride cylinder in the rhenium tube heater cylinder, wherein 4 through holes are reserved in the boron nitride cylinder and the rhenium tube heater at the positions corresponding to the 4 through holes;
3.3, putting the iron sheet cut in the step 1 into the middle of a boron nitride cylinder;
3.4, horizontally penetrating three high-purity tungsten wires and one tungsten-rhenium alloy wire in the step 2 through a through hole in the high-voltage testing assembly block, and directly contacting the high-purity tungsten wires and the tungsten-rhenium alloy wire with the cross sections of the iron sheet sample in four directions to be used as conducting wires;
3.5, sealing the upper end and the lower end of the boron nitride cylinder by using a sintered alumina ceramic rod, and sealing the outside of the alumina ceramic rod by using a brittle magnesia rod;
and 3.6, splicing the octahedral assembly block containing the test sample with eight cubic tungsten carbide blocks, and insulating each lead.
Further, the specified pressure and temperature range in step 4 is 10-20GPa, 25-440 ℃.
Further, the resistivity measurement method in step 5 includes:
step 5.1, connecting a tungsten-rhenium alloy wire I and an adjacent high-purity tungsten wire II in the step 2 to a constant current source device; inputting 100-300 milliampere stable current into the round iron sheet through a lead wire, and outputting through a lead wire;
step 5.2, connecting the remaining two high-purity tungsten wire leads to a high-precision multimeter, marking the lead close to the lead I as a lead II, marking the other lead II as a lead III, and measuring the input current twice before and after to obtain the potential value difference value of the two ends of the circular iron sheet sample; eliminating the influence of the background potential of the sample;
step 5.3, keeping the tungsten-rhenium alloy lead wire (I) of the input current unchanged, connecting the current output end with another adjacent high-purity tungsten wire (II), then repeating the step 5.2, recording current and potential data again, wherein potential measurement is completed by the lead wire (II) and the lead wire (III);
furthermore, a thermocouple is arranged in the high-voltage test assembly block.
Furthermore, the lead connected with the constant current source device in the step 5.1 and the step 5.4 can be simultaneously connected with the constant current source device and the temperature measuring device through the temperature-resistance converter, so that the switching between temperature measurement and current supply is realized.
The invention adopts three protected metal tungsten wires and one alloy wire containing 26 wt% rhenium, tungsten and rhenium to contact with the periphery of the metal iron sheet sample under the conditions of ultrahigh pressure and high temperature, so that the resistivity of the sample is measured while the temperature is measured, and the direct contact between wires is avoided. The method uses the four-probe Van der Ware method principle to measure the resistivity, and the resistivity of the sample can be calculated only by knowing the thickness of the sample, which is a single parameter. Compared with the method using a columnar sample under high temperature and high pressure, the method uses a disc-shaped sample with smaller height, and reduces the influence of the temperature gradient of the sample in a high temperature and high pressure device on the measurement result. The method separates the four leads on the same horizontal plane, and avoids mutual contact and interference.
Compared with the reported four-wire measuring method for the columnar sample under the high-temperature and high-pressure conditions, the method has the technical advantages of accurate temperature measurement, more accurate measured resistivity and the like, and provides important guarantee for the research of measuring the resistivity of the metal and the alloy under the high-temperature and high-pressure conditions. The method can reduce the experimental error to be less than 3 percent and improve the measurement precision, because the shape of the sheet sample is fixed by using the symmetrical ceramic alumina plugs, the thickness change of the sample in the high-pressure compression process is controlled, the material of the magnesia plugs is softer than metal iron, and the magnesia plugs are easy to compress under ultrahigh pressure, thereby ensuring that the sample is not excessively compressed, the experimental error mainly depends on the error of the thickness, after the thickness of the left, the middle and the right positions is measured after the experiment, the average value and the error of the thickness can be given, and the error is less than 3 percent.
In the high-voltage assembly block, chromium-containing magnesium oxide octahedron and a boron nitride sleeve are used as pressure transmission media, a metal rhenium tube is used as a heating furnace, a thermocouple is used as a temperature measuring device, and the boron nitride sleeve is used as an insulating device. The high-pressure assembly block has the advantages that: firstly, two separated leads are used as a thermocouple for measuring temperature, the temperature can be measured while the resistivity is measured, and the influence of thermoelectric force on resistance measurement caused by direct contact of the leads of the thermocouple is avoided; the octahedron containing chromium and magnesium oxide is used as a primary pressure transmission medium and has good pressure transmission performance, machinability, heat resistance and heat preservation performance and insulativity; and the metal rhenium tube is used as a heating furnace, has uniform temperature and high heating efficiency, and can not flow to generate short circuit with the sample.
Description of the drawings:
FIG. 1 is a schematic longitudinal sectional view of the high pressure test assembly block prepared in step 3 of the present invention;
FIG. 2 is a schematic diagram of the electrical circuit layout for resistivity measurements according to step 5 of the present invention;
FIG. 3 is a scanning electron microscope image of a longitudinal section of a sample prepared in step 7 of the present invention after polishing;
fig. 4 is a graph of pure iron resistivity data measured at ultra-high pressure and high temperature in example 2 of the present invention.
In the figure, 1, chromium-containing magnesium oxide octahedron, 2, rhenium tube heater, 3, alumina ceramic rod, 4, tungsten wire, 5, iron sheet, 6, boron nitride cylinder, 7, brittle magnesium oxide rod, 8, ceramic alumina tube, 9 and copper wire coil.
The specific implementation mode is as follows:
a method for measuring the resistivity of metallic iron at ultra-high pressures, comprising:
step 1: a rhenium tube heater 2 for processing the high-purity iron sheet 5 and the rhenium sheet into a circular sample and a rectangular member, respectively, by using a laser cutter, and rolling the rectangular member into a hollow cylindrical shape;
step 2: preparing three 99.9 percent high-purity tungsten wires with the diameter of 0.2mm and one tungsten-rhenium alloy wire containing 26wt percent rhenium, flattening one end of each tungsten wire, and wrapping and protecting the flattened end by using a ceramic aluminum oxide tube 8 and a copper wire coil 9;
and step 3: assembling the ultrahigh pressure test block, wherein the assembling method comprises the following steps:
3.1, selecting a chromium-containing magnesium oxide octahedron 1, drilling a cylindrical through hole in the center of the octahedron, sleeving a rhenium tube heater 2 into the cylindrical through hole, reserving 4 through holes around the middle position of the rhenium tube heater 2, and reserving 4 through holes at the positions of the octahedron block and the 4 through holes on the heater correspondingly;
3.2, sleeving a boron nitride cylinder 6 in the rhenium tube heater 2, wherein 4 through holes are reserved in the boron nitride cylinder 6 corresponding to the positions of the 4 through holes on the rhenium tube heater 2;
3.3, putting the iron sheet 5 cut in the step 1 into a boron nitride cylinder 6;
3.4, horizontally penetrating three high-purity tungsten wires and one tungsten-rhenium alloy wire in the step 2 through a through hole in the high-voltage testing assembly block, and directly contacting the cross sections of the iron sheet 5 sample in four directions to be used as conducting wires;
3.5, sealing the upper end and the lower end of the boron nitride cylinder 6 by using a sintered alumina ceramic rod 3, and sealing the outside of the alumina ceramic rod 3 by using a brittle magnesium oxide rod 7;
and 3.6, splicing the octahedral assembly block containing the test sample with eight cubic tungsten carbide blocks, and insulating each lead.
And 4, step 4: placing the high-pressure test assembly block finished in the step 3 in a cubic apparatus press, preheating, keeping the temperature for 2 hours, cooling to room temperature, and loading to a specified pressure and temperature range of 10-20GPa and 25-440 ℃, wherein the specific parameters refer to the embodiment 1-2; the temperature and pressure of the preheating are the same as the specified pressure and temperature in order to eliminate the prestress between the assembled parts, so that the subsequent pressurizing and heating processes are more uniform.
And 5: under different temperatures and pressures, measuring and recording the resistivity of the sample by adopting a four-probe Van der Ware principle; the method for measuring the resistivity in the step 5 comprises the following steps:
step 5.1, connecting a tungsten-rhenium alloy wire I and an adjacent high-purity tungsten wire II in the step 2 to a constant current source device; inputting 100-300 milliampere stable current into the round iron sheet 5 through a lead wire, and outputting through a lead wire II;
step 5.2, connecting the remaining two high-purity tungsten wire leads to a high-precision multimeter, marking the lead close to the lead I as a lead II, marking the other lead II as a lead III, and measuring the input current twice before and after to obtain the potential value difference value of the two ends of the circular iron sheet sample; eliminating the influence of the background potential of the sample;
step 5.3, keeping the tungsten-rhenium alloy lead wire (I) of the input current unchanged, connecting the current output end with another adjacent high-purity tungsten wire (II), then repeating the step 5.2, recording current and potential data again, wherein potential measurement is completed by the lead wire (II) and the lead wire (III);
and a thermocouple is arranged in the high-voltage test assembly block. The lead connected with the constant current source device in the step 5.1 and the step 5.4 can be simultaneously connected with the constant current source device and the temperature measuring device through the temperature-resistance converter, so that the switching of temperature measurement and current supply is realized.
Step 6: unloading the pressure after completing the data recording at intervals of about 50-100 ℃;
and 7: and taking out the round iron sheet sample, fixing the round iron sheet sample by using epoxy resin, then cutting, grinding and polishing to obtain a longitudinal section of the round iron sheet, measuring the average thickness d, and calculating by using a van der Waals measurement formula to obtain the resistivity values of the metal iron sheet under different temperature and pressure conditions.
| Serial number | Pressure of | Maximum temperature | Fixed current | Average thickness d |
| Example 1 | 10GPa | 300℃ | 100mA | 0.482mm |
| Example 2 | 20GPa | 440℃ | 300mA | 0.463mm |
Recording Current and potential of example 1
Recording Current and potential of example 2
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. A method for measuring the resistivity of metallic iron under ultra-high pressure, characterized in that it comprises the following steps:
step 1: a rhenium tube heater (2) which respectively processes a high-purity iron sheet (5) and a rhenium sheet into a round sample and a rectangular component by using a laser cutting machine and rolls the rectangular component into a hollow cylindrical shape;
step 2: preparing three 99.9 percent high-purity tungsten wires with the diameter of 0.2mm and one tungsten-rhenium alloy wire containing 26wt percent rhenium, flattening one end of each tungsten wire, and wrapping and protecting the flattened end by using a ceramic aluminum oxide tube (8) and a copper wire coil (9);
and step 3: assembling an ultrahigh pressure test block;
and 4, step 4: placing the ultrahigh pressure test block in the step 3 in a cubic apparatus press, preheating, cooling to room temperature, and loading to a specified pressure and temperature range;
and 5: under different temperatures and pressures, measuring and recording the resistivity of the iron sheet (5) sample by adopting a four-probe Van der Ware principle;
step 6: after the data recording is finished, unloading the pressure;
and 7: and (3) taking out a sample of the round iron sheet (5), fixing the sample by using epoxy resin, cutting, grinding and polishing a longitudinal section of the round iron sheet, measuring the thickness, and calculating by using a van der Waals measurement formula to obtain the resistivity values of the metal iron sheet under different temperature and pressure conditions.
2. The method of claim 1, wherein the method comprises the following steps: the round sample in the step 1 is 99.9 percent high-purity iron sheet with the thickness of 0.5mm and the diameter of 0.8-1.5 mm; the rectangular component is a 99.9% high purity rhenium sheet metal with a thickness of 0.2mm, a length of 8.5mm and a width of 7.5 mm.
3. The method of claim 1, wherein the method comprises the following steps: step 3 the method for assembling the ultrahigh pressure test block comprises the following steps:
3.1, selecting a chromium-containing magnesium oxide octahedron (1), drilling a cylindrical through hole in the center of the octahedron, sleeving a rhenium tube heater (2) into the cylindrical through hole, reserving 4 through holes around the middle position of the rhenium tube heater (2), and reserving 4 through holes at the positions of the octahedron block and the 4 through holes on the heater correspondingly;
3.2, sleeving a boron nitride cylinder (6) in the rhenium tube heater (2), wherein 4 through holes are reserved in the boron nitride cylinder (6) and the rhenium tube heater (2) at positions corresponding to 4 through holes;
3.3, putting the iron sheet (5) cut in the step 1 into the middle of a boron nitride cylinder (6);
3.4, horizontally penetrating three high-purity tungsten wires and one tungsten-rhenium alloy wire in the step 2 through a through hole in the high-voltage testing assembly block, and directly contacting the cross sections of the iron sheet (5) sample in four directions to be used as conducting wires;
3.5, sealing the upper end and the lower end of the boron nitride cylinder (6) by using a sintered alumina ceramic rod (3), and sealing the outside of the alumina ceramic rod (3) by using a brittle magnesia rod (7);
and 3.6, splicing the octahedral assembly block containing the test sample with eight cubic tungsten carbide blocks, and insulating each lead.
4. The method of claim 1, wherein the method comprises the following steps: the specified pressure and temperature ranges in step 4 are 10-20GPa, 25-400 ℃.
5. The method of claim 1, wherein the method comprises the following steps: the method for measuring the resistivity in the step 5 comprises the following steps:
step 5.1, connecting a tungsten-rhenium alloy wire I and an adjacent high-purity tungsten wire II in the step 2 to a constant current source device; inputting 100-300 milliampere stable current into the round iron sheet (5) through a lead wire (I), and outputting through a lead wire (II);
step 5.2, connecting the remaining two high-purity tungsten wire leads to a high-precision multimeter, marking the lead close to the lead I as a lead II, marking the other lead II as a lead III, and measuring the input current twice before and after to obtain the potential value difference value of the two ends of the circular iron sheet sample; eliminating the influence of the background potential of the sample;
and 5.3, keeping the tungsten-rhenium alloy wire (I) of the input current unchanged, connecting the current output end to another adjacent high-purity tungsten wire (II), and then repeating the step 5.2, recording current and potential data again, wherein potential measurement is completed by the wire (II) and the wire (III).
6. The method of claim 1, wherein the method comprises the following steps: and a thermocouple is arranged in the high-voltage test assembly block.
7. The method of claim 5, wherein the method comprises the following steps: the lead connected with the constant current source device in the step 5.1 and the step 5.4 can be simultaneously connected with the constant current source device and the temperature measuring device through the temperature-resistance converter, so that the switching between temperature measurement and current supply is realized.
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| CN115436710A (en) * | 2022-09-22 | 2022-12-06 | 厦门大学 | High-temperature conductivity measurement clamp, system and method |
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| CN115436710B (en) * | 2022-09-22 | 2024-05-14 | 厦门大学 | High-temperature conductivity measurement clamp, system and method |
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