Device and method for synchronously measuring material resistance signal and regulating performance

Abstract

The present invention discloses a device and method for synchronously measuring material resistance signals and regulating performance, comprising: a sample fixture table, a resistance measuring device, and a heat treatment device; the sample fixture table includes four electrodes and a pressure controller, and the pressure controller can control the pressure between one end of the electrode and the sample to form a set stress field; each electrode is connected to the resistance measuring device through a wire for measuring the sample resistance signal; the sample fixture table is arranged inside the heat treatment device, and the heat treatment device can control the ambient temperature of the sample according to a set temperature control process. The resistance signal measuring device of the present invention can realize a rapid temperature change process under certain pressure-holding conditions, and realizes synchronous material performance regulation and high-frequency resistivity measurement under a thermal field and a stress field.

Description

Technical Field

[0001] The present invention relates to the technical field of resistance signal measurement, and particularly to a device and method for synchronously measuring material resistance signals and regulating properties. Background Art

[0002] The statements in this part merely provide background technical information related to the present invention and do not necessarily constitute prior art.

[0003] The resistivity of a material is essentially related to its electronic structure and is very sensitive to structural changes. Thus, the structural characteristics and evolution patterns of materials can be studied by collecting material resistance signals. For example, as the temperature of pure metal increases, the vibration amplitude of positive ions increases, and the hindrance to free electrons also increases. Therefore, the motion law of internal particles can be obtained by detecting the change in resistivity of pure metal during the heating process. For amorphous alloys, compared with the DSC curve with only an exothermic peak, the resistivity-temperature curve provides more details about the structural evolution of amorphous alloys. In addition to the disorder-to-order transition, other factors such as different crystallization paths, phase decomposition, formation of icosahedral phases or intermetallic compounds, and different crystallization kinetics also greatly affect the change in resistivity. Different from crystalline materials, even under a stress field far below the yield strength, amorphous alloys will exhibit slow flow behavior, that is, irreversible structural changes. This change is difficult to capture by conventional testing means, and measuring resistivity provides an opportunity to explore the structural changes of amorphous alloys under a stress field.

[0004] Adjusting the ambient temperature and applying external pressure are common means for regulating material properties. Changes in the thermal field and stress field can effectively change the atomic / electronic energy states inside the material, thereby promoting the evolution of the material structure and helping to explore the physical nature such as the properties and structural information of different materials. Different from conventional thermal signals and mechanical signals, this unique angle of resistance signals can effectively detect the detailed process of the evolution of material properties and structures, providing a way to analyze the dynamic process of materials under rapid temperature change and pressure holding conditions.

[0005] Under the regulation of rapid thermal fields and stress fields, how to synchronously and rapidly measure resistivity and monitor properties is an important issue faced in research. In this process, not only a large amount of experimental data needs to be recorded, but also the experimental data needs to be converted, processed, and plotted into curves; especially in the measurement process of small-sized materials, problems such as large workload, complex operation, and difficult error control are more obvious.

[0006] Although there are also design concepts in the prior art to apply "heat / temperature" or "pressure / stress / pressure" to a sample simultaneously for resistance measurement, they all preset a heat preservation temperature and pressure value first and then measure; it is impossible to achieve rapid changes in the temperature field and real-time regulation of the pressure field, and it is impossible to simultaneously perform material resistance measurement and performance regulation under the pressure field and temperature field. Summary of the Invention

[0007] To solve the above problems, the present invention proposes a device and method for synchronously measuring material resistance signals and regulating performance, which can realize synchronous and fine acquisition of dynamic resistance signal changes of alloy materials under the conditions of rapid temperature change and pressure holding, and simultaneously realize fine regulation of material performance.

[0008] In some embodiments, the following technical solutions are adopted:

[0009] A device for synchronously measuring material resistance signals and regulating performance, comprising: a sample fixture table, a resistance measurement device, and a heat treatment device;

[0010] The sample fixture table includes four electrodes and a pressure controller. The pressure controller can control the pressure between one end of the electrode and the sample to form a set stress field; each electrode is connected to the resistance measurement device through a wire for measuring the sample resistance signal.

[0011] The sample fixture table is arranged inside the heat treatment device, and the heat treatment device can control the ambient temperature of the sample according to a set temperature control process.

[0012] As a further solution, the sample fixture table further includes: a sample carrier table, an upper insulating gasket with holes, and a lower insulating gasket with holes; the holes in the upper insulating gasket with holes and the lower insulating gasket with holes are arranged opposite to each other, and the multiple electrodes are arranged in a row at equal intervals. Each electrode is inserted into the corresponding upper and lower holes, and one end of the spring ejector pin extends out of the lower insulating gasket with holes to contact the sample surface.

[0013] As a further solution, the upper insulating gasket with holes and the lower insulating gasket with holes are fixed by a gasket clamp.

[0014] As a further solution, the pressure controller is used to apply pressure between the upper part of the upper insulating gasket with holes and the lower part of the sample carrier table.

[0015] As a further solution, the heat treatment device includes: a temperature control unit, a heating furnace, and a temperature monitoring thermocouple; the temperature control unit is connected to the heating furnace through the temperature monitoring thermocouple; the sample fixture table can be placed inside the heating furnace.

[0016] As a further solution, the resistance measurement device can output a set constant current source signal.

[0017] As a further solution, the resistance measuring device measures the resistance signal based on the Kelvin four-wire detection method; four electrodes are respectively connected to the surface of the sample, two of which are used to input the current source, and the other two are used to output the measured voltage; the resistance value is calculated based on the measured voltage.

[0018] In some other embodiments, the following technical solution is adopted:

[0019] A method for synchronously measuring the resistance signal and regulating the performance of a material, comprising:

[0020] Press the spring thimble ends of the four electrodes against the surface of the sample to be measured respectively and make full contact with the sample to be measured;

[0021] Control the pressure of each electrode on the sample to be measured through a pressure controller so that the sample to be measured is in a set non-uniform pressure-holding state to form a stress field;

[0022] Control the temperature of the sample fixture table through a heat treatment device according to the set temperature control process;

[0023] Provide a set constant current source through a resistance measuring device, record the resistance signal data during the temperature change process, and calculate the resistivity data based on the resistance signal data; thus realizing the synchronous measurement of the resistance signal and performance regulation of the material under the thermal field and stress field.

[0024] Compared with the prior art, the beneficial effects of the present invention are:

[0025] (1) The resistance signal measuring device of the present invention can realize a rapid temperature change process under certain pressure-holding conditions, realizing synchronous material performance regulation and high-frequency resistivity measurement under the thermal field and stress field. Fine regulation of material properties can be achieved through the control of a rapidly changing thermal field and a non-uniform stress field, which helps to explore the physical mechanism behind the performance structure evolution of materials during the rapid temperature change and pressure-holding process. And this device provides a unique experimental method for deeply exploring the relationship between the thermoelectric properties of materials in a dynamically unbalanced state and revealing its physical essence.

[0026] (2) The present invention uses four electrodes to provide a set pressure for the material, and at the same time measures the resistance signal of the material based on the four electrodes. The result is simple and the operation is convenient. Placing the entire sample fixture table in a heat treatment device with rapid temperature change can realize the synchronous measurement of the resistance signal and performance regulation of the material.

[0027] Other features and advantages of the additional aspects of the present invention will be partially given in the following description, partially will become obvious from the following description, or will be understood through the practice of this aspect. Description of the Drawings

[0028] Figure 1 Schematic diagram of the structure of the device for synchronously measuring the resistance signal of materials under thermal field and stress field in the embodiment of the present invention;

[0029] Figure 2(a) is a schematic diagram of the finite element simulation sample fixture table; under the condition that the clamping force is 10 N, the temperature is rapidly increased, and the strain distribution diagrams of the Ti plate at 0 °C (Figure 2(b)), 225 °C (Figure 2(c)), and 825 °C (Figure 2(d)) are obtained respectively;

[0030] Figure 3(a) is the resistivity-temperature curve of the Ti plate during the heating process, and Figure 3(b) is the resistivity-temperature curve of the Fe-based amorphous alloy strip during the heating process;

[0031] Among them, 101. Temperature control unit, 102. Infrared heating furnace, 103. Temperature monitoring thermocouple, 201. Resistance measuring device, 202. Wire, 301. Sample carrier table, 302. Upper insulating gasket with holes, 303. Lower insulating gasket with holes, 304. Electrode, 401. Gasket clamp, 402. Pressure controller, 5. Sample. Detailed implementation manners

[0032] It should be noted that the following detailed descriptions are all illustrative and are intended to provide further descriptions of the present application. Unless otherwise specified, all technical and scientific terms used in the present invention have the same meanings as those commonly understood by those of ordinary skill in the technical field to which the present application belongs.

[0033] It should be noted that the terms used herein are only for describing specific implementation manners and are not intended to limit the exemplary implementation manners according to the present application. As used herein, unless the context clearly indicates otherwise, the singular forms are also intended to include the plural forms. In addition, it should be understood that when the terms "include" and / or "comprise" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or their combinations.

[0034] Embodiment 1

[0035] In one or more embodiments, a device for synchronously measuring the resistance signal of materials under thermal field and stress field is disclosed. Referring to Figure 1 , it specifically includes: a sample fixture table, a resistance measuring device 201, and a heat treatment device;

[0036] Among them, the sample fixture table includes a sample carrier table 301, an upper insulating gasket with holes 302, a lower insulating gasket with holes 303, four electrodes, and a pressure controller 402; the upper insulating gasket with holes 302 and the lower insulating gasket with holes 303 are spaced at a set distance, the holes in the upper insulating gasket with holes 302 and the lower insulating gasket with holes 303 are arranged opposite to each other, the four electrodes 304 are arranged in a row at equal intervals, each electrode 304 is inserted into the corresponding upper and lower holes, and one end of the spring pin is extended out of the lower insulating gasket with holes 303 to contact the surface of the sample.

[0037] A small platform is provided at the lower half of the electrode, the upper insulating gasket with holes 302 and the lower insulating gasket with holes 303 are respectively arranged above and below the small platform, and the two ends of the upper insulating gasket with holes 302 and the lower insulating gasket with holes 303 are respectively fixed by gasket clips 401.

[0038] A wire 202 is wound around the upper half of each electrode small platform, and the four wires are respectively connected to the resistance measuring device 201.

[0039] The pressure controller 402 is used to apply pressure between the upper part of the upper insulating gasket with holes 302 and the lower part of the sample carrier table 301, which can make the wire 202 and the electrode 304 in full contact and conduct electricity well; in addition, one end of the spring pin of the electrode is pressed on the surface of the sample 5 on the sample carrier table 301, which can provide a set pressure for the sample 5 and make the sample in an uneven pressure-holding state to form a stress field.

[0040] The resistance measuring device 201 in this embodiment can provide a constant current source of a set size, and the resistance measuring device 201 measures the resistance signal based on the Kelvin four-wire detection method; the four electrodes are respectively connected to the sample surface, two of the electrodes are used to input the current source, and the other two electrodes are used to output the measured voltage; the sample resistance value can be calculated based on the measured voltage.

[0041] It should be noted that the resistance measuring device 201 can adopt an existing resistance measuring and collecting instrument.

[0042] The heat treatment device in this embodiment includes a temperature control unit 101, an infrared heating furnace 102, and a temperature monitoring thermocouple 103; the temperature control unit 101 is connected to the infrared heating furnace 102 through the temperature monitoring thermocouple 103;

[0043] The sample fixture table is arranged in the infrared heating furnace 102, and a specific temperature control process can be set in the temperature control unit, for example: heating from 20°C to 200°C at a rate of 1K / s, holding at 200°C for 30s, and then naturally cooling. The temperature monitoring thermocouple 103 is used to monitor the temperature in the infrared heating furnace 102 and feedback it to the temperature control unit.

[0044] In this embodiment, a stress field of a set size is provided for the sample through the pressure controller 402, so that the sample is in a set non-uniform pressure-retaining state to form a stress field; then, a set rapid temperature change process is provided for the sample through the heat treatment device. During this process, the resistance value of the sample 5 is continuously measured, and the resistivity of the sample is calculated, and the change trend of the sample resistivity can be obtained; the synchronous measurement of the resistance signal of the sample 5 material and the performance regulation under the thermal field and the stress field are realized.

[0045] In this embodiment, by using the finite element simulation method, the strain distribution and evolution process of the sample under the stress field during the temperature change process are obtained, as shown in Figures 2(a)-(d). The simulation demonstrates the simultaneous regulation of material properties and high-frequency resistivity measurement under the thermal field and the stress field, and verifies the feasibility of applying the stress field to the sample through the sample fixture table and the electrodes.

[0046] Embodiment 2

[0047] In one or more embodiments, a method for synchronously measuring the material resistance signal under the thermal field and the stress field is disclosed. In this embodiment, the sample is described by taking the Ti plate as an example, and the specific process is as follows:

[0048] (1) One end of the spring thimble of the 4 electrodes is sequentially placed into the holes of the lower insulating tape-hole gasket 303, and then 4 wires are sequentially and tightly wound above the small platform of the electrode. Then, the upper insulating tape-hole gasket 302 is pressed into the upper end of the electrode. After ensuring good connection of each part, it is fixed with the gasket clamp 401. The Ti plate is placed flat on the sample table (301), and then one end of the spring thimble of the electrode is pressed on the surface of the Ti plate to ensure full contact between the four electrode contacts and the Ti plate. The pressure controller 402 fixes the entire sample fixture table to form a set stress field;

[0049] (2) The sample fixture table is placed in the infrared heating furnace 102, and the furnace cavity is closed. The vacuum is pumped according to the following steps:

[0050] ① Turn on the mechanical pump and the vacuum valve. When the resistance vacuum gauge shows 3.0E0, close the vacuum valve;

[0051] ② Turn on the argon gas cylinder and the inflation valve. When the pressure gauge shows -0.1, close the inflation valve;

[0052] Repeat steps ① and ② twice, then close the argon gas cylinder and keep the furnace cavity in an argon atmosphere.

[0053] (3) Set the heating and cooling process in the temperature control unit 101. In this embodiment, the temperature is increased from 20°C to 200°C at a rate of 1K / s, and kept at 200°C for 30s, and then cooled naturally.

[0054] (4) Connect four wires to the resistance measuring device 201 respectively. Set the output constant current source signal to 0.1 A and the data sampling frequency to 0.1 s on the control panel of the resistance measuring device 201. -1 A total of 2400 data points are recorded. For the integrity of the data, the data sampling duration should be slightly longer than the entire test duration.

[0055] (5) Turn on the data sampling and current source output of the resistance measuring device 201 in sequence, and then turn on the temperature rising and falling program in the temperature control unit 101.

[0056] (6) After the temperature rising and falling program ends, turn off the current source output and data sampling of the resistance measuring device 201 in sequence, and then turn off the resistance measuring device 201. Turn off the mechanical pump, open the air release valve to introduce air into the furnace cavity, take out the sample, and turn off the heat treatment device.

[0057] (7) Provide a set constant current source through the resistance measuring device 201, record the resistance signal data during the temperature change process, and calculate the resistivity data based on the resistance signal data; thus realizing the test of synchronously collecting the resistance signals of the Ti plate under the thermal field and stress field, and realizing the synchronous heat treatment and stress treatment of the Ti plate. The results are shown in Fig. 3(a), and the variation trend of the resistivity with temperature conforms to the characteristics of pure metals.

[0058] In some other embodiments, replace the Ti plate sample with an Fe-based amorphous alloy strip, and use the same measurement method to measure the resistance signal. The obtained results are shown in Fig. 3(b); it can be seen that the three-stage change of the resistivity increase-decrease-increase of the amorphous alloy is significantly different from the monotonic increasing trend of pure metals, reflecting the special electronic structure inside the amorphous alloy.

[0059] Although the specific embodiments of the present invention are described above in conjunction with the accompanying drawings, it is not a limitation to the protection scope of the present invention. Those skilled in the art should understand that based on the technical solutions of the present invention, various modifications or deformations that can be made by those skilled in the art without creative labor are still within the protection scope of the present invention.

Claims

1. A device for synchronously measuring a material resistance signal and regulating performance, characterized in that Comprising: A sample fixture table, a resistance measuring device, and a heat treatment device; The sample fixture table includes four electrodes and a pressure controller. The pressure controller can control the pressure between one end of the electrode and the sample to form a set stress field; each electrode is connected to the resistance measuring device through a wire for measuring the sample resistance signal; The sample fixture table is arranged inside the heat treatment device, and the heat treatment device can control the ambient temperature of the sample according to a set temperature control process.

2. The device for synchronously measuring the material resistance signal and regulating the performance according to claim 1, characterized in that, The sample fixture table further includes: a sample carrier table, an upper insulating gasket with holes, and a lower insulating gasket with holes; the holes in the upper insulating gasket with holes and the lower insulating gasket with holes are arranged opposite to each other, and multiple electrodes are arranged in a row at equal intervals. Each electrode is inserted into the corresponding upper and lower holes, and one end of the spring ejector pin extends out of the lower insulating gasket with holes to contact the sample surface.

3. The device for synchronously measuring a material resistance signal and regulating performance according to claim 2, wherein The upper insulating gasket with holes and the lower insulating gasket with holes are fixed by a gasket clamp.

4. The device for synchronously measuring the material resistance signal and regulating the performance according to claim 2, characterized in that, The pressure controller is used to apply pressure between the upper part of the upper insulating gasket with holes and the lower part of the sample carrier table.

5. The device for synchronously measuring the material resistance signal and regulating the performance according to claim 1, wherein, The heat treatment device includes: a temperature control unit, a heating furnace, and a temperature monitoring thermocouple; the temperature control unit is connected to the heating furnace through the temperature monitoring thermocouple; the sample fixture table can be placed inside the heating furnace.

6. The device for synchronously measuring a material resistance signal and regulating performance according to claim 1, characterized in that, The resistance measuring device can output a set constant current source signal.

7. The device for synchronously measuring a material resistance signal and regulating performance according to claim 6, wherein, The resistance measuring device measures the resistance signal based on the Kelvin four-wire detection method; the four electrodes are respectively connected to the sample surface, two of which are used to input the current source, and the other two are used to output the measured voltage; the resistance value is calculated based on the measured voltage.

8. A method for synchronously measuring a material resistance signal and regulating performance, characterized in that, Comprising: Press one end of the spring ejector pins of the four electrodes on the surface of the sample to be measured and make full contact with the sample to be measured; Control the pressure of each electrode on the sample to be measured through the pressure controller to make the sample to be measured in a set non-uniform pressure-holding state and form a stress field; Control the temperature of the sample fixture table through the heat treatment device according to a set temperature control process; Provide a set constant current source through the resistance measuring device, record the resistance signal data during the temperature change process, and calculate the resistivity data based on the resistance signal data; thus realizing the synchronous measurement of the material resistance signal and performance regulation under the thermal field and stress field.

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