CN109164136B - High-flux measurement system and method for thermoelectric transport parameters - Google Patents
High-flux measurement system and method for thermoelectric transport parameters Download PDFInfo
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Abstract
The invention discloses a high-flux measuring system and method for thermoelectric transport parameters, wherein the system comprises: the system comprises a three-dimensional platform and a control system, wherein the three-dimensional platform is provided with an X-Y two-axis moving platform for placing a sample to be detected and a Z-axis moving platform provided with a four-probe assembly, and the four-probe assembly is used for measuring the conductivity and the Seebeck coefficient of a region to be detected of the sample to be detected; the heat reflection measuring device is used for dividing the pulse laser into a first laser beam and a second laser beam with preset optical path difference, the first laser beam is used for heating a region to be measured of a sample to be measured, and the second laser beam is used for measuring the heat conductivity of the region to be measured of the sample to be measured; the first laser beam simultaneously serves as a heat source for measuring the seebeck coefficient by the four-probe set. The high-throughput measurement of the thermal conductivity of a large-size sample can be realized by combining a high-precision X-Y two-axis moving platform, the measurement efficiency of the Seebeck coefficient can be ingeniously improved by using the first laser beam as a heat source for measuring the Seebeck coefficient by using the four-probe group, and the high-throughput measurement of thermoelectric transport parameters such as the electrical conductivity, the Seebeck coefficient and the thermal conductivity can be further realized.
Description
Technical Field
The invention relates to the technical field of thermoelectric materials, in particular to a high-flux measurement system and method for thermoelectric transport parameters.
Background
For large-scale application of thermoelectric materials, finding and searching for new materials and optimizing the performance of existing materials are the key points. The method for synthesizing a new material or improving the performance of the existing material adopts the traditional one-time design, preparing a sample with a single composition, and then analyzing and characterizing the composition and the structure and measuring thermoelectric transport parameters obviously consumes time and labor, and greatly increases the research and development period and the research and development cost. Therefore, the conventional methods and techniques for preparing and measuring thermoelectric materials have failed to meet the needs of their development.
In view of the above requirements, firstly, in material preparation, a preparation method based on combinatorial materials science is the mainstream method for preparing thermoelectric materials with high flux at present, and can be used for systematically researching the characteristics of the thermoelectric materials in a complex multi-component system. The sample prepared by the preparation method based on the combined materials science is completely different from the sample prepared by the traditional method, and the sample prepared by the traditional method usually contains a single system component and a single structure in one sample. While the samples prepared based on the above method usually have large size, for example, thousands or even more samples are contained on one substrate, especially the samples prepared by the above method are the samples of the micro-zone composition gradient material, that is, the composition gradient area in the sample is often micron or even submicron order. In view of the large-size sample made of the material with gradually changed micro-area components, in order to improve the efficiency of material performance optimization design and shorten the period for screening the material with optimal performance, a micro-area multi-parameter high-throughput measurement method and technology which are suitable for the large-size sample are needed, and therefore a complete new thermoelectric material research and development chain is formed. The thermoelectric transport parameters of a thermoelectric material are mainly electrical conductivity, seebeck coefficient and thermal conductivity. The material can not only represent the thermoelectric transport characteristics of the material, but also indirectly reflect the concentration and the mobility of carriers in the material. Meanwhile, the thermoelectric figure of merit, namely ZT value, calculated by the three parameters is an important index for evaluating the performance of the thermoelectric material.
However, in the prior art, it is difficult to realize high-throughput measurement of large-size samples of the micro-area component gradient material, such as measurement of electrical conductivity and seebeck coefficient, based on a static measurement method, and specifically, a large-size sample to be measured is cut into samples with preset sizes, and the samples with the preset sizes are measured by using a four-probe assembly. The measurement can only be carried out on a sample with a preset size, and if the measurement method is adopted to carry out measurement on the conductivity and the Seebeck coefficient of the material with gradually changed components in a micron or even submicron size area, the measurement efficiency is low, and the measurement structure error is large.
The thermal conductivity measurement methods and technologies of materials are more, such as: laser flash, infrared thermal radiation, scanning thermal microscopy and the like. The laser flash method is an international standard method for measuring the thermal conductivity, however, the laser flash method requires a specific geometric shape of a sample during measurement, and graphite spraying treatment is required for the sample, so that the error is large for measurement of the micro-area component gradient material.
Therefore, the measurement of the thermoelectric transport parameters of a large-size sample made of the material with gradually changed micro-area components is difficult to realize high-throughput measurement, and a complete new thermoelectric material research and development chain is difficult to form.
Disclosure of Invention
The main object of the present invention is to achieve high throughput measurement of thermoelectric transport parameters of thermoelectric materials.
To this end, according to a first aspect, the present invention provides a high-throughput measurement system for a thermoelectric transport parameter, the thermoelectric transport parameter comprising: electrical conductivity, seebeck coefficient, and thermal conductivity, the system comprising: the system comprises a three-dimensional platform and a control system, wherein the three-dimensional platform is provided with an X-Y two-axis moving platform for placing a sample to be detected and a Z-axis moving platform provided with a four-probe assembly, and the four-probe assembly is used for measuring the conductivity and the Seebeck coefficient of a region to be detected of the sample to be detected; the heat reflection measuring device is used for receiving the pulse laser and dividing the pulse laser into a first laser beam and a second laser beam with preset optical path difference, the first laser beam is used for heating a to-be-measured area of a to-be-measured sample, and the second laser beam is used for measuring the heat conductivity of the to-be-measured area of the to-be-measured sample; the first laser beam simultaneously serves as a heat source for measuring the seebeck coefficient by the four-probe set.
Optionally, a second laser beam is used to measure the thermal reflectivity and the rate of change of the thermal reflectivity of the area under test.
Optionally, the system further comprises: and the synchronous signal triggering device is used for triggering the three-dimensional platform when the second laser beam reaches the surface of the sample to be measured, and moving the four-probe assembly to the area irradiated by the second laser beam so as to measure the voltage difference caused by the temperature change of the area to be measured.
Optionally, the system further comprises: the data acquisition device is used for acquiring voltage difference, heat reflectivity and heat reflectivity change rate; the calculating device is connected with the data acquisition device and used for calculating the temperature distribution of the region to be measured according to the heat reflectivity change rate and calculating the heat conductivity of the region to be measured based on a preset mathematical model; (ii) a The calculating device is also used for calculating the Seebeck coefficient of the area to be measured according to the calculated temperature and voltage difference.
Optionally, the data acquisition device comprises: the photoelectric detector is used for receiving the second laser beam reflected by the area to be detected, converting the heat reflectivity signal into an electric signal and inputting the electric signal into the computing device; and the electrical parameter collector is used for collecting the voltage difference and the conductivity and inputting the voltage difference and the conductivity into the computing device.
Optionally, the sample to be tested includes a plurality of regions to be tested, and the regions to be tested are switched by the movement of the X-Y two-axis moving platform.
According to a second aspect, an embodiment of the present invention provides a method for measuring a high-throughput thermoelectric transport parameter, where the method for measuring a thermoelectric transport parameter of a sample to be measured by using the system for measuring a high-throughput thermoelectric transport parameter of any one of the above first aspects includes: s1, controlling the movement of an X-Y axis moving platform and a Z axis moving platform, and measuring the conductivity of a sample to be measured by adopting a four-probe assembly; s2, heating the sample to be measured by adopting a first laser beam, detecting the heat conductivity of the heated area by adopting a second laser beam, and moving the Z-axis moving platform to enable the four-probe assembly to contact the heated area so as to measure the Seebeck coefficient.
Optionally, the sample to be tested comprises a plurality of regions to be tested; controlling the movement of the X-Y two-axis moving platform and the Z-axis moving platform, and measuring the conductivity of the sample to be measured by adopting the four-probe assembly comprises the following steps: s11, determining a region to be detected in a sample to be detected; s12, controlling the X-Y two-axis moving platform to move the area to be detected to an orthographic projection area of the four-probe assembly; s13, controlling the Z-axis moving platform to move towards the sample to be measured, enabling the four-probe assembly to contact with a region to be measured of the sample to be measured, and measuring the conductivity of the contacted region to be measured; s14, controlling the Z-axis moving platform to be far away from the sample to be measured, and repeating the steps S11-S13 until the conductivity measurement of all the areas to be measured is completed.
Optionally, heating the sample to be measured by using the first laser beam, detecting the thermal conductivity of the heated region by using the second laser beam, and moving the Z-axis moving platform to make the four-probe assembly contact the heated region, wherein measuring the seebeck coefficient includes: s21, determining a region to be detected in a sample to be detected; s22, controlling the X-Y two-axis moving platform to move the area to be detected to the orthographic projection area of the four-probe assembly; s23, adopting a first laser beam to enter the area to be tested so as to heat the area to be tested; s24, when the first laser beam heats the area to be measured for a preset duration, a second laser beam is incident to the area to be measured so as to measure the heat reflectivity and the temperature of the area to be measured; s25, when the second laser beam is incident to the area to be measured, controlling the Z-axis moving platform to face the area to be measured, and enabling the four-probe assembly to contact the area to be measured so as to measure the voltage difference caused by the temperature change of the area to be measured; s26, controlling the Z-axis moving platform to be far away from the sample to be measured, and repeating the steps S21-S53 until the measurement of the thermal conductivity and the Seebeck coefficient of all the regions to be measured is completed.
The thermoelectric transport parameter high-flux measurement system and method provided by the embodiment of the invention adopt the three-dimensional platform with the X-Y two-axis moving platform and the Z-axis moving platform, can realize the measurement of large-size samples, and are particularly suitable for the measurement of thermoelectric transport parameters such as the thermal conductivity of materials with gradually changed compositions in a micro-area. The measurement of a plurality of areas can be realized through the movement of the X-Y two-axis mobile platform, the heat reflection measurement device has very high space-time resolution based on the femtosecond pulse laser technology, the time measurement resolution can be improved by three orders of magnitude compared with the traditional thermocouple temperature measurement method by the dual-wavelength femtosecond laser ultrafast temperature test technology, the signal-to-noise ratio can be improved by three orders of magnitude compared with the single-wavelength femtosecond laser ultrafast temperature test technology, the heat reflection signals of samples can be improved with high precision, and the accurate measurement of the thermoelectric spectrum signals after the femtosecond laser heating is realized. Meanwhile, by combining a high-precision X-Y two-axis moving platform, high-throughput measurement of the heat conductivity of a large-size sample can be realized, the first laser beam serving as a heat source for measuring the Seebeck coefficient by using the four-probe set can ingeniously improve the measurement efficiency of the Seebeck coefficient, and further can realize high-throughput measurement of thermoelectric transport parameters such as the electric conductivity, the Seebeck coefficient and the heat conductivity, and the like.
Drawings
FIG. 1 is a schematic diagram of a thermoelectric transport parameter high throughput measurement system according to an embodiment of the present invention;
FIG. 2 shows a schematic view of a thermal reflectance measurement apparatus of an embodiment of the present invention;
FIG. 3 is a schematic diagram of another thermoelectric transport parameter high throughput measurement system in accordance with an embodiment of the present invention;
FIG. 4 shows a schematic diagram of a four probe assembly of an embodiment of the present invention;
FIG. 5 shows a schematic diagram of a thermoelectric transport parameter high throughput measurement method according to an embodiment of the present invention;
FIG. 6 shows a schematic diagram of another thermoelectric transport parameter high throughput measurement method of an embodiment of the present invention;
FIG. 7 shows a schematic diagram of another thermoelectric transport parameter high-throughput measurement method of an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention provides a high-flux measurement system for thermoelectric transport parameters, wherein the thermoelectric transport parameters comprise: electrical conductivity, seebeck coefficient and thermal conductivity, as shown in figures 1 and 3, the system comprising: the three-dimensional platform 20 is provided with an X-Y two-axis moving platform 21 for placing a sample 30 to be measured and a Z-axis moving platform 22 provided with a four-probe assembly 23, wherein the four-probe assembly 23 is used for measuring the conductivity and the Seebeck coefficient of a region to be measured of the sample 30 to be measured; the heat reflection measuring device 10 is configured to receive a pulse laser and divide the pulse laser into a first laser beam 101 and a second laser beam 102 with a preset optical path difference, where the first laser beam 101 is configured to heat a region to be measured of the sample 30 to be measured, and the second laser beam 102 is configured to measure a thermal conductivity of the region to be measured of the sample 30 to be measured. The first laser beam 101 serves as a heat source for measuring the seebeck coefficient by the four probe set.
The three-dimensional platform 20 with the X-Y two-axis moving platform 21 and the Z-axis moving platform 22 is adopted, measurement of large-size samples can be achieved, measurement of multiple areas can be achieved through movement of the X-Y two-axis moving platform 21, the heat reflection measuring device 10 has high space-time resolution on the basis of a femtosecond pulse laser technology, time measurement resolution can be improved by three orders of magnitude compared with a traditional thermocouple temperature measuring method through a dual-wavelength femtosecond laser ultrafast temperature testing technology, signal-to-noise ratio can be improved by three orders of magnitude compared with a single-wavelength femtosecond laser ultrafast temperature testing technology, heat reflection signals of the samples can be improved with high precision, and accurate measurement of the thermoelectric spectrum signals after heating of femtosecond lasers is achieved. Meanwhile, the high-throughput measurement of the heat conductivity of a large-size sample can be realized by combining the high-precision X-Y two-axis moving platform 21. The first laser beam 101 serving as a heat source for measuring the Seebeck coefficient by the four-probe group can improve the measurement efficiency of the Seebeck coefficient ingeniously, so that high-throughput measurement of thermoelectric transport parameters such as electric conductivity, the Seebeck coefficient and thermal conductivity can be realized, the ultrafast thermoelectric process of materials can be researched by the femtosecond laser thermophysical property measurement system, and important experimental data are provided for research and development of new thermoelectric material and performance optimization.
The working principle of the high-throughput measuring system for the thermoelectric transport parameters will be described in detail below, after the first laser beam 101 heats the region to be measured, the second laser beam 102 enters the heated region to be measured to measure the thermal reflectivity of the region to be measured and the change rate of the thermal reflectivity, specifically, when the second laser beam 102 measures the thermophysical property of the material, the material to be measured needs to be calibrated first to obtain the thermal reflectivity, and then the change rate of the thermal reflectivity is measured. When the second laser beam 102 is incident on the region to be measured, the synchronization signal triggering device 40 triggers the three-dimensional platform 20 to move the four-probe assembly 23 to the region irradiated by the second laser beam 102, so as to measure the voltage difference caused by the temperature change of the region to be measured. And a data acquisition device 50 for acquiring the heat reflectivity and the voltage difference. The calculating device 60 is connected with the data acquisition device 50 and used for calculating the temperature distribution of the region to be measured according to the change rate of the heat reflectivity and calculating the heat conductivity of the region to be measured based on a preset mathematical model; the calculating means 60 is further adapted to calculate the seebeck coefficient of the area to be measured based on the calculated temperature and voltage difference. Specifically, a photoelectric detector may be used for receiving the second laser beam 102 reflected by the region to be measured, converting the thermal reflectivity into an electrical signal, and inputting the electrical signal to the computing device 60; and the electrical parameter collector is used for collecting the voltage difference and the conductivity and inputting the voltage difference and the conductivity into the computing device 60.
As shown in fig. 2, the heat reflection measuring device 10 has the following principle: the femtosecond laser is generated by the laser 11, and the femtosecond laser pulse train generates two laser beams with mutually perpendicular polarization directions, namely pumping light and probe light, namely a first laser beam and a second laser beam, by the polarizer 12 and the polarization beam splitter 13. After the second laser beam passes through the frequency doubling crystal 14, the frequency is doubled and the wavelength is reduced by half. The first laser beam 101 is used to pulse heat the sample and the second laser beam is used to obtain a temperature response signal on the sample. The first laser beam enters the electro-optical modulator 15 and is loaded with a modulation signal. The second laser beam changes its optical path through the delay line 16, thereby changing the delay time between the second laser beam and the first laser beam. The first laser beam and the second laser beam pass through the cold light mirror 17 to realize a collinear light path, and the two beams of light are focused to the same point on the surface of the sample 30 to be measured through the focusing objective lens. The reflected second laser beam signal is then converted into an electrical signal by the photodetector 18, and the signal at the desired modulation frequency is extracted by the lock-in amplifier 19 on the basis of this signal, and finally processed by the calculation means 60 to obtain a temperature measurement at a certain time delay point. And then, the delay time is changed to obtain a temperature response curve with sub-picosecond time resolution under the heating of the ultrashort pulse. Meanwhile, the X-Y two-axis moving platform is combined to scan a tested sample, so that the function of quickly measuring the thermal conductivity is realized.
The principle of measuring temperature by heat reflection is described below, and high-throughput measurement of temperature and thermal conductivity is realized by using the principle of heat reflection based on a femtosecond pulse laser technique combined with a modulation-phase-locked amplification technique, and the heat reflection method is based on measuring the variation of the reflectivity of a sample surface relative to the temperature change. When the light beam irradiates the surface or interface of the material, the change of the temperature can cause the change of the light intensity of the reflected light, thereby realizing the measurement of the temperature of the measured sample.
The thermal reflectivity of the material can be measured directly. For normally incident light, there is the following formula:
the optical constants n and k in the formula (1) are real numbers and positive numbers obtained by optical measurement. They are obtained by the following formula and complex dielectric function ∈1+i∈2And (4) associating.
The thermoreflectance technique is to measure the change in the complex dielectric function e.
The amount of change Δ ∈ caused by the external modulation1And Δ ∈2The effect on the thermal reflectivity is explained by the following differential equation.
In formula (4), a ═ n (n)2-3k2-1)，B＝k(3n2-k2-1)
In equation (4), the coefficients α and β are functions of photon energy.
In thermal reflection, modulation of temperature results in a change in lattice complex dielectric function ∈ due to a change in band gap energy and a change in the broadening coefficient Γ, as shown in the following formula
From which the relation between the heat reflectivity and the temperature can be determined. If the heat reflectivity can be measured, the temperature of the measured area can be obtained, and then the heat conductivity can be obtained through curve fitting of the corresponding mathematical model.
The principle of measuring the seebeck coefficient is described below, wherein one end of the region to be measured is at a constant temperature, the other end of the region to be measured is rapidly heated by the first laser beam to generate a temperature difference delta T, so that electric potentials V are generated at two ends of the sample, the change data of the electric potentials V in the temperature difference disappearance process is obtained by testing the four-probe assembly, the data is drawn into a V-delta T linear relation curve by combining the temperature data measured by the second laser beam, and the slope of the curve is the seebeck coefficient of the sample to be measured, namely
S＝dV/d(ΔT) (6)
The conductivity and the seebeck coefficient of the sample at different temperatures can be measured by controlling the temperature and the temperature gradient of the sample.
In this embodiment, the conductivity measurement is performed by a standard four-probe method, specifically, the conductivity measurement is performed by four probes as shown in fig. 4, when four metal probes of probe 1, probe 2, probe 3, and probe 4 are aligned in a straight line and pressed on the measured area with a certain pressure, and a current I is passed between the two points of probe 1 and probe 4, so that a potential difference V is generated between probe 2 and probe 3.
Resistivity of material
Coefficient of probe
In formula (8): s1、S2、S3The distances between probes 1 and 2, between probes 2 and 3, and between probes 3 and 4, respectively.
The voltage V is obtained through measurement, so that the resistivity can be calculated, and the conductivity of the material to be measured can be further calculated.
The four-probe assembly for measuring the Seebeck coefficient and the electric conductivity is integrated into a dual-wavelength femtosecond pulse laser heat reflection measurement system to form a complete thermoelectric material thermoelectric transport parameter measurement system, so that the measurement targets of the heat conductivity, the electric conductivity and the Seebeck coefficient are completed on one device, and the test efficiency is improved; on the other hand, the femtosecond laser thermophysical property measurement system is utilized to research the ultrafast thermoelectric process of the material, and important experimental data are provided for the research and development of a novel thermoelectric material and the performance optimization.
The embodiment of the invention also provides a thermoelectric transport parameter high-throughput measuring method, the thermoelectric transport parameter high-throughput measuring system in the embodiment is adopted to measure the thermoelectric transport parameters of the sample to be measured, as shown in fig. 5, the method comprises the following steps:
s1, controlling the movement of the X-Y axis moving platform and the Z axis moving platform, and measuring the conductivity of a sample to be measured by adopting a four-probe assembly.
S2, heating the sample to be measured by adopting a first laser beam, detecting the heat conductivity of the heated area by adopting a second laser beam, and moving the Z-axis moving platform to enable the four-probe assembly to contact the heated area so as to measure the Seebeck coefficient.
Specifically, the conductivity may be measured first, as shown in fig. 6, and the method for measuring the conductivity may include:
s11, determining a region to be detected in a sample to be detected;
and S12, controlling the X-Y two-axis moving platform to move the area to be detected to the orthographic projection area of the four-probe assembly.
And S13, controlling the Z-axis moving platform to move towards the sample to be measured, enabling the four-probe assembly to contact one area to be measured of the sample to be measured, and measuring the conductivity of the contacted area to be measured.
S14, controlling the Z-axis moving platform to be far away from the sample to be detected.
And S15, judging whether the conductivity of all the areas to be measured is measured, and if so, entering the step S2. If the measurement of all the areas is not completed, the process returns to step S11.
During the measurement of the conductivity, a certain current is supplied to the region to be measured to complete the measurement of the voltage, and the voltage measurement data is input into a computing device, such as a computer, so that the resistivity can be calculated, and further the conductivity of the region to be measured can be calculated. The specific calculation principle can be seen from the description of the conductivity measurement principle in the above embodiments.
After the electrical conductivity measurement is completed, the temperature, the thermal conductivity and the seebeck coefficient can be measured, and in particular, the measurement steps shown in fig. 7 can be referred to:
and S21, determining a region to be detected in the sample to be detected.
And S22, controlling the X-Y two-axis moving platform to move the area to be detected to the orthographic projection area of the four-probe assembly.
And S23, adopting a first laser beam to be incident to the area to be tested so as to heat the area to be tested.
S24, when the first laser beam heats the area to be measured for a preset duration, the second laser beam is incident to the area to be measured so as to measure the heat reflectivity and the heat reflectivity change rate of the area to be measured;
s25, when the second laser beam is incident to the area to be measured, controlling the Z-axis moving platform to face the area to be measured, and enabling the four-probe assembly to contact the area to be measured so as to measure the voltage difference caused by the temperature change of the area to be measured;
and S26, controlling the Z-axis moving platform to be far away from the sample to be detected.
And S27, judging whether the measurement of the thermal conductivity and the Seebeck coefficient of all the regions to be measured is finished or not, and if the measurement of all the regions to be measured is finished, entering the step S28. If the measurement of all the areas is not completed, the process returns to step S21.
S28, ending the measurement.
When the thermal conductivity is measured, the area to be measured is heated through the first laser beam, the heated area to be measured is tested through the second laser beam, reflected light is obtained, the second laser beam reflected by the area to be measured is received through the photoelectric detector, the thermal reflectivity signal is converted into an electric signal, the electric signal is input into a computing device, for example, a computer, and the thermal conductivity can be calculated. After the first laser beam heats the area to be measured, the probe is adopted to measure the change of the voltage difference along with the temperature change, and the change data of the voltage difference and the temperature change data are input into the value calculation device for fitting to obtain the Seebeck coefficient. The specific calculation principle can be seen from the description of the measurement principle of the thermal conductivity and the seebeck coefficient in the above embodiment.
The four-probe assembly for measuring the Seebeck coefficient and the electric conductivity is integrated into a dual-wavelength femtosecond pulse laser heat reflection measurement system to form a complete thermoelectric material thermoelectric transport parameter measurement system, so that the measurement targets of the heat conductivity, the electric conductivity and the Seebeck coefficient are completed on one device, and the measurement efficiency is improved; on the other hand, the system is used for researching the ultra-fast thermoelectric process of the material, and important experimental data are provided for the research and development of a novel material of the thermoelectric material and the performance optimization.
Although the embodiments of the present invention have been described in conjunction with the accompanying drawings, those skilled in the art may make various modifications and variations without departing from the spirit and scope of the invention, and such modifications and variations fall within the scope defined by the appended claims.
Claims (9)
1. A high throughput measurement system for a thermoelectric transport parameter, the thermoelectric transport parameter comprising: electrical conductivity, seebeck coefficient and thermal conductivity, characterized in that it comprises:
the system comprises a three-dimensional platform and a control system, wherein the three-dimensional platform is provided with an X-Y two-axis moving platform for placing a sample to be detected and a Z-axis moving platform provided with a four-probe assembly, and the four-probe assembly is used for measuring the conductivity and the Seebeck coefficient of a region to be detected of the sample to be detected;
the heat reflection measuring device is used for dividing the pulse laser into a first laser beam and a second laser beam with preset optical path difference, the first laser beam is used for heating a region to be measured of the sample to be measured, and the second laser beam is used for measuring the heat conductivity of the region to be measured of the sample to be measured;
the first laser beam is simultaneously used as a heat source for measuring the Seebeck coefficient by a four-probe group.
2. The thermoelectric transport parameter high throughput measurement system of claim 1, wherein the second laser beam is used to measure the thermal reflectivity and the rate of change of thermal reflectivity of the area under test.
3. A thermoelectric transport parameter high throughput measurement system as recited in claim 2, further comprising:
and the synchronous signal triggering device is used for triggering the three-dimensional platform when the second laser beam reaches the surface of the sample to be measured, and moving the four-probe assembly to the area irradiated by the second laser beam so as to measure the voltage difference caused by the temperature change of the area to be measured.
4. A thermoelectric transport parameter high throughput measurement system as recited in claim 3, further comprising:
the data acquisition device is used for acquiring the voltage difference, the heat reflectivity and the change rate of the heat reflectivity;
the calculating device is connected with the data acquisition device and used for calculating the temperature distribution of the region to be measured according to the heat reflectivity change rate and calculating the heat conductivity of the region to be measured based on a preset mathematical model;
and the calculating device is also used for calculating the Seebeck coefficient of the area to be measured according to the calculated temperature and the voltage difference.
5. A thermoelectric transport parameter high throughput measurement system as recited in claim 4, wherein said data acquisition device comprises:
the photoelectric detector is used for receiving the second laser beam reflected by the area to be detected, converting the thermal reflectivity into an electric signal and inputting the electric signal into the computing device;
and the electrical parameter collector is used for collecting the voltage difference and the conductivity and inputting the voltage difference and the conductivity into the computing device.
6. The high-throughput measurement system for thermoelectric transport parameters according to any one of claims 1-5, wherein the sample to be measured comprises a plurality of areas to be measured, and the areas to be measured are switched by the movement of the X-Y two-axis moving platform.
7. A method for high-throughput measurement of a thermoelectric transport parameter, wherein the thermoelectric transport parameter of a sample to be measured is measured by using the thermoelectric transport parameter high-throughput measurement system as claimed in any one of claims 1 to 6, the method comprising:
s1, controlling the movement of the X-Y axis moving platform and the Z axis moving platform, and measuring the conductivity of a sample to be measured by adopting a four-probe assembly;
s2, heating the sample to be measured by adopting a first laser beam, detecting the heat conductivity of the heated area by adopting a second laser beam, and moving the Z-axis moving platform to enable the four-probe assembly to contact the heated area so as to measure the Seebeck coefficient.
8. The method for high throughput measurement of thermoelectric transport parameters of claim 7, wherein the sample under test comprises a plurality of regions under test;
the control the removal of X-Y diaxon moving platform and Z axle moving platform, adopt four probe assembly to measure the conductivity of the sample that awaits measuring includes:
s11, determining a region to be detected in a sample to be detected;
s12, controlling an X-Y two-axis moving platform to move the area to be detected to the orthographic projection area of the four-probe assembly;
s13, controlling the Z-axis moving platform to move towards the sample to be detected, enabling the four-probe assembly to contact a region to be detected of the sample to be detected, and measuring the conductivity of the contacted region to be detected;
s14, controlling the Z-axis moving platform to be far away from the sample to be measured, and repeating the steps S11-S13 until conductivity measurement of all areas to be measured is completed.
9. The method of claim 7, wherein the measuring the seebeck coefficient comprises the steps of heating the sample to be measured by a first laser beam, detecting the thermal conductivity of the heated area by a second laser beam, and moving the Z-axis moving platform to enable the four-probe assembly to contact the heated area, wherein the measuring the seebeck coefficient comprises the steps of:
s21, determining a region to be detected in a sample to be detected;
s22, controlling an X-Y two-axis moving platform to move the area to be detected to the orthographic projection area of the four-probe assembly;
s23, adopting a first laser beam to enter the area to be tested so as to heat the area to be tested;
s24, when the first laser beam heats the area to be measured for a preset time, a second laser beam is incident to the area to be measured so as to measure the heat reflectivity and the temperature of the area to be measured;
s25, when the second laser beam is incident to the area to be measured, controlling the Z-axis moving platform to face the area to be measured, and enabling the four-probe assembly to be in contact with the area to be measured so as to measure a voltage difference caused by temperature change of the area to be measured;
s26, controlling the Z-axis moving platform to be far away from the sample to be measured, and repeating the steps S21-S25 until the measurement of the thermal conductivity and the Seebeck coefficient of all the regions to be measured is completed.
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| CN111948250B (en) * | 2020-08-13 | 2023-01-13 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN112268860A (en) * | 2020-10-24 | 2021-01-26 | 江苏明盈科技有限公司 | Dual-wavelength femtosecond pumping detection heat reflection system |
| CN112268861A (en) * | 2020-10-24 | 2021-01-26 | 江苏明盈科技有限公司 | Dual-wavelength femtosecond pumping detection heat reflection system |
| CN115436709B (en) * | 2022-09-22 | 2023-05-30 | 厦门大学 | Movable high-temperature conductivity measurement clamp, system and method |
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