CN109613051A - A kind of device and method using method of comparison measurement material Seebeck coefficient - Google Patents

A kind of device and method using method of comparison measurement material Seebeck coefficient Download PDF

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CN109613051A
CN109613051A CN201811242049.2A CN201811242049A CN109613051A CN 109613051 A CN109613051 A CN 109613051A CN 201811242049 A CN201811242049 A CN 201811242049A CN 109613051 A CN109613051 A CN 109613051A
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sample
test
seebeck coefficient
equation
fixture
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CN109613051B (en
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缪向水
林凯明
张军
陈子琪
童浩
王愿兵
蔡颖锐
聂群
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WUHAN SCHWAB INSTRUMENT TECHNOLOGY Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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Abstract

The present invention relates to a kind of devices using method of comparison measurement material Seebeck coefficient, device includes sample stage, heating power supply, data acquisition device, the sample stage includes fixture, fixture includes lower fixture and upper fixture, sample includes standard sample and test sample, standard sample and test sample are sandwiched between lower fixture and upper fixture, are equipped with heating rod in lower fixture.The present invention passes through the comparison of test sample and standard sample, the Seebeck coefficient of measurement material indirectly, facilitate comparison with direct measurement, avoid the problem of sample both ends temperature measurement inaccuracy, temperature measurement inaccuracy is maximum error source in the measurement of Seebeck coefficient, and the system only needs to measure the potential difference of test sample and standard sample both ends, because not needing measurement sample two sides temperature, greatly reduce the signal lead in system, keep system simpler effectively, it is contacted simultaneously using graphite electrode and sample, the problem of avoiding thermoelectricity thermogalvanic corrision in test process.

Description

A kind of device and method using method of comparison measurement material Seebeck coefficient
Technical field
The present invention relates to thermoelectric semiconductor material performance sample stages, in particular to a kind of to measure material using method of comparison The device and method of Seebeck coefficient.
Background technique
Seebeck coefficient is the intrinsic heat electrical properties of material, is mainly used for making using the thermoelectric material of Seebeck effect The temperature sensors such as thermocouple, thermoelectric generation film and semiconductor chilling plate accurately measure thermoelectric material at different temperatures Seebeck coefficient value has important meaning to the research and application of thermoelectric material.
Existing measuring device and mode are as follows: test sample is clamped between sample stage, passes through thermocouple probe A and B It is directly contacted with sample both ends, thus the potential difference between the temperature and probe A and B of two contact points of measurement.
In the Seebeck coefficient that material is calculated according to the formula for solving Seebeck coefficient, measurement in this way can exist such as Lower Railway Project:
(1) thermocouple is directly and sample surfaces contact measurement sample surface temperature can have large error, and existing Test device, temperature measurement inaccuracy are maximum error sources in the measurement of Seebeck coefficient;
(2) corrosion reaction can occur at high temperature for thermocouple and sample, make thermocouple failure can not retest.
Summary of the invention
In order to solve the above technical problems, providing a kind of device and method using method of comparison measurement material Seebeck coefficient.
As the first aspect of the present invention, a kind of device using method of comparison measurement material Seebeck coefficient is provided, including Sample stage, heating power supply, data acquisition device, the sample stage include fixture, and the fixture has there are two sample test position, In sample test position for placing standard sample, another sample test position is for placing test sample, the fixture packet Lower fixture and upper fixture are included, the standard sample and test sample are sandwiched between lower fixture and upper fixture, in the lower fixture Heating rod is installed;
The heating power supply is used to power to heating rod;
The heating rod is used for the heating one end contacted to standard sample and test sample with lower fixture;
The data acquisition module is used to acquire the potential difference of standard sample and test sample both ends.
Further, it is provided with graphite electrode on the contact surface of the upper fixture and lower fixture and sample, institute State between upper fixture and graphite electrode and be provided between the lower fixture and graphite electrode thermally conductive sheet, the heating rod with Thermally conductive sheet contact, the thermally conductive sheet are contacted with graphite electrode;
The heating rod transfers heat to the graphite electrode of lower chucking surface by thermally conductive sheet, then under passing through
The graphite electrode of chucking surface gives the standard sample being in contact with it and test sample heating.
It further, further include temperature control device, infrared heating furnace, the infrared heating furnace has closed chamber, described Sample stage is placed in the chamber of the infrared heating furnace, and the temperature control device is electrically connected with the infrared heating furnace, for pair The temperature of infrared heating furnace is controlled.
Further, the temperature control device includes PID controller and power regulator, is provided in the infrared heating furnace For detecting the temperature sensor of the chamber room temperature, the PID controller and the infrared heating furnace with the power Adjuster electrical connection, the temperature sensor are electrically connected with the PID controller.
Further, it is additionally provided on the infrared heating furnace and vacuumizes envelope mouth, the pumping for what is be controlled to a vacuum pump Vacuum seal mouth is communicated in the chamber by pipeline.
Further, the data acquisition device includes first voltage test table and second voltage test table, and described first Voltage tester table is used to measure the potential difference at the standard sample both ends, and the second voltage test table is for measuring the test The potential difference at sample both ends.
Further, further include host computer, the data acquisition device, temperature control device with the upper mechatronics.
As another aspect of the present invention, a kind of method using method of comparison measurement material Seebeck coefficient is provided, is used It is above-mentioned it is any as described in device, the described method comprises the following steps:
Step 1, it is heated for the one end of heating rod to standard sample and test sample, to standard sample and test specimens After the both ends of product have reached identical temperature difference, pass through the potential of data acquisition module measurement standard sample and test sample both ends Difference;
Step 2, the potential difference of according to standard sample and test sample both ends, establish standard sample Seebeck equation and The Seebeck equation of test sample, the Seebeck equation of according to standard sample and the Seebeck equation solution of test sample go out The absolute Seebeck coefficient value of test sample.
Further, the step 2 specifically:
If the potential difference at standard sample both ends is VCu_S, the potential difference at test sample both ends is VCu_T, get standard samples The Seebeck equation of Seebeck equation and test sample is expressed as following equation (1) and equation (2):
Equation (1): VCu_T=(SCu-ST) Δ T,
Equation (2): VCu_T=(SCu-ST) Δ T,
Wherein SCuThe absolute Seebeck coefficient value of connecting wire between sample and data acquisition module, Δ T are standard The temperature difference of sample and test sample both ends, SSFor the absolute Seebeck coefficient value of standard sample, STFor the absolute of test sample Seebeck coefficient value;
Equation (1) and equation (2) simultaneous are obtained into equation (3), are expressed as follows:
Equation (3):
The absolute Seebeck coefficient value that test sample is finally obtained according to equation (3), is expressed as follows:
Beneficial effects of the present invention:
Patent of the invention passes through the comparison of test sample and standard sample, measures the Seebeck coefficient of material indirectly, and Directly measurement facilitates comparison, avoids the problem of sample both ends temperature measurement inaccuracy, it is Seebeck coefficient that temperature, which measures inaccuracy, Maximum error source in measurement, and the system only needs to measure the potential difference of test sample and standard sample both ends, Because not needing measurement sample two sides temperature, the signal lead in system is greatly reduced, keeps system simpler effectively.Simultaneously The problem of being contacted using graphite electrode and sample, avoiding thermoelectricity thermogalvanic corrision in test process.
Detailed description of the invention
Fig. 1 is for the structure chart of the device provided in an embodiment of the present invention for measuring material Seebeck coefficient using method of comparison Schematic diagram;
Fig. 2 is the structural schematic diagram of sample stage provided in an embodiment of the present invention;
Fig. 3 is the apparatus structure schematic diagram of the measurement material Seebeck coefficient of the prior art.
Description of symbols: 1, lower fixture, 2, upper fixture, 3, standard sample, 4, test sample, 5 heating rods, 6, thermally conductive Piece, 7, graphite electrode.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiment is only present invention a part, instead of all the embodiments.Based on the present invention In embodiment, all other implementation obtained by those of ordinary skill in the art without making creative efforts Example, shall fall within the protection scope of the present invention.
As Figure 1-Figure 2, it as the first embodiment of the present invention, provides a kind of using method of comparison measurement material The device of Seebeck coefficient, including sample stage, heating power supply, data acquisition device, the sample stage include fixture, the folder Tool tool is there are two sample test position, and for placing standard sample, another sample test position is used for for one of sample test position Place test sample, the fixture includes lower fixture and upper fixture, the standard sample and test sample be sandwiched in lower fixture and Between upper fixture, heating rod is installed in the lower fixture.
The heating power supply is used to power to heating rod.
The heating rod is used for the heating one end contacted to standard sample and test sample with lower fixture.
The data acquisition module is used to acquire the potential difference of standard sample and test sample both ends.
Preferably, to guarantee good thermo-contact, the upper fixture of sample is using intermediate rotatable mechanism, when fixture and sample When product clamp, intermediary agency's adjustable angle guarantees that there is good thermo-contact in the upper surface of fixture and two samples.
Preferably, graphite electrode, the upper folder are provided on the contact surface of the upper fixture and lower fixture and sample Thermally conductive sheet, the heating rod and thermally conductive sheet are provided between tool and graphite electrode and between the lower fixture and graphite electrode Contact, the thermally conductive sheet are contacted with graphite electrode.
The heating rod transfers heat to the graphite electrode of lower chucking surface by thermally conductive sheet, then passes through lower chucking surface Graphite electrode give the standard sample that is in contact with it and test sample heating.
In above-described embodiment, what sample stage design neutralization sample directly contacted is graphite electrode, because graphite electrode respectively connects The temperature of contact is almost the same, therefore can ignore their influences to thermoelectrical potential total in circuit, wherein the thermally conductive sheet is preferably adopted It more ensure that with diamond since the cold and hot both ends of sample clamp use the composite material of diamond and high thermal conductive metallic The exit of Seebeck voltage signal is consistent with the hot and cold side temperature of fixture.
It preferably, further include temperature control device, infrared heating furnace, the infrared heating furnace has closed chamber, the sample Sample platform is placed in the chamber of the infrared heating furnace, and the temperature control device is electrically connected with the infrared heating furnace, for red The temperature of externally heated oven is controlled.
Preferably, which is characterized in that the temperature control device includes PID controller and power regulator, the infrared heating The temperature sensor for detecting the chamber room temperature is provided in furnace, the PID controller and the infrared heating furnace are equal It is electrically connected with the power regulator, the temperature sensor is electrically connected with the PID controller.
In above-described embodiment, the power output of power regulator is controlled by PID controller, can accurately be controlled infrared The temperature of heating furnace.
Preferably, it is additionally provided on the infrared heating furnace and vacuumizes envelope mouth for what is be controlled to a vacuum pump, the pumping is true Sky envelope mouth is communicated in the chamber by pipeline.
In above-described embodiment, entire contrast test sample stage is placed in the varying temperature environment of infrared heating furnace, when test Envelope mouth will be vacuumized to be controlled to a vacuum pump, cavity will be vacuumized, to guarantee that sample temperature is unanimously and not oxidized, on sample stage Various signal wires are drawn out in external data acquisition device by vacuum sealing plug and are measured.
Preferably, the data acquisition device includes first voltage test table and second voltage test table, first electricity Pressure test table is used to measure the potential difference at the standard sample both ends, and the second voltage test table is for measuring the test specimens The potential difference at product both ends.
Preferably, described device further includes host computer, the data acquisition device, temperature control device with the upper electromechanics Connection, the temperature control device and data acquisition device for controlling infrared heating furnace can pass through computer software all with host computer compunlcation It is operated.
Wherein, the present invention is carried out according to the difference of the Seebeck coefficient magnitude of test sample using different standard samples Contrast test, specifically, standard sample uses metallic thermocouple material health for the test sample of lesser Seebeck coefficient Copper, thermocouple is the most important purposes of thermoelectric material, therefore has standard at different temperatures for metallic thermocouple material Seebeck coefficient can be consulted, and metallic thermocouple material property is stablized, can repeated measurement, be that standard specimen is most as a comparison Good selection;For the semiconductor test sample of higher Seebeck coefficient, standard sample uses semiconductor silicon germanium alloy, and SiGe closes Golden high temperature resistant, and performance is stablized, it is comparatively ideal right that Seebeck coefficient is varied with temperature to be changed between (100-300) uV/K Than standard specimen, the standard sample in the embodiment of the present invention uses metallic thermocouple material constantan, the connection of voltage tester table and sample By fine copper conducting wire, the absolute Seebeck coefficient value of the fine copper conducting wire is also known.
In above-described embodiment, by the comparison of test sample and standard sample, the Seebeck coefficient of material is measured indirectly, Facilitate comparison with direct measurement, avoids the problem of sample both ends temperature measurement inaccuracy, it is Seebeck system that temperature, which measures inaccuracy, Maximum error source in number measurement, and the system only needs to measure the potential difference at test sample and standard sample both ends i.e. Can, because not needing measurement sample two sides temperature, the signal lead in system is greatly reduced, keeps system simpler effectively. The problem of being contacted simultaneously using graphite electrode and sample, avoiding thermoelectricity thermogalvanic corrision in test process.
As the second embodiment of the present invention, a kind of method using method of comparison measurement material Seebeck coefficient, institute are provided Method is stated using the device of any of the above-described kind of measurement material Seebeck coefficient, the described method comprises the following steps:
Step 1, it is heated for the one end of heating rod to standard sample and test sample, to standard sample and test specimens After the both ends of product have reached identical temperature difference, pass through the potential of data acquisition module measurement standard sample and test sample both ends Difference;
Step 2, the potential difference of according to standard sample and test sample both ends, establish standard sample Seebeck equation and The Seebeck equation of test sample, the Seebeck equation of according to standard sample and the Seebeck equation solution of test sample go out The absolute Seebeck coefficient value of test sample.
In above-described embodiment, Seebeck coefficient test when using the heating rod in the fixture of lower end be sample heating one end, After the time of one end and it can reach thermal balance, because the both ends of the high-termal conductivity of fixture, standard specimen and sample can reach identical temperature Difference.
Preferably, the step 2 specifically:
If the potential difference at standard sample both ends is VCu_S, the potential difference at test sample both ends is VCu_T, get standard samples The Seebeck equation of Seebeck equation and test sample is expressed as following equation (1) and equation (2):
Equation (1): VCu_T=(SCu-ST)ΔT。
Equation (2): VCu_T=(SCu-ST)ΔT。
Wherein SCuThe absolute Seebeck coefficient value of connecting wire between sample and data acquisition module, Δ T are standard The temperature difference of sample and test sample both ends, SSFor the absolute Seebeck coefficient value of standard sample, STFor the absolute of test sample Seebeck coefficient value.
Equation (1) and equation (2) simultaneous are obtained into equation (3), are expressed as follows:
Equation (3):
The absolute Seebeck coefficient value that test sample is finally obtained according to equation (3), is expressed as equation (4):
Equation (4):
In above-described embodiment, according to equation (4), which only needs to measure the electricity of standard sample and test sample both ends The absolute Seebeck coefficient of sample can be calculated in pressure, therefore data collection terminal only acquires two voltage values.
In specific measurement, in order to reduce test error, the heating electricity in data acquisition device in control figure 2 can be passed through The potential difference of the watt level in source, the temperature difference T of change sample upper and lower ends, standard sample and test sample should be in multiple groups temperature Repeatedly measurement acquires average value under poor Δ T.
In addition, the test device including entire sample stage is placed in the varying temperature environment in infrared heating furnace, time control is measured Infrared heating furnace processed reaches different environment temperatures, is then measured by test device.Finally by the survey under different temperatures The Seebeck coefficient value of test agent summarizes, so that it may which obtain that the absolute Seebeck coefficient value of test sample varies with temperature becomes Power curve, to guarantee that it is uniform with temperature that sample does not aoxidize at high temperature, vacuumize process inside infra-red furnace, the control of infrared heating furnace System part is connected by communication line with host computer with data acquisition device, and realizes coordinated control, is realized in upper computer software In the automatic operation of whole system, use simple and convenient.
Fig. 3 is the test device of the prior art, as shown in figure 3, in the prior art, only test sample is individually tested, sample Product are clamped between sample stage, and thermocouple probe A and B and sample directly contact, thus the temperature of two contact points of measurement, and Potential difference between probe A and B.
The Seebeck coefficient of material is calculated according to the following formula:
Wherein, S is the Seebeck coefficient of test sample material, VA-VBFor the potential difference at test sample both ends, TA-TBFor The temperature difference at test sample both ends both ends, in this way measurement can have following Railway Project:
(1) thermocouple is directly and sample surfaces contact measurement sample surface temperature can have large error, and existing Test device, temperature measurement inaccuracy are maximum error sources in the measurement of Seebeck coefficient.
(2) corrosion reaction can occur at high temperature for thermocouple and sample, make thermocouple failure can not retest.
And the invention patent passes through the comparison of test sample and standard sample, measures the Seebeck coefficient of material indirectly, and Directly measurement facilitates comparison, avoids the problem of sample both ends temperature measurement inaccuracy, it is Seebeck coefficient that temperature, which measures inaccuracy, Maximum error source in measurement, and the system only needs to measure the potential difference of test sample and standard sample both ends, Because not needing measurement sample two sides temperature, the signal lead in system is greatly reduced, keeps system simpler effectively.Simultaneously The problem of being contacted using graphite electrode and sample, avoiding thermoelectricity thermogalvanic corrision in test process.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (9)

1. it is a kind of using method of comparison measurement material Seebeck coefficient device, which is characterized in that including sample stage, heating power supply, Data acquisition device, the sample stage include fixture, and there are two sample test position, one of sample test positions for the fixture tool For placing standard sample, for placing test sample, the fixture includes lower fixture and upper fixture for another sample test position, The standard sample and test sample are sandwiched between lower fixture and upper fixture, are equipped with heating rod in the lower fixture;
The heating power supply is used to power to heating rod;
The heating rod is used for the heating one end contacted to standard sample and test sample with lower fixture;
The data acquisition module is used to acquire the potential difference of standard sample and test sample both ends.
2. the device according to claim 1 using method of comparison measurement material Seebeck coefficient, which is characterized in that described It is provided with graphite electrode on the contact surface of the upper fixture and lower fixture and sample, between the upper fixture and graphite electrode And thermally conductive sheet is provided between the lower fixture and graphite electrode, the heating rod is contacted with thermally conductive sheet, the thermally conductive sheet It is contacted with graphite electrode;
The heating rod transfers heat to the graphite electrode of lower chucking surface, then the stone by lower chucking surface by thermally conductive sheet Electrode ink gives the standard sample being in contact with it and test sample heating.
3. the device according to claim 1 using method of comparison measurement material Seebeck coefficient, which is characterized in that also wrap Include temperature control device, infrared heating furnace, the infrared heating furnace has a closed chamber, the sample stage be placed in it is described infrared plus In the chamber of hot stove, the temperature control device is electrically connected with the infrared heating furnace, is controlled for the temperature to infrared heating furnace System.
4. the device according to claim 3 using method of comparison measurement material Seebeck coefficient, which is characterized in that described Temperature control device includes PID controller and power regulator, is provided in the infrared heating furnace for detecting the chamber Indoor Temperature The temperature sensor of degree, the PID controller and the infrared heating furnace are electrically connected with the power regulator, the temperature Sensor is electrically connected with the PID controller.
5. the device according to claim 4 using method of comparison measurement material Seebeck coefficient, which is characterized in that described It is additionally provided on infrared heating furnace and vacuumizes envelope mouth for what is be controlled to a vacuum pump, the envelope mouth that vacuumizes is communicated to by pipeline In the chamber.
6. the device according to claim 1 using method of comparison measurement material Seebeck coefficient, which is characterized in that described Data acquisition device includes first voltage test table and second voltage test table, and the first voltage test table is described for measuring The potential difference at standard sample both ends, the second voltage test table are used to measure the potential difference at the test sample both ends.
7. the device according to claim 3 using method of comparison measurement material Seebeck coefficient, which is characterized in that also wrap Include host computer, the data acquisition device, temperature control device with the upper mechatronics.
8. a kind of method using method of comparison measurement material Seebeck coefficient, which is characterized in that appointed using such as claim 1-7 Device described in one, the described method comprises the following steps:
Step 1, it is heated for the one end of heating rod to standard sample and test sample, to standard sample and test sample After both ends have reached identical temperature difference, pass through the potential difference of data acquisition module measurement standard sample and test sample both ends;
Step 2, the potential difference of according to standard sample and test sample both ends establishes Seebeck equation and the test of standard sample The Seebeck equation of sample, the Seebeck equation of according to standard sample and the Seebeck equation solution of test sample go out to test The absolute Seebeck coefficient value of sample.
9. the method for method of comparison measurement material Seebeck coefficient according to claim 7, which is characterized in that the step 2 Specifically:
If the potential difference at standard sample both ends is VCu_S, the potential difference at test sample both ends is VCu_T, get standard samples The Seebeck equation of Seebeck equation and test sample is expressed as following equation (1) and equation (2):
Equation (1): VCu_T=(SCu-ST) Δ T,
Equation (2): VCu_T=(SCu-ST) Δ T,
Wherein SCuThe absolute Seebeck coefficient value of connecting wire between sample and data acquisition module, Δ T are standard sample With the temperature difference at test sample both ends, SSFor the absolute Seebeck coefficient value of standard sample, STFor the absolute of test sample Seebeck coefficient value;
Equation (1) and equation (2) simultaneous are obtained into equation (3), are expressed as follows:
Equation (3):
The absolute Seebeck coefficient value that test sample is finally obtained according to equation (3), is expressed as follows:
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Denomination of invention: A device and method for measuring Seebeck coefficient of materials using comparative method

Granted publication date: 20210817

Pledgee: Guanggu Branch of Wuhan Rural Commercial Bank Co.,Ltd.

Pledgor: WUHAN JOULE YACHT SCIENCE & TECHNOLOGY Co.,Ltd.

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