CN101413908B - System and method for testing thin film thermoelectricity material Seebeck coefficient - Google Patents

System and method for testing thin film thermoelectricity material Seebeck coefficient Download PDF

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CN101413908B
CN101413908B CN 200810153534 CN200810153534A CN101413908B CN 101413908 B CN101413908 B CN 101413908B CN 200810153534 CN200810153534 CN 200810153534 CN 200810153534 A CN200810153534 A CN 200810153534A CN 101413908 B CN101413908 B CN 101413908B
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threeway
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CN101413908A (en
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王为
李菲晖
李晋楼
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Tianjin University
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Tianjin University
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Abstract

The invention relates to a system used for testing Seebeck coefficient of film thermoelectric material and a method thereof. The system comprises a testing device and a control and test circuit system; the sample to be tested is arranged on an insulative sheet on a sample supporting frame and closely contacts with two thermocouples used for measuring the temperature of the sample by a sample fixed clamp; temperature difference is established in the sample to be tested by an electric heating block which is arranged at one side of the sample to be tested; furthermore, the temperature of the film thermoelectric material at the position where the thermocouple is arranged is measured by the two thermocouples which are used for measuring the temperature of the sample and intermittently distributed along the temperature difference direction; the Seebeck electromotive force generated by the sample inside the film thermoelectric material at the position where the thermocouple is arranged is measured by the Seebeck electromotive force measuring line educed by one of two leads which are respectively arranged in the two thermocouples used for measuring the temperature of the sample. The structure used for testing Seebeck coefficient of the film thermoelectric material and the method thereof can quickly and exactly measure the Seebeck coefficient of the film thermoelectric material and solve the problem that the Seebeck coefficient of the film thermoelectric material can not be measured at present.

Description

Thin film thermoelectricity material Seebeck coefficient test macro and method
Technical field
The present invention relates to thermoelectric material Performance Testing Technology in material science, particularly a kind of thin film thermoelectricity material Seebeck (Seebeck) coefficient test macro and method.
Background technology
Thermoelectric material is a kind of functional material that can realize mutual conversion between heat energy and electric energy, has widespread use aspect thermo-electric generation, refrigeration and sensor.The Seebeck coefficient is the important indicator of estimating the thermoelectric material performance.The Seebeck Coefficient Definition is as follows: when there is temperature difference T=T in thermoelectric material two ends 1-T 2, and T 1T 2The time, have a potential difference (PD) E at the two ends of thermoelectric material abOccur, its numerical value is:
E ab=α abΔT (1)
(1) α in formula abBe constant, this constant is called as the Seebeck coefficient of thermoelectric material.
Present business-like thermoelectric material Seebeck coefficient tester all designs and makes for the block thermoelectric material, still is not applicable to the instrument of thin-film thermoelectric material Seebeck coefficient test.
This patent has proposed a kind of test macro and structure thereof that is specifically designed to the test of thin-film thermoelectric material Seebeck coefficient.
Summary of the invention
The present invention proposes a kind of test macro that is specifically designed to thin-film thermoelectric material Seebeck coefficient test, this system is made of proving installation and control and test circuit system two parts.Thin-film thermoelectric material sample to be measured is placed in proving installation, and proving installation can move in atmospheric environment, also can move in airtight vacuum environment or in protective atmosphere.Control and the test circuit system is used for the temperature of the inner sample to be tested of regulation and control proving installation and surrounding environment thereof and keeps temperature constant, realization is to the control of proving installation close beta process and the collection of test data, and test data is transferred to microcomputer, realize the control to whole test system and test process, the processing of test data and the real-time demonstration of test data by microcomputer.This system can realize the accurate measurement to thin-film thermoelectric material Seebeck coefficient.
The test macro of a kind of thin-film thermoelectric material Seebeck coefficient test of the present invention comprises proving installation and control and test circuit system; Proving installation by sample support frame outer cover 1, sample support frame 2, heat block 3, sample to be tested 4, insulating trip 5, sample fixed card 6, sample fixed card gib screw 34, sample temperature thermocouple 7, sample chamber temperature thermocouple 8, sealing clamp 9, outer lead interface 10, connect outer lead threeway 11, sample support frame connectivity port 22, sample chamber well heater 23, O-ring seal 24, threeway gland bonnet 35 and form; The inside that it is characterized in that sample support frame outer cover 1 forms the sample chamber of placing sample to be tested; Sample to be tested 4 is held in place on insulating trip 5 on sample support frame 2, and by sample fixed card 6 respectively with two sample temperature thermocouple 7 close contacts; Set up the temperature difference by the electrical heating piece 3 that is positioned at sample to be tested one side in the inside of sample to be tested 4, and by with sample to be tested 4 close contacts and temperature record two sample temperature thermocouples, 7 positions places thin-film thermoelectric materials along two sample temperature thermocouples 7 that temperature difference direction is intervally distributed with, respectively by means of by each the Seebeck electro-motive force measurement line 28 that wire is drawn in these two sample temperature thermocouples 7, record sample at these two temperature thermocouples, 7 inner Seebeck electromotive force that produce of place, position thin-film thermoelectric material simultaneously; Control and the test circuit system is: sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27 and Seebeck electro-motive force measurement line 28 all extend proving installation by being arranged on the outer lead interface 10 that connects in outer lead threeway 11.Sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27, the Seebeck electro-motive force measurement line 28 that is connected by the sample temperature thermocouple 7 in proving installation, sample chamber temperature thermocouple 8, electrical heating piece 3 and sample chamber well heater 23 and sample chamber heater power lead 29 is connected respectively to or first control and data collector 30 through being connected to after ice-water bath 31; Control and data collector 30 are comprised of A/D converter, single-chip microcomputer, serial ports conversion, power supply, the electronic circuit that carries out signal transmission and signal processing, pushbutton switch etc.; Control and data collector 30 are connected on microcomputer 33 by data line 32; Processed by the data that 33 pairs of microcomputers are controlled and data collector 30 collects, and show in real time data processed result on the display of microcomputer 33.
The present invention is according to the temperature difference T=T of thermoelectric material two ends existence 1-T 2, and T 1T 2The time, have a potential difference (PD) E at the two ends of thermoelectric material abOccur, its numerical value is:
E ab=α abΔT (1)
(1) α in formula abBe constant, this constant is called as the Seebeck coefficient of thermoelectric material.Seebeck coefficient calculations principle according to (1) formula, work out out control and data processing software according to the flow chart of Fig. 4: open testing software and begin test, the right button of clicking the mouse, jump out a dialog box, select " opening serial ports ", begin to gather the Seebeck electromotive force that the voltage signal that represents sample cold junction and hot-side temperature and sample produce under this temperature difference, by program, the voltage signal of the representation temperature that collects is converted into its corresponding temperature value, and calculates the temperature difference.The temperature difference that utilization collects and electromotive force calculate corresponding Seebeck coefficient, and demonstrate in real time Seebeck coefficient and Seebeck electromotive force-temperature difference fitting a straight line equation on the display of microcomputer 33.After test was completed, the right button of clicking the mouse ejected a dialog box, clicked " time-out " to stop data acquisition, if finish test after preserving test result, withdrawed from test interface; If need to continue test, after click " time-out " stops data acquisition and preserves test result, click " emptying " to remove last test result, then click " beginning " to carry out the test of next sample.
The test macro of thin-film thermoelectric material Seebeck coefficient of the present invention test can be according to different requirements, carry out test under corresponding conditions by join dependency external unit in system.
Under at vacuum condition, the Seebeck coefficient of thin-film thermoelectric material is tested, the threeway gland bonnet 35 in Fig. 1 test macro can be removed, by sealing clamp 9 with connect pressure meter three-way 13 be connected (Fig. 5, Fig. 6).Connect the tensimeter 12 of installing on pressure meter three-way and be used for demonstration with the pressure of vacuum system proving installation inside.Connect thermocouple vacuum gauge threeway 15 by sealing clamp 9 with connect pressure meter three-way 13 and be connected, the thermocouple vacuum gauge 14 of installing on it is used for showing the vacuum tightness with vacuum system proving installation inside.Connect vacuum pump threeway 18 by sealing clamp 9 with connect thermocouple vacuum gauge threeway 15 and be connected, the manual vacuum valve 16 of installing on it is used for the vacuum tightness of accommodation zone vacuum system proving installation inside, and the vacuum pump interface 17 that is connected on manual vacuum valve 16 by sealing clamp 9 is used for being connected with vacuum pump by external pipeline.Connect air release threeway 20 by sealing clamp 9 with connect vacuum pump threeway 18 and be connected, the air release 19 of installing on it is used for the gaseous tension of accommodation zone vacuum system proving installation inside.
Test as the Seebeck coefficient to thin-film thermoelectric material under the blanket gas condition; threeway gland bonnet 35 in band vacuum test system (Fig. 5, Fig. 6) can be removed, (Fig. 7, Fig. 8) is connected with manual vacuum valve 16 by sealing clamp 9.The blanket gas interface 21 that is connected on manual vacuum valve 16 by sealing clamp 9 is used for being connected to outer protection gas by external pipeline; it is inner that blanket gas can enter band blanket gas proving installation by blanket gas interface 21; regulate amount and the pressure thereof that enters with the blanket gas of blanket gas proving installation inside by manual vacuum valve 16, by tensimeter 12 and the thermocouple vacuum gauge 14 monitoring pressure with blanket gas proving installation inside.
Adopt structure and the method for thin-film thermoelectric material Seebeck coefficient test macro of the present invention, can measure rapidly and accurately the Seebeck coefficient of thin-film thermoelectric material, solved the problem that current thin film thermoelectric material Seebeck coefficient can't be measured.
Description of drawings
Accompanying drawing 1 proving installation structural representation;
Accompanying drawing 2 proving installation structure partial cut-open views;
Circuit connection diagram between accompanying drawing 3 thin-film thermoelectric material Seebeck coefficient test macro each several parts;
Accompanying drawing 4 is arranged on the data processing software flow chart on microcomputer 33;
Accompanying drawing 5 band vacuum system proving installation structural representations;
Accompanying drawing 6 band vacuum system proving installation structure partial cut-open views;
Accompanying drawing 7 band blanket gas proving installation structural representations;
Accompanying drawing 8 band blanket gas proving installation structure partial cut-open views;
In accompanying drawing: 1, sample support frame outer cover; 2, sample support frame; 3, heat block; 4, sample to be tested; 5, collets; 6, sample fixed card; 7, sample temperature thermocouple; 8, sample chamber temperature thermocouple; 9, sealing clamp; 10, outer lead interface; 11, connect the outer lead threeway; 12, tensimeter; 13, connect pressure meter three-way; 14, thermocouple vacuum gauge; 15, connect the thermocouple vacuum gauge threeway; 16, manual vacuum valve; 17, vacuum pump interface; 18, vacuum pump threeway; 19, air release; 20, connect the air release threeway; 21, blanket gas interface; 22, sample support frame connectivity port; 23, sample chamber well heater; 24, O-ring seal; 25, sample chamber temperature thermocouple wire; 26, heat block power lead; 27, test piece temperature thermocouple wire; 28, Seebeck electro-motive force measurement line; 29, sample chamber heater power lead; 30, control and data collector; 31, ice-water bath; 32, data line; 33, microcomputer; 34, sample fixed card gib screw; 35, threeway gland bonnet.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing:
Fig. 1 and Fig. 2 are proving installation surface structure schematic diagram and partial interior structure cut-open view.Proving installation by sample support frame outer cover 1, sample support frame 2, heat block 3, sample to be tested 4, insulating trip 5, sample fixed card 6, sample fixed card gib screw 34, sample temperature thermocouple 7, sample chamber temperature thermocouple 8, sealing clamp 9, outer lead interface 10, connect outer lead threeway 11, sample support frame connectivity port 22, sample chamber well heater 23, O-ring seal 24, threeway gland bonnet 35 etc. and form.The inside of sample support frame outer cover 1 forms the sample chamber of placing sample to be tested.Sample to be tested 4 is held in place on insulating trip 5 on sample support frame 2, and by sample fixed card 6 respectively with two sample temperature thermocouple 7 close contacts.Set up the temperature difference by the electrical heating piece 3 that is positioned at sample to be tested one side in the inside of sample to be tested 4, and by with sample to be tested 4 close contacts and temperature record two sample temperature thermocouples, 7 positions places thin-film thermoelectric materials along two sample temperature thermocouples 7 that temperature difference direction is intervally distributed with, respectively by means of by each the Seebeck electro-motive force measurement line 28 that wire is drawn in these two sample temperature thermocouples 7, record sample at these two temperature thermocouples, 7 inner Seebeck electromotive force that produce of place, position thin-film thermoelectric material simultaneously.
Sample chamber temperature thermocouple 8 is for detection of the temperature that is positioned at sample support frame outer cover 1 inner sample chamber.Sample support frame 2 by sample support frame connectivity port 22 with connect outer lead threeway 11 and be connected, by sealing clamp 9 with sample support frame outer cover 1 with connect outer lead threeway 11 and be connected.The port that connects outer lead threeway 11 is connected with threeway gland bonnet 35 by clip 9, and whole like this proving installation is in the masked state of sealing, and test process is avoided external interference.Whole proving installation sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27 and Seebeck electro-motive force measurement line 28 all extend proving installation by being arranged on the outer lead interface 10 that connects in outer lead threeway 11.
Circuit connection diagram between thin-film thermoelectric material Seebeck coefficient test macro each several part as shown in Figure 3, sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27, the Seebeck electro-motive force measurement line 28 that is connected by the sample temperature thermocouple 7 in proving installation, sample chamber temperature thermocouple 8, electrical heating piece 3 and sample chamber well heater 23 and sample chamber heater power lead 29 is connected respectively to or first control and data collector 30 through being connected to after ice-water bath 31.Control and data collector 30 are comprised of A/D converter, single-chip microcomputer, serial ports conversion, power supply, the electronic circuit that carries out signal transmission and signal processing, pushbutton switch etc.Control and data collector 30 are connected on microcomputer 33 by data line 32.By good data processing software prepared in advance on microcomputer 33, the data of controlling and data collector 30 collects are carried out comprehensive processing, and show in real time data processed result on the display of microcomputer 33.
Data processor as shown in Figure 4, measuring method is: open testing software and begin test, the right button of clicking the mouse, jump out a dialog box, select " opening serial ports ", begin to gather the Seebeck electromotive force that the voltage signal that represents sample cold junction and hot-side temperature and sample produce under this temperature difference, by program, the voltage signal of the representation temperature that collects is converted into its corresponding temperature value, and calculates the temperature difference.The temperature difference that utilization collects and electromotive force calculate corresponding Seebeck coefficient, and demonstrate in real time Seebeck coefficient and Seebeck electromotive force-temperature difference fitting a straight line equation on the display of microcomputer 33.After test was completed, the right button of clicking the mouse ejected a dialog box, clicked " time-out " to stop data acquisition, if finish test after preserving test result, withdrawed from test interface; If need to continue test, after click " time-out " stops data acquisition and preserves test result, click " emptying " to remove last test result, then click " beginning " to carry out the test of next sample.
The present invention can measure under many needed environmental baselines, is specifically described as follows:
Proving installation structural representation when under vacuum condition, the Seebeck coefficient of membraneous material being tested is in Fig. 5 and shown in Figure 6.Fig. 5 and Fig. 6 are band vacuum system proving installation surface structure schematic diagram and inner structure partial sectional view.band vacuum system proving installation is by sample support frame outer cover 1, sample support frame 2, heat block 3, sample to be tested 4, insulating trip 5, sample fixed card 6, sample fixed card gib screw 34, sample temperature thermocouple 7, sample chamber temperature thermocouple 8, sealing clamp 9, outer lead interface 10, connect outer lead threeway 11, tensimeter 12, connect pressure meter three-way 13, thermocouple vacuum gauge 14, connect thermocouple vacuum gauge threeway 15, manual vacuum valve 16, vacuum pump interface 17, connect vacuum pump threeway 18, air release 19, connect air release threeway 20, sample support frame connectivity port 22, sample chamber well heater 23, O-ring seal 24, threeway gland bonnet 35 compositions such as grade.Whole band vacuum system proving installation consists of an enclosed system by sample support frame outer cover 1, and the inside of sample support frame outer cover 1 forms the sample chamber of placing sample to be tested.Sample to be tested 4 is held in place on insulating trip 5 on sample support frame 2, and by sample fixed card 6 respectively with two sample temperature thermocouple 7 close contacts.Set up the temperature difference by the electrical heating piece 3 that is positioned at sample to be tested one side in the inside of sample to be tested 4, and by with sample to be tested 4 close contacts and temperature record two sample temperature thermocouples, 7 positions places thin-film thermoelectric materials along two sample temperature thermocouples 7 that temperature difference direction is intervally distributed with, respectively by means of by each the Seebeck electro-motive force measurement line 28 that wire is drawn in these two sample temperature thermocouples 7, record sample at these two temperature thermocouples, 7 inner Seebeck electromotive force that produce of place, position thin-film thermoelectric material simultaneously.
Sample chamber temperature thermocouple 8 is for detection of the temperature that is positioned at sample support frame outer cover 1 inner sample chamber.Sample support frame 2 by sample support frame connectivity port 22 with connect outer lead threeway 11 and be connected, by sealing clamp 9 with sample support frame outer cover 1 with connect outer lead threeway 11 and be connected.Sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27 and Seebeck electro-motive force measurement line 28 all extend band vacuum system proving installation by being arranged on the outer lead interface 10 that connects in outer lead threeway 11.Connect pressure meter three-way 13 by sealing clamp 9 with connect outer lead threeway 11 and be connected, the tensimeter 12 of installing on it is used for showing the pressure with vacuum system proving installation inside.Connect thermocouple vacuum gauge threeway 15 by sealing clamp 9 with connect pressure meter three-way 13 and be connected, the thermocouple vacuum gauge 14 of installing on it is used for showing the vacuum tightness with vacuum system proving installation inside.Connect vacuum pump threeway 18 by sealing clamp 9 with connect thermocouple vacuum gauge threeway 15 and be connected, the manual vacuum valve 16 of installing on it is used for the vacuum tightness of accommodation zone vacuum system proving installation inside, and the vacuum pump interface 17 that is connected on manual vacuum valve 16 by sealing clamp 9 is used for being connected with vacuum pump by external pipeline.Connect air release threeway 20 by sealing clamp 9 with connect vacuum pump threeway 18 and be connected, the air release 19 of installing on it is used for the gaseous tension of accommodation zone vacuum system proving installation inside.
By the sample chamber temperature thermocouple wire 25 that connects with the sample temperature thermocouple 7 in the vacuum system proving installation, sample chamber temperature thermocouple 8, electrical heating piece 3 and sample chamber well heater 23, heat block power lead 26, test piece temperature thermocouple wire 27, Seebeck electro-motive force measurement line 28 and sample chamber heater power lead 29 is connected respectively to or first control and data collector 30 through being connected to after ice-water bath 31.Control and data collector 30 by A/D converter, single-chip microcomputer, serial ports conversion, power supply, carry out electronic circuit, pushbutton switch that signal transmission and signal process and form.Control and data collector 30 are connected on microcomputer 33 by data line 32.By good data processing software prepared in advance on microcomputer 33, the data of controlling and data collector 30 collects are carried out comprehensive processing, and show in real time data processed result on the display of microcomputer 33.
Proving installation structural representation when under the blanket gas condition, the Seebeck coefficient of membraneous material being tested is in Fig. 7 and shown in Figure 8.Fig. 7 and Fig. 8 are band blanket gas proving installation surface structure schematic diagram inner structure cut-open view.band blanket gas proving installation is by sample support frame outer cover 1, sample support frame 2, heat block 3, sample to be tested 4, insulating trip 5, sample fixed card 6, sample fixed card gib screw 34, sample temperature thermocouple 7, sample chamber temperature thermocouple 8, sealing clamp 9, outer lead interface 10, connect outer lead threeway 11, tensimeter 12, connect pressure meter three-way 13, thermocouple vacuum gauge 14, connect thermocouple vacuum gauge threeway 15, manual vacuum valve 16, vacuum pump interface 17, connect vacuum pump threeway 18, air release 19, connect air release threeway 20, blanket gas interface 21, sample support frame connectivity port 22, sample chamber well heater 23, O-ring seal 24 compositions such as grade.Whole band blanket gas proving installation consists of an enclosed system by sample support frame outer cover 1, and the inside of sample support frame outer cover 1 forms the sample chamber of placing sample to be tested.Sample to be tested 4 is held in place on insulating trip 5 on sample support frame 2, and by sample fixed card 6 respectively with two sample temperature thermocouple 7 close contacts.Set up the temperature difference by the electrical heating piece 3 that is positioned at sample to be tested one side in the inside of sample to be tested 4, and by with sample to be tested 4 close contacts and temperature record two sample temperature thermocouples, 7 positions places thin-film thermoelectric materials along two sample temperature thermocouples 7 that temperature difference direction is intervally distributed with, respectively by means of by each the Seebeck electro-motive force measurement line 28 that wire is drawn in these two sample temperature thermocouples 7, record sample at these two temperature thermocouples, 7 inner Seebeck electromotive force that produce of place, position thin-film thermoelectric material simultaneously.
Sample chamber temperature thermocouple 8 is for detection of the temperature that is positioned at sample support frame outer cover 1 inner sample chamber.Sample support frame 2 by sample support frame connectivity port 22 with connect outer lead threeway 11 and be connected, by sealing clamp 9 with sample support frame outer cover 1 with connect outer lead threeway 11 and be connected.Sample chamber temperature thermocouple wire 25, heat block power lead 26, test piece temperature thermocouple wire 27 and Seebeck electro-motive force measurement line 28 all extend band blanket gas proving installation by being arranged on the outer lead interface 10 that connects in outer lead threeway 11.Connect pressure meter three-way 13 by sealing clamp 9 with connect outer lead threeway 11 and be connected, the tensimeter 12 of installing on it is used for showing the pressure with blanket gas proving installation inside.Connect thermocouple vacuum gauge threeway 15 by sealing clamp 9 with connect pressure meter three-way 13 and be connected, the thermocouple vacuum gauge 14 of installing on it is used for showing the vacuum tightness with blanket gas proving installation inside.Connect vacuum pump threeway 18 by sealing clamp 9 with connect thermocouple vacuum gauge threeway 15 and be connected; the manual vacuum valve 16 of installing on it is used for the vacuum tightness of accommodation zone blanket gas proving installation inside, and the vacuum pump interface 17 that is connected on manual vacuum valve 16 by sealing clamp 9 is used for being connected with vacuum pump by external pipeline.Connect air release threeway 20 by sealing clamp 9 with connect vacuum pump threeway 18 and be connected, the air release 19 of installing on it is used for the gaseous tension of accommodation zone blanket gas proving installation inside.Manual vacuum valve 16 by sealing clamp 9 with connect air release threeway 20 and be connected; the blanket gas interface 21 that is connected thereto by sealing clamp 9 is used for being connected to outer protection gas by external pipeline; it is inner that blanket gas can enter band blanket gas proving installation by blanket gas interface 21, regulates amount and the pressure thereof that enters with the blanket gas of blanket gas proving installation inside by manual vacuum valve 16.
By the sample chamber temperature thermocouple wire 25 that connects with the sample temperature thermocouple 7 in the blanket gas proving installation, sample chamber temperature thermocouple 8, electrical heating piece 3 and sample chamber well heater 23, heat block power lead 26, test piece temperature thermocouple wire 27, Seebeck electro-motive force measurement line 28 and sample chamber heater power lead 29 is connected respectively to or first control and data collector 30 through being connected to after ice-water bath 31.Control and data collector 30 by A/D converter, single-chip microcomputer, serial ports conversion, power supply, carry out electronic circuit, pushbutton switch that signal transmission and signal process and form.Control and data collector 30 are connected on microcomputer 33 by data line 32.By good data processing software prepared in advance on microcomputer 33, the data of controlling and data collector 30 collects are carried out comprehensive processing, and show in real time data processed result on the display of microcomputer 33.
Method of testing is as follows:
1. test the Seebeck coefficient of P type Bi2Te3 thermoelectric membraneous material under atmospheric conditions
Test operating procedure:
1) start microcomputer 33, click thin-film thermoelectric material Seebeck coefficient testing software icon, open test interface;
2) the sample support frame outer cover with proving installation takes off, the thin-film thermoelectric material test piece is placed on ceramic block 5 in the sample chamber, and after fixing with sample fixed card 6, sample support frame outer cover is fixed to clip connects in the outer lead threeway, this moment, whole proving installation was in air-tight state;
3) the sample chamber heater button on startup control and data collector 30, sample chamber well heater 23 is started working, and measure by means of the temperature of sample chamber temperature thermocouple 8 pairs of sample chambers, by controlling and data collector 30 Quality control chamber heaters 23, make the temperature in the sample chamber reach also constant in predetermined value;
4) the heat block switch that starts on control and data collector 30 makes heat block 3 begin heating, sets up the temperature difference in the inside of sample to be tested 4;
5) right button of clicking the mouse, a plurality of dialog boxes appear in the test interface on microcomputer 33 displays, click " opening serial ports ", the data that control and data collector 30 collect begin to be transferred to microcomputer 33, the relation curve that shows in real time the temperature difference between two sample temperature thermocouples, the 7 inner Seebeck electromotive force that form of place, place sample to be tested and this two points for measuring temperature in beginning on the display of microcomputer 33, microcomputer 33 is processed the data that collect simultaneously, and Seebeck coefficient and the match Seebeck electromotive force-temperature difference relation curve equation that processing obtains is presented at the below at this interface.
6) test finishes, the right button of clicking the mouse, and a plurality of dialog boxes appear in test interface.Click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.If finish whole test process, click " withdrawing from " in dialog box, close heat block switch, sample chamber heater button, close general supply, open clip and take off sample support frame outer cover, take out specimen.
7) after the test that finishes a certain sample, if need to continue the Seebeck coefficient of other sample of test, the right button of clicking the mouse, a plurality of dialog boxes appear in test interface, click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.Click " emptying " in dialog box, to remove the test result on the interface.Open clip and take off sample support frame outer cover 1, take out specimen, another testing sample is placed on ceramic block 5 in the sample chamber, and fixes with sample fixed card 6, repeat above-mentioned 3)~8) step complete the test of Seebeck coefficient.
Test result, P type Bi2Te3 thermoelectric membraneous material Seebeck coefficient is 127.3 μ V/K.
2. test the Seebeck coefficient of N-type Bi2Te3 thermoelectric membraneous material under vacuum condition
Test operating procedure:
1) start microcomputer 33, click thin-film thermoelectric material Seebeck coefficient testing software icon, open test interface;
2) will take off with the sample support frame outer cover of vacuum system proving installation, the thin-film thermoelectric material test piece is placed on ceramic block 5 in the sample chamber, and fix with sample fixed card 6, sample support frame outer cover is fixed to clip connects in the outer lead threeway, this moment, whole band vacuum system proving installation was in air-tight state;
3) the sample chamber heater button on startup control and data collector 30, sample chamber well heater 23 is started working, and measure by means of the temperature of sample chamber temperature thermocouple 8 pairs of sample chambers, by controlling and data collector 30 Quality control chamber heaters 23, make the temperature in the sample chamber reach also constant in predetermined value;
4) start vacuum pump, open manual vacuum valve 16, and the pressure that detects with vacuum system proving installation inside by tensimeter 12 and thermocouple vacuum gauge 14, when being with vacuum system proving installation internal pressure to reach required vacuum tightness, close manual vacuum valve 16 and vacuum pump;
5) the heat block switch that starts on control and data collector 30 makes heat block 3 begin heating, sets up the temperature difference in the inside of sample to be tested 4;
6) right button of clicking the mouse, a plurality of dialog boxes appear in the test interface on the indicator screen of microcomputer 33, click " opening serial ports ", the data that control and data collector 30 collect begin to be transferred to microcomputer 33, the relation curve that shows in real time the temperature difference between two sample temperature thermocouples, the 7 inner Seebeck electromotive force that form of place, place sample to be tested and this two points for measuring temperature in beginning on the display of microcomputer 33, microcomputer 33 is processed the data that collect simultaneously, and Seebeck coefficient and the match Seebeck electromotive force-temperature difference relation curve equation that processing obtains is presented at the below at this interface.
7) test finishes, the right button of clicking the mouse, and a plurality of dialog boxes appear in test interface.Click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.If finish whole test process, click " withdrawing from " in dialog box, close heat block switch, sample chamber heater button, close general supply, open air release, open clip and take off sample support frame outer cover, take out specimen.
8) after the test that finishes a certain sample, if need to continue the Seebeck coefficient of other sample of test, the right button of clicking the mouse, a plurality of dialog boxes appear in test interface, click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.Click " emptying " in dialog box, to remove the test result on the interface.Open clip and take off sample support frame outer cover 1, take out specimen, another test piece to be measured is placed on ceramic block 5 in the sample chamber, and fixes with sample fixed card 6, repeat above-mentioned 3)~8) step complete the test of Seebeck coefficient.
The test result demonstration, the Seebeck coefficient of this thin-film thermoelectric material is-118.6 μ V/K.
3. test the Seebeck coefficient of N-type Bi2Te3 thermoelectric membraneous material under condition of nitrogen gas
Test operating procedure:
1) start microcomputer 33, click thin-film thermoelectric material Seebeck coefficient testing software icon, open test interface;
2) will take off with the sample support frame outer cover of blanket gas proving installation, the thin-film thermoelectric material test piece is placed on ceramic block 5 in the sample chamber, and fix with sample fixed card 6, sample support frame outer cover is fixed to clip connects in the outer lead threeway, this moment, whole band blanket gas proving installation was in air-tight state;
3) the sample chamber heater button on startup control and data collector 30, sample chamber well heater 23 is started working, and measure by means of the temperature of sample chamber temperature thermocouple 8 pairs of sample chambers, by controlling and data collector 30 Quality control chamber heaters 23, make the temperature in the sample chamber reach also constant in predetermined value;
4) start vacuum pump, open manual vacuum valve 16, and the pressure that detects with blanket gas proving installation inside by tensimeter 12 and thermocouple vacuum gauge 14, when being with blanket gas proving installation internal pressure to reach required vacuum tightness, close manual vacuum valve 16 and vacuum pump;
5) open nitrogen cylinder and manual vacuum valve 16, and the pressure that detects with blanket gas proving installation inside by tensimeter 12 and thermocouple vacuum gauge 14, when reaching desirable value to the pressure with blanket gas proving installation internal gas, close manual vacuum valve 16 and nitrogen cylinder;
6) the heat block switch that starts on control and data collector 30 makes heat block 3 begin heating, sets up the temperature difference in the inside of sample to be tested 4;
7) right button of clicking the mouse, a plurality of dialog boxes appear in the test interface on the indicator screen of microcomputer 33, click " opening serial ports ", the data that control and data collector 30 collect begin to be transferred to microcomputer 33, the relation curve that shows in real time the temperature difference between two sample temperature thermocouples, the 7 inner Seebeck electromotive force that form of place, place sample to be tested and this two points for measuring temperature in beginning on the display of microcomputer 33, microcomputer 33 is processed the data that collect simultaneously, and Seebeck coefficient and the match Seebeck electromotive force-temperature difference relation curve equation that processing obtains is presented at the below at this interface.
8) test finishes, the right button of clicking the mouse, and a plurality of dialog boxes appear in test interface.Click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.If finish whole test process, click " withdrawing from " in dialog box, close heat block switch, sample chamber heater button, close general supply, open clip and take off sample support frame outer cover, take out specimen.
9) after the test that finishes a certain sample, if need to continue the Seebeck coefficient of other sample of test, the right button of clicking the mouse, a plurality of dialog boxes appear in test interface, click " time-outs ", stop controlling and the data of data collector 30 collections to the transmission of microcomputer 33.Click " preservation " in dialog box, test result is saved in computing machine.Click " emptying " in dialog box, to remove the test result on the interface.Open clip and take off sample support frame outer cover 1, take out specimen, another test piece to be measured is placed on ceramic block 5 in the sample chamber, and fixes with sample fixed card 6, repeat above-mentioned 3)~8) step complete the test of Seebeck coefficient.
The test result demonstration, the Seebeck coefficient of this thin-film thermoelectric material is-118.6 μ V/K.

Claims (3)

1. thin-film thermoelectric material Seebeck coefficient test macro is characterized in that being made of proving installation and control and test circuit system two parts, its proving installation is by sample support frame outer cover (1), sample support frame (2), heat block (3), sample to be tested (4), insulating trip (5), sample fixed card (6), sample fixed card gib screw (34), sample temperature thermocouple (7), sample chamber temperature thermocouple (8), sealing clamp (9), outer lead interface (10), connect outer lead threeway (11), sample support frame connectivity port (22), sample chamber well heater (23), O-ring seal (24), threeway gland bonnet (35) forms, the inside of sample support frame outer cover (1) forms the sample chamber of placing sample to be tested, sample to be tested (4) is held in place on insulating trip (5) on sample support frame (2), and by sample fixed card (6) respectively with two sample temperature thermocouples (7) close contact, set up the temperature difference by the electrical heating piece (3) that is positioned at sample to be tested one side in the inside of sample to be tested (4), and by with sample to be tested (4) close contact, and record the temperature of place, two sample temperature thermocouples (7) position thin-film thermoelectric material along two sample temperature thermocouples (7) that temperature difference direction is intervally distributed with, simultaneously respectively by means of by each the Seebeck electro-motive force measurement line (28) that wire is drawn in these two sample temperature thermocouples (7), record sample at the inner Seebeck electromotive force that produces of this place, two temperature thermocouples (7) position thin-film thermoelectric material, its control and test circuit system are: sample chamber temperature thermocouple wire (25), heat block power lead (26), test piece temperature thermocouple wire (27) and Seebeck electro-motive force measurement line (28) all extend proving installation by being arranged on the outer lead interface (10) that connects in outer lead threeway (11), by the sample temperature thermocouple (7) in proving installation, sample chamber temperature thermocouple (8), the sample chamber temperature thermocouple wire (25) that electrical heating piece (3) and sample chamber well heater (23) connect, heat block power lead (26), test piece temperature thermocouple wire (27), Seebeck electro-motive force measurement line (28) and sample chamber heater power lead (29) are connected respectively to or first pass through ice-water bath (31) and be connected to afterwards control and data collector (30), control and data collector (30) by A/D converter, single-chip microcomputer, serial ports conversion, power supply, carry out electronic circuit, pushbutton switch that signal transmission and signal process and form, control and data collector (30) are connected on microcomputer (33) by data line (32), by microcomputer (33), the data of controlling and data collector (30) collects are processed, and shown in real time data processed result on the display of microcomputer (33).
2. thin-film thermoelectric material Seebeck coefficient test macro claimed in claim 1, when it is characterized in that described test macro is tested the Seebeck coefficient of membraneous material under vacuum condition, need the threeway gland bonnet (35) in test macro is removed, by sealing clamp (9) with connect pressure meter three-way (13) and be connected; Connect the tensimeter (12) of installing on pressure meter three-way and be used for demonstration with the pressure of vacuum system proving installation inside, connect thermocouple vacuum gauge threeway (15) by sealing clamp (9) with connect pressure meter three-way (13) and be connected, the thermocouple vacuum gauge (14) of installing on it is used for showing the vacuum tightness with vacuum system proving installation inside; Connect vacuum pump threeway (18) by sealing clamp (9) with connect thermocouple vacuum gauge threeway (15) and be connected, the manual vacuum valve (16) of installing on it is used for the vacuum tightness of accommodation zone vacuum system proving installation inside, and the vacuum pump interface (17) that is connected on manual vacuum valve (16) by sealing clamp (9) is used for being connected with vacuum pump by external pipeline; Connect air release threeway (20) by sealing clamp (9) with connect vacuum pump threeway (18) and be connected, the air release (19) of installing on it is used for the gaseous tension of accommodation zone vacuum system proving installation inside.
3. thin-film thermoelectric material Seebeck coefficient test macro as claimed in claim 1, it is characterized in that described test macro is when testing the Seebeck coefficient of membraneous material under the blanket gas condition, need the threeway gland bonnet (35) in test macro is removed, by sealing clamp (9) with connect pressure meter three-way (13) and be connected; Connect the tensimeter (12) of installing on pressure meter three-way and be used for demonstration with the pressure of blanket gas proving installation inside; Connect thermocouple vacuum gauge threeway (15) by sealing clamp (9) with connect pressure meter three-way (13) and be connected, the thermocouple vacuum gauge (14) of installing on it is used for showing the vacuum tightness with blanket gas proving installation inside; Connect vacuum pump threeway (18) by sealing clamp (9) with connect thermocouple vacuum gauge threeway (15) and be connected, the manual vacuum valve (16) of installing on it is used for the vacuum tightness of accommodation zone blanket gas proving installation inside, and the vacuum pump interface (17) that is connected on manual vacuum valve (16) by sealing clamp (9) is used for being connected with vacuum pump by external pipeline; Connect air release threeway (20) by sealing clamp (9) with connect vacuum pump threeway (18) and be connected, the air release (19) of installing on it is used for the gaseous tension of accommodation zone blanket gas proving installation inside; Manual vacuum valve (16) by sealing clamp (9) with connect air release threeway (20) and be connected; the blanket gas interface (21) that is connected thereto by sealing clamp (9) is used for being connected to outer protection gas by external pipeline; it is inner that blanket gas can enter band blanket gas proving installation by blanket gas interface (21), regulates amount and the pressure thereof that enters with the blanket gas of blanket gas proving installation inside by manual vacuum valve (16).
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