CN201903526U - Conductivity and Seebeck coefficient test device for semiconductor film materials at low temperatures - Google Patents
Conductivity and Seebeck coefficient test device for semiconductor film materials at low temperatures Download PDFInfo
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- CN201903526U CN201903526U CN2010206555434U CN201020655543U CN201903526U CN 201903526 U CN201903526 U CN 201903526U CN 2010206555434 U CN2010206555434 U CN 2010206555434U CN 201020655543 U CN201020655543 U CN 201020655543U CN 201903526 U CN201903526 U CN 201903526U
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Abstract
The utility model relates to a conductivity and Seebeck coefficient test device for semiconductor film materials at low temperatures, and the conductivity and Seebeck coefficient test device comprises a temperature control unit, a low-temperature test unit and a data acquisition unit which are connected with one another and is characterized in that the temperature control unit comprises a liquid nitrogen Dewar tank (1), a low-temperature vacuum container (2) placed in the liquid nitrogen Dewar tank (1), a temperature control instrument (3) connected with the liquid nitrogen Dewar tank (1), a film electric heating plate (4) and a steady-current source (5); the low-temperature test unit comprises a cold-end temperature measurement thermocouple (6) and a hot-end temperature measurement thermocouple (7) and an electrodynamic potential measuring line (8), wherein the cold-end temperature measurement thermocouple (6) and the hot-end temperature measurement thermocouple (7) are connected with a thermoelectric film material sample (16) positioned in the low-temperature vacuum container (2); and the electrodynamic potential measuring line (8) is suitable for the temperature range from 80K to the room temperature. The conductivity and seebeck coefficient test device is simple in structure, has no moving part, can conveniently measure the conductivity and the Seebeck coefficient at the low temperatures and also can effectively realize the measurement to the thermoelectric performance parameters of LNG (liquefied natural gas) cold energy temperature-difference power generating film materials at the low temperatures.
Description
Technical field
The utility model relates to the development and use of new forms of energy, particularly, the utility model relates to a kind of semiconductor thermoelectric membraneous material conductivity and Seebeck coefficient proving installation at low temperatures, the test macro of described semiconductor thermoelectric membraneous material conductivity and Seebeck (Seebeck) coefficient testing device branch relating to the Engineering Thermophysics subject at low temperatures---the development of temperature-difference power generation module, especially involvement aspect conductivity and Seebeck coefficient under the low temperature of the thermo-electric generation semiconductor thermoelectric membraneous material that utilizes the LNG cold energy that low temperature uses.
Background technology
LNG (liquefied natural gas (LNG)) is low temperature (162 ℃) liquid mixture that rock gas forms by the low temperature process cryogenic liquefaction, is a kind of energy of clean and effective.At present, the LNG cold energy generation mainly is to utilize the cryogenic cold energy of LNG to make in the Blast Furnace Top Gas Recovery Turbine Unit (TRT) cycle fluid liquefaction, and then, working medium is through heating and gasifying, and expansion working in gas-turbine again is to drive generator for electricity generation.
To thermo-electric generation, the work of this area both at home and abroad mainly concentrates in the research of thermo-electric converting material.Yet, still be in the starting stage at home towards the thermoelectric material research of low temperature utilization.
In the semiconductor temperature differential generating material performance index, relate to figure of merit Z=α
2σ/κ.
At described figure of merit Z=α
2In the definition of σ/κ, α is associating Seebeck (Seebeck) coefficient, and σ is a conductivity, and κ is a coefficient of heat conductivity.The thermoelectricity capability of material can be weighed with Z or ZT, and we claim α
2σ is the power factor of material, and the ZT value is a dimensionless parameters, and wherein T is the mean value of material working temperature.
By the expression formula of above-mentioned figure of merit Z as can be seen, promptly increasing Seebeck (Seebeck) factor alpha of thermoelectric material and reduce its coefficient of heat conductivity κ, is the key that increases ZT value, raising semiconductor temperature differential generating efficient.But in fact, because 3 factors of decision Z value are the parameters that is mutually related, all be the function of carrier concentration, can not they be optimized, this be the not high main cause of present pyroelectric material performance.
Therefore the accurate measurement of conductivity and Seebeck (Seebeck) factor alpha has very important using value and theory significance to the further investigation thermoelectricity capability of semiconductor material and development of new semi-conductor thermoelectric material and device.
Developed at present the proving installation that much is used for testing film resistivity and Seebeck coefficient, but these devices all are pyrometric devices in reaching at normal temperature.
For example, to be " 200710072785.3 ", denomination of invention disclose a kind of device that is used for the measuring semiconductor conducting material thermoelectricity performance for people's such as Chen Gang, the Pei Jian of Harbin Institute of Technology, Zhou Nan utility model patent for " semi-conducting material thermoelectricity performance test system ", utility model people to the patent No..This device mainly be at block materials in ℃ temperature range of room temperature～800, conductivity and Seebeck (Seebeck) factor alpha proving installation that dependence on temperature is done just.To be " 200720067899.4 ", denomination of invention disclose a kind of semiconductor heat electric tester for people's such as Cai Kefeng, the Zhang Aixia of Tongji University, Yan Chong utility model patent for " a kind of semiconductor thermoelectric ability meter ", utility model people to the patent No..This tester can be tested room temperature～600 ℃ semiconductor body conductivity of electrolyte materials, Seebeck coefficient and ZT value.The patent No. be " 200720084694.7 ", denomination of invention for " a kind of device of measuring semiconductor thermoelectric membraneous material Seebeck coefficient and resistivity ", utility model people for people's such as Yang Junyou, the Xiao Chengjing of the Central China University of Science and Technology, red legend patent utility model patent discloses a kind of device of measuring Seebeck coefficient and resistivity under the semiconductor thermoelectric membraneous material room temperature.But this device does not relate to the measurement of the thermoelectricity capability parameter of semiconductor thermoelectric membraneous material in the low temperature environment.
Thereby, up to now, still do not have both at home and abroad for semiconductor thermoelectric membraneous material measuring system of conductivity and Seebeck coefficient under low temperature environment and to relate to.
The utility model content
For overcoming the problems referred to above, the purpose of this utility model is: a kind of semiconductor thermoelectric membraneous material conductivity at low temperatures and the proving installation of Seebeck coefficient are provided, and this square law device can accurately be measured the conductivity and the Seebeck coefficient of thermoelectric film material under the low temperature.
The utility model is achieved through the following technical solutions:
Conductivity under a kind of semiconductor film material low temperature and Seebeck coefficient proving installation, whole testing device comprises temperature control unit, low-temperature test unit and the data acquisition unit of connection, it is characterized in that described temperature control unit comprises: Dewar container for liquefied nitrogen jar, the cryogenic vacuum container that places the Dewar container for liquefied nitrogen jar, the temperature controller that is connected in the Dewar container for liquefied nitrogen jar, thin-film electro heating plate and constant current source;
Described low-temperature test unit comprises cold junction temperature thermocouple and the hot junction temperature thermocouple that connects the thermoelectric film material sample that is arranged in cryogenic vacuum container 2, the electro-motive force measurement line that is suitable for to the room temperature with temperature range 80K, described thermopair selects for use temperature range at 200～25 ℃ T type thermopair, i.e. copper-constantan thermocouple;
Described data acquisition unit comprises via cold junction temperature thermocouple and hot junction temperature thermocouple, the data acquisition unit of electro-motive force measurement line and the computing machine that is connected thereof.
According to conductivity under the semiconductor film material low temperature described in the utility model and Seebeck coefficient proving installation, it is characterized in that, get the temperature difference and between 4～15K, change.
According to conductivity under the semiconductor film material low temperature described in the utility model and Seebeck coefficient proving installation, it is characterized in that described low temperature is the low temperature of 80K to 200K.
According to conductivity under the semiconductor film material low temperature described in the utility model and Seebeck coefficient proving installation, it is characterized in that, constant current source amount of exports definite value scope 0～35V/0.8A, precision is less than 0.2%+10mA, and the electro-motive force measurement line selection is with the platinum line of diameter 0.025 ~ 0.05mm.
According to conductivity under the semiconductor film material low temperature described in the utility model and Seebeck coefficient proving installation, it is characterized in that, specimen holder (12) and sample support frame (11) are set in the described cryogenic vacuum container, end at described thermoelectric film material sample is provided with thin-film electro heating plate (4), described thin-film electro heating plate size is sixth ~ 1/4th of membraneous material sample, and described cryogenic vacuum container adopts feed-through collar (19) sealing.
According to the conductivity under the employing semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, described method comprises the steps:
1) thermoelectric film material sample to be measured is fixed on the specimen holder, the end heating that the film heating plate is given the membraneous material sample by the heat conduction copper sheet makes its inside set up the temperature difference;
2) the cold and hot end temperature thermocouple of sample closely contacts with described membraneous material sample by specimen holder, record the temperature of its cold and hot end, respectively by means of by each the Seebeck electro-motive force measurement line that lead is drawn in these two the described membraneous material sample temperature thermocouples, record described membraneous material sample simultaneously at the inner Seebeck electromotive force that produces of this place, two temperature thermocouple positions thermoelectric film material;
3) will fix sample and the membraneous material sample support frame of turning on the electricity is put into a low-temperature (low temperature) vessel (as accompanying drawing 1) and is evacuated,
4) then this container is put into the Dewar jar of splendid attire liquid nitrogen, the temperature by temperature controller is regulated low temperature environment concerns with variation of temperature under low temperature environment with this conductivity and Seebeck coefficient of measuring semiconductor thermoelectric membraneous material sample.
Conductivity and Seebeck coefficient method of testing according under the semiconductor thermoelectric membraneous material low temperature of the present utility model is characterized in that, in step 1), according to the definition of Seebeck coefficient:
Apply a small temperature difference Δ T at membraneous material sample two ends, promptly an end temperature is T
1=T
0, the temperature of the other end is T
2=T
0+ Δ T, then membraneous material sample two ends Seebeck electromotive force V (T
1, T
2) be:
If
Enough little, can get:
According to above-mentioned, described semiconductor thermoelectric membraneous material is in a certain temperature T
0The time, α (T
0) mensuration can measure the Seebeck electromotive force of described semiconductor thermoelectric membraneous material sample under Δ T by applying a small temperature difference T at described semiconductor thermoelectric membraneous material sample two ends, obtain Seebeck factor alpha (T by following formula
0).
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, get the temperature difference and between 4～15K, change, treat that the cold and hot end temperature difference begins data acquisition when reaching 3K.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, gather the data point more than 50 during each the test, obtain straight slope by least-squares algorithm linear fitting, be Seebeck coefficient value (unit is μ V/K).
In step 1), bring bigger test error in order to reduce excessive difference variation to test result, get the temperature difference and between 4～15K, change.Treat can begin data acquisition when the cold and hot end temperature difference reaches 3K, maximum temperature difference generally is controlled at about 15K, should gather 50-100 data point when testing at every turn, obtains straight slope by least-squares algorithm linear fitting, is the Seebeck coefficient value.
In step 1), bring bigger test error in order to reduce excessive difference variation to test result, get the temperature difference and between 4～15K, change.Treat can begin data acquisition when the cold and hot end temperature difference reaches 3K, maximum temperature difference generally is controlled at about 15K, should gather the data point more than 50 when testing at every turn, obtains straight slope by least-squares algorithm linear fitting, is the Seebeck coefficient value.
Be preferably, in step 1), gather 50-100 data point when testing at every turn, obtain straight slope, be the Seebeck coefficient value by least-squares algorithm linear fitting.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, the conductivity test philosophy is, when four metal probes are arranged in a line, and when being pressed on the thermoelectric film material with certain pressure, between peripheral two probes, feed electric current I, then between inboard two probes, produce potential difference (PD) U, calculate the conductivity (S/m) of semiconductor thermoelectric membraneous material according to following formula:
σ＝ΔX·I/U.A (4)
Wherein σ is conductivity (S/m), and Δ X is two needle tip spacings (m), and A is membraneous material sample sectional area (m
2).
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, the deviation of bringing for the Peltier effect of eliminating thermoelectric material, flow through the direction of current of described membraneous material sample in the measuring process by change, make the current opposite in direction that flows through the membraneous material sample for twice, and twice measurement result is averaged as final measurement.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, described low temperature is the low temperature of 80K to 200K.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, described thin-film electro heating plate size is sixth ~ 1/4th of membraneous material sample.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, produce Joule heat and Peltier effect for fear of feeding too big electric current, bring measuring error, constant current source selects for use lower range, precision high, it is enough little to feed electric current, and it is fast that test speed is wanted.The electro-motive force measurement line selection platinum line of diameter 0.025 ~ 0.05mm.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, described constant current source 5 amount of exports definite value scopes 0～35V/0.8A, precision is less than 0.2%+10mA.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, constant current source can adopt Agilent E3641A, promptly adopt lower range, precision high, it is enough little to feed electric current, the constant current source that test speed is fast is with the measuring error of avoiding feeding too big electric current generation Joule heat and Peltier effect and bringing.
Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, specimen holder and sample support frame are set in the described cryogenic vacuum container, end at described thermoelectric film material sample is provided with the thin-film electro heating plate, and the cryogenic vacuum container adopts the feed-through collar sealing.
According to the semiconductor thermoelectric membraneous material of the present utility model conductivity at low temperatures and the proving installation of Seebeck coefficient, thermoelectric film material sample to be measured is placed in the proving installation, and proving installation moves in the enclosed vacuum environment; Temperature control system is used to regulate and control the environment temperature of proving installation and keeps temperature constant, realizes treating the low temperature thermoelectricity capability test of calorimetric conductive film material sample.Gather data-signal such as high low side temperature, electromotive force by data collecting instrument and be connected to computing machine, realize the control of whole test process, the processing of test data and the real-time demonstration of test data.The conductivity and the Seebeck coefficient of thermoelectric film material under the low temperature can accurately be measured by this system.Adopt the conductivity under the semiconductor film material low temperature described in the utility model and the method for testing of Seebeck coefficient proving installation, have simple, movement-less part, carry out lot of advantages such as conductivity and the measurement of Seebeck coefficient easily, can effectively realize the LNG cold energy thermo-electric generation membraneous material thermoelectricity capability parameter measurement of temperature 80K to the room temperature.
Description of drawings
Fig. 1 is the main structure synoptic diagram that conductivity and Seebeck coefficient are measured under the semiconductor thermoelectric membraneous material low temperature
Fig. 2 is the synoptic diagram of semiconductor thermoelectric film sample material anchor clamps and cryogenic vacuum container.
Wherein: 1-Dewar container for liquefied nitrogen jar, 2-cryogenic vacuum container, 3-temperature controller, 4-thin-film electro heating plate, the 5-constant current source, 6-cold junction temperature thermocouple (T type thermopair), 7-hot junction temperature thermocouple (T type thermopair), 8-electro-motive force measurement line, 9-data acquisition unit, 10-computing machine, 11-sample support frame, 12-specimen holder, 13-gib screw, the 14-copper sheet, 15-insulating substrate, 16-thermoelectric film material sample to be measured, 17-vacuum pump interface, 18-gasket seal, 19-feed-through collar.
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in further detail with embodiment.
To homemade Zn
4Sb
3Semiconductor thermoelectric membraneous material (thickness is hundreds of Nai Mi-tens of microns) carries out the conductivity under the 100K-120K low temperature and the measurement of Seebeck coefficient.
Fig. 1 and Fig. 2 are test macro surface structure synoptic diagram and partial interior structure cut-open view.As depicted in figs. 1 and 2, prepared thermoelectric film material sample 16 is placed on the sample support frame 11 of the present utility model, tightens fixing with gib screw 13.Draw two Pt leads as electrode at semiconductor thermoelectric membraneous material sample two ends by the cohesive action of silver slurry, and adopt thin-film electro heating plate 4 to heat near the place of electrode, produce the temperature difference about 4K to guarantee the film two ends at film one end.
Described thin-film electro heating plate size is below 1/4th of membraneous material sample.In the present embodiment, described thin-film electro heating plate size is at 1/4th of membraneous material sample.
The membraneous material sample support frame that fixes sample and turn on the electricity is put into cryogenic vacuum container (2), described its drum diameter of cryogenic vacuum container and height are according to the size decision of thermoelectric film material sample to be measured and specimen holder, and assurance sample and anchor clamps can be put into container fully.Then, vacuum feed-through collar 19 is installed on the described cryogenic vacuum container, is guaranteed the sealing of vacuum tank and pump it to vacuum with vacuum pump.Measuring lead picks out by the feed-through collar of vacuum tank.
Whole vacuum tank 2 is put into the Dewar container for liquefied nitrogen jar 1 that holds liquid nitrogen.Described Dewar container for liquefied nitrogen jar 1 its openings of sizes that holds liquid nitrogen can just be put cryogenic vacuum container 2 into.Cryogenic vacuum container 2 2/ 3 immerses in the liquid nitrogen, guarantees that the low energy of its inner cryogenic environment reaches 80K.
Regulate container environment temperature on every side by temperature controller, test lead and low temperature are connected to collector 9, one computing machines with thermopair and are connected with collector 9 respectively at constant current source.
Described constant current source 5 can adopt selects for use lower range, precision high, and it is enough little to feed electric current, the constant current source that test speed is fast, for example, and gilent E3641A, the amount of exports definite value scope 0～35V/0.8A of described constant current source 5, precision is less than 0.2%+10mA.
Thus, can avoid feeding too big electric current and produce Joule heat and Peltier effect, cause bringing measuring error. described constant current source.
Described thermopair selects for use temperature range at 200～25 ℃ T type thermopair, i.e. copper-constantan thermocouple; Described electro-motive force measurement line 8 is selected the platinum line of diameter 0.025mm for use, its conductivity height, good stability, the thermoelectric effect error that produces in the time of can reducing energising.
1.Seebeck the measurement of coefficient
Definition according to the Seebeck coefficient:
Apply a small temperature difference (4～15K) Δ T, promptly an end temperature is T at membraneous material sample two ends
1=T
0, the temperature of the other end is T
2=T
0+ Δ T, then membraneous material sample two ends Seebeck electromotive force V (T
1, T
2) be:
Bring bigger test error in order to reduce excessive difference variation to test result, get the temperature difference and between 4～15K, change.Treat to begin data acquisition when the cold and hot end temperature difference reaches 3K.
In the present embodiment, gather 50 data points, obtain straight slope, be the Seebeck coefficient value by least-squares algorithm linear fitting.
2. the measurement of conductivity
Four probe method is adopted in the measurement of conductivity, test philosophy is, when four metal probes are arranged in a line, and when being pressed on the thermoelectric film material with certain pressure, between peripheral two probes, feed electric current I, then between inboard two probes, produce potential difference (PD) U, calculate the conductivity of membraneous material according to following formula:
σ＝ΔX·I/U·A (4)
Wherein σ is conductivity (S/m), and Δ X is two needle tip spacings (m), and A is membraneous material sample sectional area (m
2).
For the deviation that the Peltier effect of eliminating thermoelectric material is brought, flow through the direction of current of sample in the measuring process by change, make the current opposite in direction that flows through the membraneous material sample for twice, and twice measurement result is averaged as final measurement.
In the present embodiment, the Zn that magnetron sputtering is prepared
4Sb
3The semiconductor thermoelectric membraneous material is tested.Apply temperature difference 4～15K at membraneous material sample two ends in the time of-50 ℃, the Seebeck coefficient value that records is 3.746 * 10
-3μ V/K.
In the present embodiment, the two needle tip spacing Δ X=0.0067m that record, Zn
4Sb
3The value of membraneous material sample sectional area is 3.556 * 10
-9m
2, the conductivity value that records is 1.020 * 10
8S/m.
Embodiment 2
Except following difference, other are as embodiment 1, and homemade BiSb semiconductor thermoelectric membraneous material is carried out the conductivity under the low temperature and the test of Seebeck coefficient.
Described thermopair selects for use temperature range at 200～25 ℃ T type thermopair, i.e. copper-constantan thermocouple;
Described electro-motive force measurement line 8 is selected the platinum line of diameter 0.025mm for use;
Getting the temperature difference changes between 4～10K;
In the present embodiment, described thin-film electro heating plate size is at 1/5th of membraneous material sample.
Gather 75 data points;
Two needle tip spacing Δ X=0.0078m, membraneous material sample sectional area A=2.503 * 10
-9m
2, the conductivity and the Seebeck coefficient value that record in the time of-120 ℃ are respectively 4.6003 * 10
4S/m, 0.823 μ V/K.
According to the semiconductor thermoelectric membraneous material of the present utility model conductivity at low temperatures and the proving installation of Seebeck coefficient, thermoelectric film material sample to be measured is placed in the proving installation, and proving installation moves in the enclosed vacuum environment; Temperature control system is used to regulate and control the environment temperature of proving installation and keeps temperature constant, realizes treating the low temperature thermoelectricity capability test of calorimetric conductive film material sample.Gather data-signal such as high low side temperature, electromotive force by data collecting instrument and be connected to computing machine, realize the control of whole test process, the processing of test data and the real-time demonstration of test data.The conductivity and the Seebeck coefficient of thermoelectric film material under the low temperature can accurately be measured by this system.
The low-temperature conductivity of semiconductor thermoelectric membraneous material of the present utility model and Seebeck coefficient measuring method and device, have simple, movement-less part, carry out lot of advantages such as conductivity and the measurement of Seebeck coefficient easily, can effectively realize the LNG cold energy thermo-electric generation membraneous material thermoelectricity capability parameter measurement of 80K to the room temperature.
Claims (4)
1. conductivity and the Seebeck coefficient proving installation under the semiconductor film material low temperature, whole testing device comprises temperature control unit, low-temperature test unit and the data acquisition unit of connection, it is characterized in that described temperature control unit comprises: Dewar container for liquefied nitrogen jar (1), the cryogenic vacuum container (2) that places Dewar container for liquefied nitrogen jar (1), the temperature controller (3) that is connected in Dewar container for liquefied nitrogen jar (1), thin-film electro heating plate (4) and constant current source (5);
Described low-temperature test unit comprises the electro-motive force measurement line (8) that the cold junction temperature thermocouple (6) that connects the thermoelectric film material sample (16) be arranged in cryogenic vacuum container (2) and hot junction temperature thermocouple (7) and temperature range 80K are suitable for to the room temperature;
Described data acquisition unit comprises via cold junction temperature thermocouple (6) and hot junction temperature thermocouple (7), the data acquisition unit (9) of electro-motive force measurement line (8) and the computing machine (10) that is connected thereof.
2. conductivity under the semiconductor film material low temperature according to claim 1 and Seebeck coefficient proving installation is characterized in that, described thermopair selects for use temperature range at 200～25 ℃ T type thermopair, i.e. copper-constantan thermocouple.
3. conductivity under the semiconductor film material low temperature according to claim 1 and Seebeck coefficient proving installation is characterized in that, the described electro-motive force measurement line selection platinum line of diameter 0.025 ~ 0.05mm.
4. conductivity under the semiconductor film material low temperature according to claim 1 and Seebeck coefficient proving installation, it is characterized in that, specimen holder (12) and sample support frame (11) are set in the described cryogenic vacuum container, end at described thermoelectric film material sample is provided with thin-film electro heating plate (4), described thin-film electro heating plate size is sixth ~ 1/4th of membraneous material sample, and described cryogenic vacuum container adopts feed-through collar (19) sealing.
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