CN102914560A - Device and method for measuring film thermoelectric performance parameters - Google Patents
Device and method for measuring film thermoelectric performance parameters Download PDFInfo
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- CN102914560A CN102914560A CN2012103905177A CN201210390517A CN102914560A CN 102914560 A CN102914560 A CN 102914560A CN 2012103905177 A CN2012103905177 A CN 2012103905177A CN 201210390517 A CN201210390517 A CN 201210390517A CN 102914560 A CN102914560 A CN 102914560A
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Abstract
The invention relates to a device and a method for measuring film thermoelectric performance parameters. The device mainly comprises a temperature measuring resistor, a heat sink, a current source, a carrier, a data acquiring device, a computer, a temperature control box and a pressure gauge. A sample to be measured is fixed on the carrier, an edge of the sample to be measured is connected with the heat sink, and the rest edges of the sample to be measured are connected with the temperature measuring resistor. Current required by the measuring device is controlled by the current source, and various performance parameters of a film thermoelectric material is monitored and recorded in real time by the data acquiring device. The device and the method for measuring film thermoelectric performance parameters have the advantages that thermal conductivity coefficient, seebeck coefficient, electric conductivity coefficient and thermoelectric merit figure of film thermoelectric materials in different shapes can be measured by the same device, and measured thermoelectric merit figure and formula computing value can be compared. Four-wire system is adopted in the whole process of measuring, and affection of contact resistance is practically avoided. The device and the method for measuring film thermoelectric performance parameters is simple, convenient to operate, small in size, high in measuring accuracy and vast in testing functions.
Description
Technical field
The invention belongs to the material properties test technical field, be specifically related to a kind of apparatus and method of measuring thermoelectric parameters of film, can measure simultaneously thermal conductivity κ, conductivityσ, Seebeck coefficient S and the thermoelectric figure of merit ZT of membraneous material.
Background technology
The efficient of thermoelectric material is directly proportional with nondimensional thermoelectric figure of merit:
ZT=
（1）
In the formula (1), S is Seebeck coefficient, and κ is thermal conductivity, and σ is conductivity, and T is absolute temperature.Searching improves the material of thermoelectricity capability, needs simple, effective characterizing method.Existing measurement mechanism and method, the problem that mainly has following several respects: 1. conductivity, thermal conductivity and the Seebeck coefficient of measuring respectively mostly in different ways film, the more employing four-wire system of conductivity or two-wire system are measured, thermal conductivity is sent out by steady state method or transient state and is obtained, and the measurement of Seebeck coefficient then adopts the two ends temperature differential method to measure usually.This with the inevasible religion of different device assessment overall thermal electrical property (being the thermoelectric figure of merit) the large error of professing, and still do not have relevant apparatus can obtain simultaneously thermal conductivity, conductivity, Seebeck coefficient and the thermoelectric figure of merit of membraneous material at present.2. more existing thermoelectricity capability evaluation systems can only be measured the performance of block thermoelectric material, and are then unable to do what one wishes for membraneous material.3. existing metering system needs strict preparation of samples, and measuring accuracy is not high.Along with the gradually filming of thermo-electric device, and the application of the thermoelectric film material such as superlattice, in the urgent need to the thermoelectricity capability evaluation method of a kind of accurate measurement membraneous material conductivity, thermal conductivity, Seebeck coefficient and thermoelectric figure of merit.
Summary of the invention
Defective for the prior art existence, the purpose of this invention is to provide a kind of apparatus and method of measuring thermoelectric parameters of film, can directly obtain by this method all relevant parameters, such as thermal conductivity κ, conductivityσ, Seebeck coefficient S and thermoelectric figure of merit.This method is insensitive to contact resistance.This method is easy to implement, and does not need a large amount of preparation of samples and most advanced and sophisticated equipment.
For achieving the above object, technical scheme of the present invention is:
A kind of device of measuring thermoelectric parameters of film comprises: temperature measuring equipment, data collector, heat sink, current source, objective table, computing machine, temperature-controlled box and voltage table, and it is characterized in that: described testing sample is fixed on the objective table; First contact point of testing sample connects heat sink, in addition second, third, the four or three contact point respectively connect respectively a temperature measuring equipment, power supply is connected to current source through temperature-controlled box, current source is connected to heat sink, temperature measuring equipment connects voltage table, current source and voltage table are connected to data collector, and the output of data collector is connected to computing machine; Current source provides temperature measuring equipment needed electric current, input direct-current or AC signal; Connect a voltage table between the 3rd contact point and the 4th contact point, be used for measuring two electric potential differences between the contact point; Utilize the required parameters of data collector Real-Time Monitoring record experiment; Utilize computing machine that data are carried out analyzing and processing, obtain thermal conductivity, conductivity, Seebeck coefficient and the thermoelectric figure of merit of film to be measured.
Above-mentioned temperature measuring equipment comprises Pt100, Pt10, Pt1000, Cu50 and Cu100 temperature detecting resistance, perhaps thermopair.
A kind of method of measuring thermoelectric parameters of film uses the device of above-mentioned measurement thermoelectric parameters of film to measure, and it is characterized in that: concrete operation step is:
1) prepare the film sample to be measured of several different-thickness, and cutting and described objective table 5 similar shapes;
2) film sample to be measured first make contact connection is heat sink, and other three contact points connect respectively an electric resistance heater;
3) to first, second two contact point input currents wherein, measure the voltage between other the 3rd, the 4 two contact point, again to the first, the 3rd contact point input current, measure the voltage between the second, the 4th contact point, the conductivityσ who extrapolates described testing sample according to the vanderburg equation;
4) since first make contact connected one heat sink, be thermo-contact unique in the sample, the hot-fluid between the first and second contact points is equivalent to the heat that well heater produces;
5) the second contact point is as thermal source, measure the temperature difference between the 3rd, the 4th contact point, again the 3rd contact point as thermal source, measure the temperature difference between the second, the 4th contact point, extrapolate the thermal conductivity κ of described testing sample according to the vanderburg equation;
6) temperature difference and the voltage between measurement the second, the 4th contact point is measured temperature difference and voltage between the third and fourth contact point, according to the definition of Seebeck coefficient, calculates the Seebeck coefficient S of film sample to be measured;
7) second and first make contact between respectively by the AC and DC electric current, measure the voltage between the third and fourth contact point, can extrapolate the ZT value of membraneous material according to formula, adopt a temperature-controlled box just can obtain the thermoelectric figure of merit of membraneous material under the different temperatures.
With the ZT value that obtains in the step 7) with step 3), 5), 6) the ZT value obtained of the conductivityσ, thermal conductivity κ, the Seebeck coefficient S that obtain respectively makes comparisons the degree of accuracy of testing result.
The present invention compared with prior art has following apparent outstanding feature and remarkable advantage: existing measurement mechanism, measure respectively mostly in different ways thermal conductivity, conductivity and the Seebeck coefficient of film, function singleness and be inconvenient to operate.Measurement mechanism volume of the present invention is little, cost is low, can directly obtain all relevant thermoelectric parameters, and insensitive to contact resistance, can mutually verify with the ZT value that (1) formula is obtained by the ZT value that this method directly measures, prove the correctness of acquired results.
Description of drawings
Fig. 1 is a kind of apparatus structure synoptic diagram (square) of measuring thermoelectric parameters of film
Fig. 2 is a kind of apparatus structure synoptic diagram (circle) of measuring thermoelectric parameters of film
Fig. 3 is a kind of apparatus structure synoptic diagram (irregular polygon) of measuring thermoelectric parameters of film
Fig. 4 is the conductivity of the Ni that records among the embodiment and the relation of temperature
Fig. 5 is the thermal conductivity of the Ni that records among the embodiment and the relation of temperature
Fig. 6 is the Seebeck coefficient of the Ni that records among the embodiment and the relation of temperature
Fig. 7 is the thermoelectric figure of merit of the Ni that records among the embodiment and the relation of temperature
Fig. 8 is the conductivity of the InSb that records among the embodiment and the relation of temperature
Fig. 9 is the Seebeck coefficient of the InSb that records among the embodiment and the relation of temperature
Figure 10 is the thermal conductivity of the InSb that records among the embodiment and the relation of temperature
Figure 11 is the thermoelectric figure of merit of the InSb that records among the embodiment and the relation of temperature.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment one:
Referring to Fig. 1 ~ Fig. 3, this measurement comprises: temperature measuring equipment (2,3,4), data collector (8), heat sink (1), current source (7), objective table (5), computing machine (9), temperature-controlled box (10) and voltage table (6) is characterized in that: described testing sample is fixed on the objective table (5); First contact point (1 ') of testing sample connects heat sink (1), in addition second, third, the four or three contact point (2 '), (3 '), (4 ') respectively connect respectively a temperature measuring equipment, power supply (11) is connected to current source (7) through temperature-controlled box (10), current source (7) is connected to heat sink (1), temperature measuring equipment a(2), temperature measuring equipment b(3) is connected with temperature measuring equipment c(4 and connects voltage table (6), current source (7) and voltage table (6) are connected to data collector (8), and the output of data collector (8) is connected to computing machine (9); Current source (7) provides temperature measuring equipment (2,3,4) needed electric current, input direct-current or AC signal; Connect a voltage table (6) between the 3rd contact point (3 ') and the 4th contact point (4 '), be used for measuring two electric potential differences between the contact point; Utilize the required parameters of data collector (8) Real-Time Monitoring record experiment; Utilize computing machine (9) that data are carried out analyzing and processing, obtain thermal conductivity, conductivity, Seebeck coefficient and the thermoelectric figure of merit of film to be measured.
Embodiment two:
Present embodiment and embodiment one are basic identical, and special feature is: described film to be measured can be homogeneous film or non-uniform film, and can be arbitrary shape.Temperature measuring equipment (2,3,4) is Pt100, Pt10, Pt1000, Cu50 or Cu100 temperature detecting resistance, or thermopair.Contact point is a series of contact point, and the number of described contact point is 4 ~ 20.The operation steps of measuring is as follows:
1) described sample need be cut into the shape similar to described objective table (5);
2) first contact point (1 ') of film sample to be measured connects heat sink (1), in addition second, third, the four or three contact point (2 ', 3 ', 4 ') connect respectively a temperature detecting resistance (2,3,4);
3) to described first, second two contact points (1 ', 2 ') input current, measure the voltage between other the 3rd, the 4 two contact point (3 ', 4 '), again to the first, the 3rd contact point (1 ', 3 ') input current, measure the voltage between the second, the 4th contact point (2 ', 4 '), according to vanderburg equation exp (π σ dR
21,43)+exp (π σ dR
31,42The conductivityσ of described testing sample is extrapolated in)=1;
4) because contact point (1 ') has connected one heat sink (1), be thermo-contact unique in the sample, the hot-fluid between first make contact (1 ') and the second contact point (2 ') is equivalent to the heat that well heater produces; The second contact point (2 ') is as thermal source, measure the temperature difference between the 3rd contact point (3 ') and the 4th contact point (4 '), again the 3rd contact point (3 ') as thermal source, measure the temperature difference between the second contact point (2 ') and the 4th contact point (4 '), according to vanderburg equation exp (π κ d
)+exp (π κ d
The thermal conductivity κ of described testing sample is extrapolated in)=1;
5) temperature difference and the voltage between measurement the second contact point (2 ') and the 4th contact point (4 ') is measured temperature difference and voltage between the 3rd contact point (3 ') and the 4th contact point (4 '), according to the definition S=of Seebeck coefficient
=
Calculate the Seebeck coefficient S of film sample to be measured;
6) between the second contact point (2 ') and the first make contact (1 ') respectively by the AC and DC electric current, measure the voltage between the 3rd contact point (3 ') and the 4th contact point (4 '), according to formula ZT=
=
Can directly extrapolate the ZT value of membraneous material, adopt a temperature-controlled box (10) just can obtain the thermoelectric figure of merit of membraneous material under the different temperatures.
7) with the ZT value that obtains in the step 6) with step 3), 4), 5) in the ZT value obtained of the conductivityσ, thermal conductivity κ, the Seebeck coefficient S that obtain make comparisons the degree of accuracy of testing result.
Embodiment three:
The method of this measurement thermoelectric parameters of film is used the device of above-mentioned measurement thermoelectric parameters of film, and the implementation step of this method is:
1) prepare the film sample to be measured of several different-thickness, and square similar to described objective table (5) of cutting;
2) film sample to be measured one of limit connection is heat sink, and other three limits connect respectively a heating resistor and thermopair;
3) to wherein first make contact (1 ') and the second contact point (2 ') input current, measure the voltage between the 3rd contact point (3 ') and the 4th contact point (4 '), again to the first, the 3rd contact point (1 ' and 3 ') input current, measure the voltage between the second, the 4th contact point (2 ', 4 '), the conductivityσ who extrapolates described testing sample according to the vanderburg equation;
4) since first make contact (1 ') connected one heat sink, be thermo-contact unique in the sample, the hot-fluid between the first and second contact points (1 ', 2 ') is equivalent to the heat that well heater produces;
5) the second contact point (2 ') is as thermal source, measure the temperature difference between the third and fourth contact point (3 ', 4 '), again the 3rd contact point (3 ') as thermal source, measure the temperature difference between the second and the 4th contact point (2 ', 4 '), extrapolate the thermal conductivity κ of described testing sample according to the vanderburg equation;
6) measure temperature difference and voltage between the second and the 4th contact point (2 ', 4 '), measure temperature difference and voltage between the third and fourth contact point (3 ', 4 '), according to the definition of Seebeck coefficient, calculate the Seebeck coefficient S of film sample to be measured;
7) by second and the AC and DC electric current of first make contact (2 ', 1 '), measure the voltage between the third and fourth contact point (3 ', 4 '), can extrapolate the ZT value of membraneous material according to formula, adopt a temperature-controlled box (10) just can obtain the thermoelectric figure of merit of membraneous material under the different temperatures.
Embodiment four:
At first, prepare the Ni film sample of several different-thickness, and be cut into similar to described objective table (5) square.
Sample is placed on the objective table, first make contact (1 ') connect one heat sink, in addition second, third, the four or three contact point (2 ', 3 ', 4 ') connect respectively 3 pt100 heating resistors.
The enforcement principle of step 3) is: for first resistance measurement, and an electric current I
21From the second contact point (2 ') to first make contact (1 '), can measure the electric potential difference U between two other contact
43. so just can obtain R
21,43=
. another one contact resistance R
31,42=
, by an electric current from the 3rd contact point (3 ') to first make contact (1 '), the electric potential difference between the 4th contact point (4 ') and the second contact point (2 ') obtains.If know the thickness d of film, just can obtain σ by separating the vanderburg equation:
exp( πσdR
21,43) + exp( πσdR
31,42) = 1. （2）
The enforcement principle of step 5) is: utilize the pt100 resistance of the second contact point (2 ') to cause one from the hot-fluid P of the second contact point (2 ') to heat sink (1) as contact heater
21Because heat sink (1) is thermo-contact unique in the sample, hot-fluid P
21The power consumption that is equivalent to the heat of well heater generation or is equivalent to measure easily.By the 3rd contact point (3 ') and the 4th contact point (4 ') as thermopair (such as Fig. 1), temperature difference Δ T
43Can determine simply by resistance and the resistance temperature calibration of measuring the 3rd contact point (3 ') and the 4th contact point (4 ').Hot-fluid P
21With temperature difference Δ T
43Provided first thermal resistance
. then adopt the 3rd contact point (3 ') as thermal source, the 4th contact point (4 ') and the second contact point (2 ') are as thermopair.This has provided second thermal resistance
. if the thickness d of film knows,
Substitution vanderburg equation:
exp( πκd
) + exp( πκd
) = 1. （3）
Just can be in the hope of thermal conductivity coefficient κ.
The enforcement principle of step 6) is: two temperature difference T that measured by step 5)
43With Δ T
42Two corresponding voltage U have been measured in addition
43And U
42So Seebeck coefficient S just can directly obtain:
S=
=
（4）
The enforcement principle of step 7) is: obtain electric current by thermoelectric material and usually can cause two kinds of effects.The first, because the Ohmage of material an electric potential difference occurs, and 1/ σ is directly proportional.In addition, electric current also can produce a thermograde (paltie effect), causes successively extra voltage drop (Seebeck coefficient).The contribution of this pure thermoelectricity and
Be directly proportional.Fortunately, two kinds of contributions need the different time to reach fully effectively.The appearance of ohmic voltage drop is instantaneous, contributes needs to reach several seconds for the thermoelectricity of macroscopical sample.Therefore, measure AC resistance (R
AC) be under enough high frequencies, only to survey Ohmage, on the contrary direct current resistance (R
DC) reflected ohm and response thermoelectricity.Thermoelectric sample AC measurment is for determining that from equation σ is necessary.R
DC-R
ACObtain the contribution of net heat electricity, divided by R
ACJust can obtain thermoelectric figure of merit ZT.
By the AC and DC electric current of the second contact point (2 ') to first make contact (1 '), measuring voltage U
43, can obtain respectively resistance
With
,
ZT=
=
（5）
So just can obtain thermal conductivity κ, conductivityσ, Seebeck coefficient S and the thermoelectric figure of merit ZT of film.
Embodiment five:
At first, prepare the InSb film sample of several different-thickness, and be cut into similar to described objective table (5) square.
Sample is placed on the objective table, first make contact (1 ') connect one heat sink, in addition second, third, the four or three contact point (2 ', 3 ', 4 ') connect respectively 3 pt100 heating resistors.
The enforcement principle of step 3) is: for first resistance measurement, and an electric current I
21From the second contact point (2 ') to first make contact (1 '), can measure the electric potential difference U between two other contact
43. so just can obtain R
21,43=
. another one contact resistance R
31,42=
, by an electric current from the 3rd contact point (3 ') to first make contact (1 '), the electric potential difference between the 4th contact point (4 ') and the second contact point (2 ') obtains.If know the thickness d of film, just can obtain σ by separating the vanderburg equation:
exp( πσdR
21,43) + exp( πσdR
31,42) = 1. （2）
The enforcement principle of step 5) is: utilize the pt100 resistance of the second contact point (2 ') to cause one from the hot-fluid P of the second contact point (2 ') to heat sink (1) as contact heater
21Because heat sink (1) is thermo-contact unique in the sample, hot-fluid P
21The power consumption that is equivalent to the heat of well heater generation or is equivalent to measure easily.By contact point (3) and contact point (4) as thermopair (such as Fig. 1), temperature difference Δ T
43Can determine simply by resistance and the resistance temperature calibration of measuring the 3rd contact point (3 ') and the 4th contact point (4 ').Hot-fluid P
21With temperature difference Δ T
43Provided first thermal resistance
. then adopt the 3rd contact point (3 ') as thermal source, the 4th contact point (4 ') and the second contact point (2 ') are as thermopair.This has provided second thermal resistance
. if the thickness d of film knows,
Substitution vanderburg equation:
exp( πκd
) + exp( πκd
) = 1. （3）
Just can be in the hope of thermal conductivity coefficient κ.
The enforcement principle of step 6) is: two temperature difference T that measured by step 5)
43With Δ T
42Two corresponding voltage U have been measured in addition
43And U
42So Seebeck coefficient S just can directly obtain:
S=
=
（4）
The enforcement principle of step 7) is: obtain electric current by thermoelectric material and usually can cause two kinds of effects.The first, because the Ohmage of material an electric potential difference occurs, and 1/ σ is directly proportional.In addition, electric current also can produce a thermograde (paltie effect), causes successively extra voltage drop (Seebeck coefficient).The contribution of this pure thermoelectricity and
Be directly proportional.Fortunately, two kinds of contributions need the different time to reach fully effectively.The appearance of ohmic voltage drop is instantaneous, contributes needs to reach several seconds for the thermoelectricity of macroscopical sample.Therefore, measure AC resistance (R
AC) be under enough high frequencies, only to survey Ohmage, on the contrary direct current resistance (R
DC) reflected ohm and response thermoelectricity.Thermoelectric sample AC measurment is for determining that from equation σ is necessary.R
DC-R
ACObtain the contribution of net heat electricity, divided by R
ACJust can obtain thermoelectric figure of merit ZT.
By the AC and DC electric current of the second contact point (2 ') to first make contact (1 '), measuring voltage U
43, can obtain respectively resistance
With
,
ZT=
=
（5）
So just can obtain thermal conductivity κ, conductivityσ, Seebeck coefficient S and the thermoelectric figure of merit ZT of film.
Claims (5)
1. device of measuring thermoelectric parameters of film, comprise: temperature measuring equipment (2,3,4), data collector (8), heat sink (1), current source (7), objective table (5), computing machine (9), temperature-controlled box (10) and voltage table (6) is characterized in that: described testing sample is fixed on the objective table (5); First contact point (1 ') of testing sample connects heat sink (1), in addition second, third, the four or three contact point (2 '), (3 '), (4 ') respectively connect respectively a temperature measuring equipment, power supply (11) is connected to current source (7) through temperature-controlled box (10), current source (7) is connected to heat sink (1), temperature measuring equipment a(2), temperature measuring equipment b(3) is connected with temperature measuring equipment c(4 and connects voltage table (6), current source (7) and voltage table (6) are connected to data collector (8), and the output of data collector (8) is connected to computing machine (9); Current source (7) provides temperature measuring equipment (2,3,4) needed electric current, input direct-current or AC signal; Connect a voltage table (6) between the 3rd contact point (3 ') and the 4th contact point (4 '), be used for measuring two electric potential differences between the contact point; Utilize the required parameters of data collector (8) Real-Time Monitoring record experiment; Utilize computing machine (9) that data are carried out analyzing and processing, obtain thermal conductivity, conductivity, Seebeck coefficient and the thermoelectric figure of merit of film to be measured.
2. a kind of device of measuring thermoelectric parameters of film according to claim 1, it is characterized in that: described film to be measured can be homogeneous film or non-uniform film, and can be arbitrary shape.
3. a kind of device of measuring thermoelectric parameters of film according to claim 1, it is characterized in that: described temperature measuring equipment (2,3,4) is Pt100, Pt10, Pt1000, Cu50 or Cu100 temperature detecting resistance, or thermopair.
4. a kind of device of measuring thermoelectric parameters of film according to claim 1, it is characterized in that: contact point is a series of contact point, the number of described contact point is 4 ~ 20.
5. a device of measuring thermoelectric parameters of film adopts the device of measurement thermoelectric parameters of film according to claim 1 to measure, and it is characterized in that: the operation steps of measurement is as follows:
1) described sample need be cut into the shape similar to described objective table (5);
2) first contact point (1 ') of film sample to be measured connects heat sink (1), in addition second, third, the four or three contact point (2 ', 3 ', 4 ') connect respectively a temperature detecting resistance (2,3,4);
3) to described first, second two contact points (1 ', 2 ') input current, measure the voltage between other the 3rd, the 4 two contact point (3 ', 4 '), again to the first, the 3rd contact point (1 ', 3 ') input current, measure the voltage between the second, the 4th contact point (2 ', 4 '), according to vanderburg equation exp (π σ dR
21,43)+exp (π σ dR
31,42The conductivityσ of described testing sample is extrapolated in)=1;
4) because contact point (1 ') has connected one heat sink (1), be thermo-contact unique in the sample, the hot-fluid between first make contact (1 ') and the second contact point (2 ') is equivalent to the heat that well heater produces; The second contact point (2 ') is as thermal source, measure the temperature difference between the 3rd contact point (3 ') and the 4th contact point (4 '), again the 3rd contact point (3 ') as thermal source, measure the temperature difference between the second contact point (2 ') and the 4th contact point (4 '), according to vanderburg equation exp (π κ d
)+exp (π κ d
The thermal conductivity κ of described testing sample is extrapolated in)=1;
5) temperature difference and the voltage between measurement the second contact point (2 ') and the 4th contact point (4 ') is measured temperature difference and voltage between the 3rd contact point (3 ') and the 4th contact point (4 '), according to the definition S=of Seebeck coefficient
=
Calculate the Seebeck coefficient S of film sample to be measured;
6) between the second contact point (2 ') and the first make contact (1 ') respectively by the AC and DC electric current, measure the voltage between the 3rd contact point (3 ') and the 4th contact point (4 '), according to formula ZT=
=
Can directly extrapolate the ZT value of membraneous material, adopt a temperature-controlled box (10) just can obtain the thermoelectric figure of merit of membraneous material under the different temperatures;
7) with the ZT value that obtains in the step 6) with step 3), 4), 5) in the ZT value obtained of the conductivityσ, thermal conductivity κ, the Seebeck coefficient S that obtain make comparisons the degree of accuracy of testing result.
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| CN113758961A (en) * | 2020-06-02 | 2021-12-07 | 厦门稀土材料研究所 | Horizontal test equipment and method for thermoelectric material Seebeck coefficient and electric conductivity |
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