CN107255650A - One kind is on thermoelectric material Seebeck coefficient testing methods - Google Patents
One kind is on thermoelectric material Seebeck coefficient testing methods Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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Abstract
The invention discloses a kind of thermoelectric material Seebeck coefficient testing methods, the characteristics of this method combines steady state method and dynamic method mainly includes the following steps that：Step one：According to dynamic method of testing, the low-temperature end temperature of sample is kept to be basically unchanged, control temperature end is rapidly heated, temperature difference T and electrical potential difference Δ U, linear fit Δ U and Δ T that two ends are recorded in real time relation are Δ U=α1*ΔT+Δu；Step 2：According to above formula, Δ U is obtained as Δ T=0Partially, or Δ U=0 obtains Δ TPartially, both at systematic error；Step 3：Keep sample average temperature T0And two ends the temperature difference it is constant between 5~10K when, electrical potential difference Δ U is measured respectively according to steady state test method0With temperature difference T0, according to formulaBring Δ U intoPartiallyOr Δ TPartiallyObtain αTruly.The present invention, which is realized, accurately to be measured Seebeck coefficients, eliminates the systematic error that test process is introduced；Reduce requirement to test condition, and for grinding certainly, the data acquisition of to be developed and existing business equipment and the formulation of processing mode and optimization there is high reference.
Description
Technical field：The invention belongs to the technical field of material electrical performance testing, specially a kind of thermoelectric material
Seebeck coefficient testing methods.
Background technology：
Thermoelectric material is hopeful to solve the energy that is faced of Present Global and the critical function material of environmental crisis as a kind of
Expect and receive much concern, its energy conversion efficiency has direct relation with conducting material thermoelectricity performance.It is current general excellent by dimensionless thermoelectricity
Value ZT weighs the quality of conducting material thermoelectricity performance, and ZT expression is as shown in formula 1.：
ZT=α2ρ-1κ-1T
Wherein α is Seebeck coefficients, and ρ is resistivity, and κ is thermal conductivity, and T is thermodynamic temperature.α, ρ and κ are material
Physical parameter, and it is relevant with temperature.Therefore, α, ρ and κ variation with temperature relation are accurately tested, conducting material thermoelectricity performance is commented
Sentence significant.
Material Seebeck coefficient α and electricalresistivityρ that current commercial commercial instrument is typically surveyed simultaneously.Current more maturation
Test commercial instrument has：The LRS of German Linseis companies production, the ZEM of ULVAC-RIKO companies of Japan production, the U.S.
The PPMS of Quantum Design companies production, the Namicro of domestic Wuhan Jia Yitong companies production, Ke Rui Europe, Beijing science and technology have
CTA of limit company production etc., and all improve Seebeck coefficients, resistivity test system in continuous release.But commented according to its own
Estimate, there is error in the test of these two aspects.
The content of the invention
It is an object of the invention to provide a kind of thermoelectric material Seebeck coefficient testing methods, material Seebeck systems are improved
The accuracy of number test, simplifies test process, reduces testing cost.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of thermoelectric material Seebeck coefficient testing methods, comprising dynamic method of testing and steady state test method, the dynamic is surveyed
Examination method and steady state test method contain Research on Automatic Measuring System of Temperature and voltage testing system, further comprising the steps of：
Step one：Keep the low-temperature end temperature of testing sample to be basically unchanged, control the temperature end temperature of testing sample quick
Rise, according to dynamic measurement method, with the synchronous two ends of record testing sample in real time of Research on Automatic Measuring System of Temperature and voltage testing system
Temperature difference T and thermoelectrical potential Δ U, by linear fit Δ U and Δ T relation, tries to achieve the relationship of the two formula Δ U=α1* Δ T+ Δs u,
The wherein systematic error of Δ u unknown sizes；
Step 2：Try to achieve when temperature is T0When due to the introduced Δ U of systematic errorPartiallyWith Δ TPartially, according to formula Δ U=α1*
Δ T+ Δ u, Δ U can be tried to achieve as Δ T=0Partially, or Δ U=0 can obtain Δ TPartially；
Step 3：Keep testing sample temperature T0, two ends temperature difference T it is constant between 5~10K when, according to stable state survey
Amount method uses voltage testing system and Research on Automatic Measuring System of Temperature synchronous acquisition sample two ends electrical potential difference Δ U respectively0With temperature difference T0, root
According to formulaBy Δ UPartiallyOr Δ TPartiallyBring into, solution obtains αTruly。
Further, it is raising measuring accuracy, the Δ U in step 30Using selection average potential difference, the method tried to achieve is
Keep testing sample temperature T0And test temperature difference T0In the case of being basically unchanged, the electricity that repeatedly (n times) measurement sample two ends are produced
Potential difference Δ Ui, by the average potential for calculating n testAccording to formula,Understand, it is many
The secondary method averaged that measures can be reduced effectively because of the error that potential test is inaccurate and introduces.
The beneficial effects of the invention are as follows：
Realize and Seebeck coefficients are accurately measured, eliminate because method of testing imperfection and test equipment precision be not high
And the systematic error introduced, i.e. Δ UPartiallyOr Δ TPartially；The requirement to test condition, cheap common thermocouple are reduced simultaneously
(or self-control) can also be used in actual measurement process, reduce testing cost；In addition, the present invention is set for most grind certainly
The formulation and improvement of the data processing processing mode of new equipment standby, to be developed and existing commercial instrument also there is higher reference to anticipate
Justice.
Brief description of the drawings
Fig. 1 is the present invention based on the dynamic true electrical potential difference-temperature difference of method of testing (Δ V- Δ T), the test electrical potential difference-temperature difference (Δ
U- Δ T) linear fit schematic diagram.
Fig. 2 is stable to certain performance but α of 1# samples of unknown Seebeck coefficients steady using 1# thermocouples for the present invention
State method is tested and the test of data processed result and the inventive method and data processed result contrast legend.
Fig. 3 utilizes 2# thermocouples, steady state method test and the inventive method 2# sample Seebeck stable to performance for the present invention
Coefficient is tested and data processed result.
Fig. 4 is 3# sample of the present invention to performance stabilization, and commercial instrument and the inventive method test Seebeck is respectively adopted
The Comparative result of coefficient.
Fig. 5 is standard sample of the present invention to a certain known Seebeck coefficients, is utilized respectively different commercial instruments and Ben Fa
Bright method test result contrast.
Fig. 6 is invention test philosophy figure.
Embodiment
Embodiments of the invention are described in detail below in conjunction with accompanying drawing, but the present invention can be defined by the claims
Implement with the multitude of different ways of covering.
The current general quality that conducting material thermoelectricity performance is weighed by dimensionless thermoelectric figure of merit ZT, and ZT expression such as formula 1.
It is shown：
ZT=α2ρ-1κ-1T formula 1.
Wherein α is Seebeck coefficients, and ρ is resistivity, and κ is thermal conductivity, and T is thermodynamic temperature.α, ρ and κ are material
Physical parameter, and it is relevant with temperature.Therefore, α, ρ and κ variation with temperature relation are accurately tested, conducting material thermoelectricity performance is commented
Sentence significant.
To the measure Main Basiss Seebeck effects of material Seebeck coefficient, that is, the two ends that there is temperature difference dT samples can be produced
Heat potential dU, expression formula is as follows：
α=dU/dT formula 2.
Known according to formula 2.：If sample one end temperature is T1=T0- Δ T/2, other end temperature is T2=T0+ Δ T/2, then
The electrical potential difference Δ U (T of generation1, T2)：
In T0It is as follows that place carries out Taylor expansion to α (T)：
Formula 4. is substituted into formula 3., obtained
Thus seem：As Δ T/2T0When sufficiently small, then α (T0)=Δ U (T1,T2)/ΔT。
Based on above-mentioned analysis, two kinds can be generally divided into material Seebeck coefficient method for measuring at present, one kind is
State method, one kind is steady state method.Dynamic method, the i.e. change according to Seebeck coefficients under slight temperature change be not obvious, can be with
It is approximately considered in the range of temperature of very little, the thermoelectrical potential Δ U produced by sample and temperature difference T has linear relationship, i.e.,
Δ U=α * Δ T formula 6.
So in the case where ensureing that low-temperature end temperature change is little, quickly raise temperature end temperature, test Δ U and Δ
T, using least square method or other method fitted figure as slope, i.e., tries to achieve the Seebeck coefficients of material using dynamic method of testing.
Steady state method refers to when material two ends have moderately stable temperature difference T, determines the thermoelectrical potential Δ U produced, utilizes
Formula 7. calculates the Seebeck coefficients for obtaining material：
α=Δ U/ Δ T formula 7.
It is however noted that：When using steady state method test, it can be seen from Seebeck coefficient definitions：In potential
Under the premise of difference test accurately, tested temperature difference T is smaller, then measured Seebeck coefficients are closer to definition value；But
It is that the temperature difference is smaller, measurement error is bigger, therefore temperature difference T is general between 5~10K, to reduce not knowing because of temperature test
Property and the error caused, while an electrical potential difference that is sufficiently large and easily detecting can be obtained again.
Which kind of, no matter method of testing, during test Seebeck coefficients, it is required for gathering data below：Sample hot junction
Temperature Th, cold junction temperature Tc, hot junction potential Uh, cold end potential Uc, or directly measure the electrical potential difference Δ U between cold and hot end.It is (logical
In the case of often, the temperature of material at high temperature end and low-temperature end is measured using a pair of thermoelectricity occasionally thermal resistance, and thermocouple is wherein
One lead is as voltage electrode, for measuring the electrical potential difference Δ U of generation) so material two ends exist the temperature difference be Δ T=Th-
Tc, temperature corresponding with Seebeck coefficients is T0=(Th+Tc)/2.As can be seen here, cause material Seebeck coefficient test inaccurate
True property ηαFollowing formula can be expressed as：
|ηα|=| ηΔU|/ΔU+|ηΔT|/Δ T formula 8.
Some systematic errors introduced by instrumental sensitivity or precision can be reduced by improving equipment self performance,
It is noted that be：The error and cold only effect that thermal contact resistance is introduced can directly result in two thermocouple assay temperature and sample
Immesurable contact temperature difference T is there is between true temperaturehWith Δ TcIf, the test temperature difference T of sample, then the actual temperature difference
Should be Δ T+ (Δ Th-ΔTc), wherein Δ TPartially=Δ Th-ΔTc.So, found in test process：As test temperature difference T
When=0, and sample two ends are in the presence of an electrical potential difference Δ U being not zeroPartially.And thermocouple welding situation, solder joint are contacted with sample
Situation, the disposition of sample surfaces and lead node etc. can all cause the error during temperature test, and it is difficult to ensure that
The Δ T that two thermocouple assays are producedhWith Δ TcUnanimously.
For the assessment of dynamic method of testing error：Assuming that the Δ T of two thermocouple assaysh、ΔTcStablize relatively, i.e., one
Do not fluctuated with ambient temperature change in secondary heating test process, that is,
So tested using dynamic method, it is possible to directly eliminate because of the error that temperature test is inaccurate and introduces.But
On the premise of this method is built upon " small range temperature change influences little to material Seebeck coefficient ".And actual test table
It is bright：Even if the small temperature difference (1~3K) changes again, slight change can occur for the Seebeck coefficients of material, therefore Δ U- Δs T
Linear relationship is a kind of approximate, therefore the slope being fitted (tests Seebeck coefficient SsSurvey) and the true Seebeck systems of material
Number S0Error is certainly existed, therefore the systematic error of this method is certainly existed.
It is now assumed that testing a certain p-type thermoelectric material, and its true Seebeck coefficient S using dynamic method0With temperature rise
Increase, then test electrical potential difference Δ UiWith true electrical potential difference Δ ViBetween certainly exist a systematic error delta ui, and with test
Seebeck coefficient SsSurveyBetween there is following relationship：
ΔVi=Δ Ui-Δui=Δ Ui–(SSurvey–S0) Δ T formula 10.
So corresponding gathered data should be as shown in table 1.：
The true electrical potential difference of table 1. and test electrical potential difference corresponding table
Using least-squares algorithm linear fitting result as shown in Figure 1, the accompanying drawing is obtained according to theory analysis：
Known by accompanying drawing 1, the test actual Seebeck coefficients of Seebeck coefficients are bigger than normal.Profit in the case of other can similarly be analyzed
The deviation tested with dynamic method between Seebeck coefficients test result and actual value, as shown in table 2.：
The dynamic method of table 2. test Seebeck system errors statistics
And tested for steady state method, go to calculate material Seebeck coefficient according only to formula 7., it is impossible to eliminate Δ UPartiallyOr Δ TPartially
Influence, so an additional Seebeck coefficient deltas α will necessarily be introduced, test Seebeck factor alphasTestIt can be asked by formula 11.
, and the true Seebeck factor alphas of materialTrulyExpression formula can be provided by formula 12..
Wherein Δ U0For test electrical potential difference, Δ T0For the test temperature difference.And Δ α=αTruly-αTest。
In summary, in addition to the systematic error introduced in method of testing principle, other main errors are mainly derived from
Test equipment precision not enough, there is at following 2 points：
(1) because of thermocouple precision, thermal contact resistance, asynchronous, signal transformed error of temperature acquisition of temp measuring system etc. and make
Into temperature test ηΔT；
(2) by voltage testing system response speed and precision, and the asynchronous electrical potential difference test error caused is gathered
ηΔU；
And know, it is extremely harsh to thermocouple requirement in order to reduce test error in commercial instrument, therefore commercially available business instrument
The thermocouple price of device is sufficiently expensive.
The method of testing collection dynamic method and the respective advantage of steady state method of the present invention.Can be with Δ U by above-mentioned analysisPartiallyOr Δ
TPartiallyIt can be obtained by dynamic method.I.e. in dynamic method test, using the linear relationship between Δ U and Δ T, i.e.,
Δ U=α * Δ T+ Δ u formula 13.
Δ U can be tried to achieve as Δ T=0Partially, or Δ U=0 can obtain Δ TPartially, and the two meets formula 14..
ΔUPartially=-α * Δs TPartially, formula 14.
Know according to another formula 9.：In certain range of temperature, Δ TPartiallyChange can ignore.So for steady state method
In test process, it can be tried to achieve first with dynamic method in temperature T0Under Δ UPartiallyOr Δ TPartially, steady state method test is recycled in temperature T0
The lower temperature difference is the electrical potential difference Δ U produced by Δ T, and the Seebeck coefficients of material, this method can be accurately calculated according to formula 11.
It can eliminate because of the systematic error that the incomplete and test equipment precision of method of testing is not high and introduces.
Know further accordance with formula 15.：If keeping sample temperature T0And test temperature difference T0In the case of being basically unchanged, multiple (n
It is secondary) measure the electrical potential difference Δ U that sample two ends are producedi, by the average potential for calculating n testCan effectively it reduce because of electricity
The error that gesture test is inaccurate and introduces.
A kind of thermoelectric material Seebeck coefficient testing methods, including steady-state method of test and dynamic testing method, in addition to
Following steps：
Step one：Keep the low-temperature end temperature of testing sample to be basically unchanged, control the temperature end temperature of testing sample quick
Rise, according to dynamic testing method, with the synchronous two ends of record testing sample in real time of Research on Automatic Measuring System of Temperature and voltage testing system
Temperature difference T and thermoelectrical potential Δ U, by linear fit Δ U and Δ T relation, tries to achieve the relationship of the two formula Δ U=α1* Δ T+ Δs u,
Wherein Δ u is systematic error；
Step 2：According to formula Δ U=α1* Δ T+ Δs u, Δ U can be tried to achieve as Δ T=0Partially, or Δ U=0 can obtain
ΔTPartially；
Step 3：Keep testing sample temperature T0, two ends temperature difference T it is constant between 5~10K when, according to stable state survey
Method for testing uses voltage testing system and Research on Automatic Measuring System of Temperature synchronous acquisition sample two ends electrical potential difference Δ U respectively0With temperature difference T0, root
According to formulaBy Δ UPartiallyOr Δ TPartiallyBring into, solution obtains αTruly.Wherein Δ U0It is flat using selection
Equal electrical potential difference, the method tried to achieve is holding testing sample temperature T0And test temperature difference T0In the case of being basically unchanged, multiple (n
It is secondary) measure the electrical potential difference Δ U that sample two ends are producedi, by the average potential for calculating n testCan effectively it reduce because of electricity
The error that gesture test is inaccurate and introduces, formula,
Carry out being tested in test equipment as shown in Figure 6 using testing sample now, pressed from both sides using left and right copper seat 1
Hold testing sample 3, be provided with calandria 2 on copper seat 1, the energization of wire 6 is heated, by adjusting heated current to control sample
Product two ends temperature, wherein carrying out thermometric (including thermocouple has magnetic pole 4, and thermocouple is without magnetic pole 5) using K-type thermocouple, is connected to
High/low temperature end temperature is recorded on temp measuring system；There is magnetic pole 4 as voltage electrode with thermocouple, be connected to System of voltage acquisition, adopt
The electrical potential difference that collection high and low temperature end is produced by the temperature difference；Another copper seat acts also as electric current pole, and current feed 7 is connected respectively, is ensureing material
In the case that material is temperature-resistant, by 7 input current signals, and System of voltage acquisition collection voltages signal at 4 is utilized, you can
According to calculating resistivity of material.Test result shown in accompanying drawing 2~5.
Particular embodiments disclosed above is merely illustrative, and with the help of instructing herein, those skilled in the art can
To change and put into practice the application in different but equivalent way.It is therefore apparent that particular embodiments disclosed above can be changed
Become or change, and all these modifications are considered as falling in the scope and spirit of the present application.Therefore, protection sought herein model
Enclose as being proposed in the description.It is clear that the application for having been described above and illustrating has significant advantage.Although this
Application is shown in a limited number of forms, but it is not limited only to these forms, and is appropriate for various changes and modification and not
Deviate its spirit.
Claims (2)
1. a kind of thermoelectric material Seebeck coefficient testing methods, contain dynamic method of testing and steady state test method, the dynamic is surveyed
Examination method and steady state test method contain Research on Automatic Measuring System of Temperature and voltage testing system, it is characterised in that further comprising the steps of：
Step one：Keep the low-temperature end temperature of testing sample to be basically unchanged, control the temperature end temperature rapid increase of testing sample,
According to dynamic method of testing, with the temperature difference T at the synchronous two ends of record testing sample in real time of Research on Automatic Measuring System of Temperature and voltage testing system
With thermoelectrical potential Δ U, by linear fit Δ U and Δ T relation, the relationship of the two formula Δ U=α are tried to achieve1* Δ T+ Δs u, wherein Δ u
The systematic error of unknown size；
Step 2：Try to achieve when temperature is T0When due to the introduced Δ U of systematic errorPartiallyWith Δ TPartially, according to formula Δ U=α1*ΔT+
Δ u, Δ U can be tried to achieve as Δ T=0Partially, or Δ U=0 can obtain Δ TPartially；
Step 3：Keep testing sample temperature T0, two ends temperature difference T it is constant between 5~10K when, according to steady state test method point
Yong not voltage testing system and Research on Automatic Measuring System of Temperature synchronous acquisition sample two ends electrical potential difference Δ U0With temperature difference T0, according to formulaBy Δ UPartiallyOr Δ TPartiallyBring into, try to achieve αTruly。
2. thermoelectric material Seebeck coefficient testing methods according to claim 1, it is characterised in that：Used in step 3
Δ U0For average potential difference, the method tried to achieve is to maintain testing sample temperature T0And test temperature difference T0Situation about being basically unchanged
Under, the electrical potential difference Δ U that repeatedly (n times) measurement sample two ends are producedi, by the average potential for calculating n testAccording to public affairs
Formula,Understand, repeatedly measuring the method averaged can effectively reduce because potential test is inaccurate
And the error introduced.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109613051A (en) * | 2018-10-24 | 2019-04-12 | 武汉嘉仪通科技有限公司 | A kind of device and method using method of comparison measurement material Seebeck coefficient |
| CN109781781A (en) * | 2019-01-18 | 2019-05-21 | 中国工程物理研究院材料研究所 | A kind of alternating-current measurement device and method of Seebeck coefficient |
| CN110530927A (en) * | 2019-10-10 | 2019-12-03 | 王雪强 | A kind of thermoelectric material Seebeck coefficient test device and method |
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