CN206990487U - The thermoelectricity capability measuring system of nano material - Google Patents
The thermoelectricity capability measuring system of nano material Download PDFInfo
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- CN206990487U CN206990487U CN201720450926.XU CN201720450926U CN206990487U CN 206990487 U CN206990487 U CN 206990487U CN 201720450926 U CN201720450926 U CN 201720450926U CN 206990487 U CN206990487 U CN 206990487U
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Abstract
The utility model proposes a kind of thermoelectricity capability measuring system of nano material, including：Substrate；First be arranged in substrate is suspended to the 3rd and taken, and the first suspension takes to suspend to take with second to be connected by hot line, and testing sample is arranged at the 3rd suspension and taken between the central point of hot line；Harvester, harvester suspends to take with first to the 3rd respectively to be connected, to gather the terminal voltage of the terminal voltage of hot line and testing sample.The measuring system can realize the purpose of accurate measurement thermoelectricity capability, simple easily realization to measure electricity, heat and the Thermoelectric Physicss property of nanotube sample on same sample.
Description
Technical field
It the utility model is related to micron, nano material electrology characteristic, thermal conduction characteristic, thermoelectric conversion Performance Testing Technology neck
Domain, the thermoelectricity capability measuring system of more particularly to a kind of nano material.
Background technology
In terms of the heat to electricity conversion performance measurement of nano material, mainly there is following several method at present：(1) direct measurement
Method：Between nano material is overlapped on into micro-heater, the temperature difference is established at nano material both ends by electrically heated method, measurement is received
Rice material electromotive force as caused by the temperature difference, obtains Seebeck coefficients；(2) AFM-exchange current flow method：Utilize atom
The thermoelectricity detection probe of force microscope, the temperature difference is established at print both ends, then by detecting the 2 ω voltages and 3 ω electricity at sample both ends
The ratio of pressure is derived by the Seebeck coefficients of print；(3) hetero-junctions-exchange current flow method：Testing sample and standard sample are taken
Connect to form hetero-junctions, then hetero-junctions is suspended and overlapped, alternating current is loaded at hetero-junctions both ends, by solving Temperature Distribution and measurement
Seebeck voltages solve to obtain Seebeck coefficients.Characterize the figure of merit ZT=S of the heat to electricity conversion performance of material2σ T/ λ, bag
The electrical conductivity, thermal conductivity, Seebeck coefficients of material are contained.In nano material, the physical property dispersion degree of sample is big, i.e.,
Make be same technique with a batch of sample, there is also significant difference for its physical property.It is excellent for accurate characterization nanotube sample
Value coefficient, optimal situation are to same sample while measure electrical conductivity, thermal conductivity, Seebeck coefficients.It is however, above-mentioned
Method all can only independent measurement sample Seebck coefficients, it is necessary to reference to other measuring methods measurement electrical conductivity, thermal conductivity, it is impossible to
The figure of merit of accurate characterization nanotube sample.
Physical measurement system with the features such as its scalability is high, measurement procedure automates, the fields such as material, physics extensively by
Welcome.With PPMS (Physical Property Measurement System, comprehensive physical property measuring system) exemplified by, physical property
Measuring system can measure the physical properties such as magnetics, electricity, calorifics, pattern, ferroelectricity and the dielectric of block materials.However, PPMS
Measurement object based on block materials, it is impossible to the physical property of direct measurement nanotube sample.Measurement is received in world wide at present
The method of rice sample can only measure the electrical properties or thermal property or heat to electricity conversion property of sample, and even lacking can be same
The physical measurement system of systematic survey nanotube sample physical property on sample.Due to the unstability of nanotube sample physical property,
With a collection of nanotube sample by same treatment physical property excursion much larger than block materials physical property change
Change scope, therefore want the physical property of accurate characterization nanotube sample, it is necessary to measured on same sample.
Utility model content
The utility model is intended to one of technical problem at least solving in correlation technique to a certain extent.
Therefore, the purpose of this utility model is the thermoelectricity capability measuring system for proposing a kind of nano material, the measurement system
System can be with accurate measurement thermoelectricity capability.
To reach above-mentioned purpose, the utility model proposes a kind of thermoelectricity capability measuring system of nano material, including：Base
Bottom；First be arranged in the substrate suspends to the 3rd and taken, and first suspension, which takes to suspend to take with described second, passes through hot line
Suspend and be connected, and testing sample suspension is arranged at the 3rd suspension and taken between the central point of the hot line；Collection
Device, the harvester suspend with described first to the 3rd and take and is connected respectively, to gather the terminal voltage of the hot line and described
The terminal voltage of testing sample.
According to the thermoelectricity capability measuring system of nano material of the present utility model, by gathering the terminal voltage of hot line and to be measured
The terminal voltage of sample, so as to measure electricity, heat and the Thermoelectric Physicss property of nanotube sample on same sample, realize accurate survey
The purpose of calorimetric electrical property, the applicability of measuring system is improved, it is simple easily to realize.
Further, said system also includes：Controller, the controller are connected with the harvester, the control
Device is used for the terminal voltage for controlling the harvester to gather the hot line and the terminal voltage of the testing sample, and then obtains described
Electrical conductivity, thermal conductivity, heat absorption coefficient and the Seebeck coefficient of testing sample, further to obtain the resistance temperature of the testing sample
Spend coefficient, specific heat, thermal diffusivity, merit figue and thermal contact resistance.
Further, said system also includes：Power supply, the power supply is according to default connected mode and described first to the 3rd
Suspension take it is connected, wherein, described first suspends take including first it is heat sink take with second it is heat sink take, wherein, described first heat sink takes
On be provided with first electrode, the described second heat sink cost is provided with second electrode；Described second, which suspends, takes and heat sink is taken including the 3rd
With the 4th it is heat sink take, wherein, the described 3rd heat sink cost is provided with the 3rd electrode, the described 4th it is heat sink cost be provided with the 4th electricity
Pole；It is described 3rd suspend take including the 5th it is heat sink take with the 6th it is heat sink take, wherein, the described 5th it is heat sink cost be provided with the 5th electricity
Pole, the described 6th heat sink cost are provided with the 6th electrode.
Further, in the T-shaped submethod of four-wire system, the positive pole of the power supply is connected with the second electrode, the electricity
The negative pole in source is connected by first resistor with the 6th electrode, wherein, the power supply is dc source.
Further, in the T-shaped submethod of direct current, the positive pole of the power supply is connected with the 3rd electrode, the power supply
Negative pole be connected by second resistance with the second electrode, wherein, the power supply is dc source.
Further, in 3 ω-T-shaped submethod, the positive pole of the power supply is connected with the 3rd electrode, the power supply
Negative pole be connected by 3rd resistor with the second electrode, wherein, the power supply is AC power.
Further, in exchange heating-direct current detection submethod, the positive pole of the power supply and the 3rd electrode phase
Even, the negative pole of the power supply is connected by the 4th resistance with the second electrode, wherein, the power supply is AC power.
Alternatively, the harvester includes the data acquisition that multiple can gather DC voltage or alternating voltage sequence
Card.
Alternatively, the hot line can be platinum filament.
In addition, the testing sample is one-dimensional line sample, the one-dimensional line sample includes nanotube sample and micron sample
Product.
The additional aspect of the utility model and advantage will be set forth in part in the description, partly by from following description
In become obvious, or by it is of the present utility model practice recognize.
Brief description of the drawings
The above-mentioned and/or additional aspect of the utility model and advantage from the following description of the accompanying drawings of embodiments will
Become obvious and be readily appreciated that, wherein：
Fig. 1 is the structural representation according to the thermoelectricity capability measuring system of the nano material of the utility model one embodiment
Figure；
Fig. 2 is the structural representation according to the thermoelectricity capability measuring system of the nano material of the utility model another embodiment
Figure；
Fig. 3 is the structural representation according to the suspension hot-wire transducer of the utility model one embodiment；
Fig. 4 is the structural representation according to the thermoelectricity capability measuring system of the nano material of the utility model further embodiment
Figure；
Fig. 5 is the electrical block diagram according to the T-shaped submethod of four-wire system of the utility model one embodiment；
Fig. 6 is the electrical block diagram according to the T-shaped submethod of direct current of the utility model one embodiment；
Fig. 7 is the electrical block diagram according to the 3 ω-T-shaped submethod of the utility model one embodiment；
Fig. 8 is that the circuit structure that submethod is detected according to the exchange heating-direct current of the utility model one embodiment is illustrated
Figure；
Fig. 9 is to be shown according to the structure of the thermoelectricity capability measuring system of the nano material of one specific embodiment of the utility model
It is intended to.
Embodiment
Embodiment of the present utility model is described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning
Same or similar element is represented to same or similar label eventually or there is the element of same or like function.Below by ginseng
The embodiment for examining accompanying drawing description is exemplary, it is intended to for explaining the utility model, and it is not intended that to the utility model
Limitation.
It is simple first below before the thermoelectricity capability measuring system for the nano material that description proposes according to embodiments of the present invention
The importance of the thermoelectricity capability of accurate measurement nano material once is singly described.
Nanoscale solid material is all study hotspot and emphasis in the basic science such as physics, material field all the time,
It is huge in field application potentials such as micro-nano electronics, micro-nano sensor, energy conversion and Medical Devices.In nano material, heat
It is dramatically different with macroscopic material in atomic small restricted clearance, thermal conduction characteristic to transmit generation.Therefore, accurate measurement nano material
Thermal conduction characteristic for nanoscale thermal conduction study research and nano material practical application it is significant.Heat to electricity conversion system
System is solving energy crisis with possessing in environmental problem extensively with the features such as its movement-less part is compact-sized, noise-less pollution
Application prospect and development potentiality.And nano pyroelectric material is solving first have that thermo-electric device figure of merit is low, conversion efficiency is low
There is important breakthrough in problem.Therefore, the thermoelectricity capability that accurate measurement characterizes nano material is research nanometer thermoelectric
The important foundation of material.
The thermal conduction characteristic of nano material mainly includes thermal conductivity, thermal diffusivity.At present, researcher successfully develops one
The experimental method of a little measurement nano material thermal conduction characteristics, is contacted according to whether temperature sensor contacts to be divided into testing sample
Formula and contactless two class.Non-contact method mainly includes transient state photothermal reflectance method and Raman spectroscopy.Transient state photothermal reflectance
Method realizes temperature survey based on metal film surfaces reflectivity to the dependency characteristic of temperature.This method utilizes a branch of ultrashort pumping arteries and veins
Impulse light heating metal film sample, another beam direct impulse detect sample surfaces reflectivity changes in the time delay of setting,
The thermal conductivity and thermal diffusivity of nanotube sample are extracted by being fitted time domain heat reflection signal curve.Raman spectroscopy is drawn based on material
The temperature frequency shift property of graceful spectrum realizes temperature survey.This method heats nanoscale sample using continuous laser and excites its drawing
Graceful spectrum.According to the mean temperature in the Raman peak position offset measurement hot spot of sample, by estimating that laser absorption coefficient is swashed
Light heating amount, and then its thermal conductivity is tried to achieve by steady heat conduction model.Non-contact measurement is primarily present problems with：(1) draw
Graceful spectroscopic methodology suitable material is limited, it is necessary to which material has stable Raman spectrum temperature frequency shift property, and common suitable material is nanometer
Carbon pipe, graphene, are not suitable for metal material, in general semi-conducting material Raman peaks are not notable or Raman spectrum temperature frequency
Move not notable；(2) measurement temperature precision is low, and usual measurement temperature error is 5K~20K.In contact method, including it is powered certainly
Heating and sensing metal film device method, both of which are to realize temperature survey by the temperature dependent properties of resistance.It is powered and adds certainly
Hot method is directly powered at nanotube sample both ends, measures the voltage x current by nanotube sample, utilizes the resistance of nanotube sample in itself
Temperature dependent properties, calculate nanotube sample temperature rise；It can be counted with reference to one-dimensional stable conduction model and the physical dimension of nanotube sample
Calculation obtains the thermal conductivity of nanotube sample.Sensing metal film device method is needed to prepare metal nano sensor, and nanotube sample is overlapped
On sensor, the temperature rise of sensor is calculated using the resistance-temperature characteristic of sensor, with reference to the temperature difference at nanotube sample both ends
The thermal conductivity of nanotube sample can be calculated with the hot-fluid by nanotube sample.Metal sensor method proposes that its sensor is first
Two panels broken line platinum electrode, also commonly known as suspension dimensional device method (UCB), then propose T-shaped method, successfully measure carbon first and receive
The thermal conductivity of mitron, and subsequent this method is by Successful utilization in measurement asphalt-based carbon fiber, porous nano gold thin film, overlength carbon
The thermal conductivity of the materials such as nanotube.
The present invention is based on above-mentioned T-shaped method, and proposes a kind of thermoelectricity capability measuring system of nano material.
The thermoelectricity capability measuring system of nano material proposed according to the utility model embodiment is described with reference to the accompanying drawings.
Fig. 1 is the structural representation of the thermoelectricity capability measuring system of the nano material of the utility model one embodiment.
As shown in figure 1, the thermoelectricity capability measuring system of the nano material includes：Substrate 100, first suspends and takes 201, second
Suspension takes the 202, the 3rd suspension and takes 203 and harvester.
Wherein, first to the 3rd suspend and set up and is placed in substrate 100, first, which suspends, takes 201 and second and suspend and take 202 and pass through
Hot line 300, which suspends, to be connected, and the suspension of testing sample 400 is arranged at the 3rd suspension and taken between 203 and the central point of hot line 300.
Harvester suspends to take with first to the 3rd respectively to be connected, to gather the end of the terminal voltage of hot line 300 and testing sample 400 electricity
Pressure.The measuring system of the utility model embodiment can be to measure the physical property of nanotube sample on same sample, it is accurate to realize
The purpose of thermoelectricity capability is measured, it is simple easily to realize.
It is understood that the suspending column of hot line 300 is connected between the first suspending column 201 and the second suspending column 202, and it is to be measured
The suspending column of sample 400 is connected between the 3rd suspending column 203 and the central point of hot line 300.
Further, in one embodiment of the present utility model, the system of the utility model embodiment also includes：Control
Device.Wherein, controller is connected with harvester, and controller is used for the end electricity of the terminal voltage and testing sample 400 according to hot line 300
Pressure obtains electrical conductivity, thermal conductivity, heat absorption coefficient and the Seebeck coefficient of testing sample 400, further to obtain testing sample 400
Temperature-coefficient of electrical resistance, specific heat, thermal diffusivity, merit figue and thermal contact resistance.
Alternatively, in one embodiment of the present utility model, as shown in Fig. 2 left side is mum sample schematic diagram in figure,
Right side is nanotube sample schematic diagram, and testing sample 400 is one-dimensional line sample, and one-dimensional line sample includes the He of nanotube sample 401
Mum sample 402.
It is understood that the shape of testing sample 400 can be cylinder, cylinder cluster or rectangular body thin film.Treat test sample
Product 400 can be conductive material or non-conducting material.Testing sample 400 can be nano material or micro materials.So-called nanometer
Material refers to that the diameter of cylindrical material or the wide and high size of cuboid material are less than 1um.
In addition, testing sample 400 should be positioned over temperature control, sealing function thermostat in.In experiment, testing sample
The temperature fluctuation of 400 environment is less than 0.1K, and the vacuum of sample environment is less than 10-4Pa, taken out by mechanical pump and molecular pump two-stage
Filter is realized.Radiation shield is provided with thermostat, ensures that the temperature of radiation shield is close with sample 400.In the environment, test sample is treated
Radiation and convection heat losses of the product 400 to environment can be ignored.
Specifically, in embodiment of the present utility model, T-shaped suspend of one-dimensional line sample to be measured and hot line is overlapped,
It is placed in vacuum constant temperature environment, (will be described in detail below) in 4 kinds of different submethods, use direct current or simple alternating current
It is powered, gathers hot line both ends, the voltage signal at sample both ends, measures the electrical conductivity, thermal conductivity, heat absorption system of same sample successively
Number, Seebeck coefficient, and the resistance temperature system of same sample can further be calculated based on four foregoing physical property results
Number, specific heat, thermal diffusivity, merit figue and thermal contact resistance, altogether nine kinds of measurement results.
Alternatively, in one embodiment of the present utility model, hot line 300 can be platinum filament.
It is understood that hot line 300 can be platinum micro wire or platinum nanoribbons.The buying of platinum micro wire is certainly
Alfa Aesar, cross section are circle, and purity is more than 99.9%, a diameter of 10um, 25um, 50um, 100um.Platinum is received
The suspension platinum nanoribbons that rice band is prepared using deposition-etch technique.
Wherein, prepared by the hot line in being tested for mum sample, the copper sheet that 50mm square 3mm can be used thick does substrate
100, diameter 2mm copper cash do electrode and wire, are installed into after electrode jacket insulating ceramics in substrate 100.Then platinum filament is used
Hot line 300 is made across between two heat sink.The both ends of hot line 300 and heat sink overlap joint, hot line centre do not contact with substrate 100.Heat
The heavy and good contact of substrate 100, heat sink temperature is always environment temperature.There is electric insulation layer on the surface of substrate 100, is not led between heat sink
Electricity.Electrode 1 and electrode 2 are made on heat sink a (suspended equivalent to first and take 201), (suspends and takes equivalent to second in heat sink b
202) electrode 3 and electrode 4 are made on.
For nanotube sample, the covering of experience photoresist, e-book etching, physical vapour deposition (PVD), stripping photoresist, etching
SiO2The step such as layer and etching Si substrates, can prepare a suspension hot-wire transducer, as shown in Figure 3
Further, in one embodiment of the present utility model, the system of the utility model embodiment also includes：Electricity
Source.Wherein, power supply suspends to take and is connected according to default connected mode with first to the 3rd.Wherein, default connected mode is appreciated that
It is connected to suspend to take with first to the 3rd respectively in different submethods.
Specifically, first suspend take 201 include first it is heat sink take with second it is heat sink take, wherein, first heat sink costs setting
There is first electrode 1, the second heat sink cost is provided with second electrode 2；Second suspend take including the 3rd it is heat sink take with the 4th it is heat sink take,
Wherein, the 3rd heat sink cost is provided with the 3rd electrode 3, and the 4th heat sink cost is provided with the 4th electrode 4；3rd, which suspends, takes including the
Five it is heat sink take with the 6th it is heat sink take, wherein, the 5th heat sink cost is provided with the 5th electrode 5, and the 6th heat sink cost is provided with the 6th
Electrode 6.
It is understood that as shown in figure 4, Fig. 4 and Fig. 2 right side schematic views be repeat, will treat survey line suspend be overlapped on
Heat sink c (suspended equivalent to the 3rd and take 203) is between the center of hot line 300.Treat that survey line one end is connected on heat sink c, one end connection
In Call Center, treat not contact with substrate 100 among survey line.Electrode 5 and electrode 6 are made on heat sink c.By substrate 100 together with
Testing sample 400 is put into vacuum constant temperature groove together.
Alternatively, in one embodiment of the present utility model, harvester include multiple can gather DC voltage or
The data collecting card of alternating voltage sequence.
Further, in one embodiment of the present utility model, in the T-shaped submethod of four-wire system, the positive pole of power supply with
Second electrode 2 is connected, and the negative pole of power supply is connected by first resistor with the 6th electrode 6, wherein, power supply is dc source.
As shown in figure 5, connect circuit by mode in figure：DC power anode flows into electrode 2, and electric current passes through the He of hot line 300
Testing sample 400 is flowed out by electrode 6, and then series connection finally flows back to power cathode by measuring resistance.Two pieces of data collecting cards point
The indescribably DC voltage component between power taking pole 3- electrodes 5 and the DC voltage component of standard resistor at two terminals.Pass through data acquisition
The resistance of testing sample 400 can be calculated in the data of card, with reference to the dimension information of testing sample 400, can be calculated
The electrical conductivity of testing sample 400.
Further, in one embodiment of the present utility model, in the T-shaped submethod of direct current, the positive pole of power supply and
Three electrodes 3 are connected, and the negative pole of power supply is connected by second resistance with second electrode 2, wherein, power supply is dc source.
As shown in fig. 6, connect circuit by mode in figure：DC power anode flows into electrode 3, and electric current is after hot line 300
Flowed out by electrode 2, then flow through measuring resistance and finally flow back to power cathode.Two pieces of data collecting cards extract electrode 4- electrodes respectively
The DC voltage component of DC voltage component and standard resistor at two terminals between 1.It can be calculated by the data of data collecting card
Obtain the resistance of hot line 300.The average temperature rising of hot line 300 is calculated according to the resistance-temperature relationship of hot line 300.With reference to heat
The physical dimension of the physical dimension of line 300, thermal conductivity and testing sample 400, the thermal conductivity of testing sample 400 can be calculated
Rate.
Further, in one embodiment of the present utility model, in 3 ω-T-shaped submethod, the positive pole of power supply and
Three electrodes 3 are connected, and the negative pole of power supply is connected by 3rd resistor with second electrode 2, wherein, power supply is AC power.
As shown in fig. 7, circuit is connected in the way of in figure：AC power positive pole flows into electrode 3, and electric current passes through hot line 300
Flowed out afterwards by electrode 2, then flow through measuring resistance and finally flow back to power cathode (ground connection).AC power output amplitude is V, frequency
For ω.Two pieces of data collecting cards extract continuous ac voltage signal between electrode 4- electrodes 1 and standard resistor at two terminals respectively
Continuous ac voltage signal.Using virtual Phase Lock Technique, 1 ω voltage magnitudes, the 3 ω voltage amplitudes between electrode 4- electrodes 1 are extracted
1 ω voltage magnitudes of value and standard resistor at two terminals.With reference to the geometry of the physical dimension of hot line 300, thermal conductivity and testing sample 400
Size, the heat absorption coefficient of testing sample 400 can be calculated.
Further, in one embodiment of the present utility model, in exchange heating-direct current detection submethod, power supply
Positive pole be connected with the 3rd electrode 3, the negative pole of power supply is connected by the 4th resistance with second electrode 2, wherein, power supply is alternating current
Source.
As shown in figure 8, circuit is connected in the way of in figure：AC power positive pole flows into electrode 3, and electric current passes through hot line 300
Flowed out afterwards by electrode 2, then flow through measuring resistance and finally flow back to power cathode (ground connection).AC power output amplitude is V, frequency
For ω.Two pieces of data collecting cards extract continuous ac voltage signal between electrode 3- electrodes 5 and standard resistor at two terminals respectively
Continuous ac voltage signal.Using virtual Phase Lock Technique, the DC voltage amplitude and measuring resistance between electrode 3- electrodes 5 are extracted
The 1f voltage magnitudes at both ends.With reference to the physical dimension of the physical dimension of hot line 300, thermal conductivity and testing sample 400, can calculate
Obtain the Seebeck coefficients of testing sample 400.
In embodiment of the present utility model, using the resistance temperature property of hot line 300, by the resistance signal of hot line 300
Change is scaled the change of hot line mean temperature.The resistance of hot line 300 and the relation of temperature can be described as：R (Δ T)=R0×(1
+βΔT).Wherein Δ T represents the temperature rise of hot line 300, R0Represent zero temperature rise electricity when hot line 300 does not heat at ambient temperature
Resistance, R (Δ T) represent resistance of the hot line 300 in temperature rise Δ T.When considering that the temperature distributing disproportionation of one-dimensional hot line is even, above formula is still
Set up.
The utility model embodiment can measure electrical conductivity, the resistance temperature of sample on same platform, same sample
Coefficient, thermal conductivity, heat absorption coefficient, thermal diffusivity, specific heat, Seebeck coefficient, merit figue are spent, without multiple samples, without changing
Become sample overlap joint, without changing sample stage, it is ensured that measurement result is reliably effective.
Specifically, the measuring system of the utility model embodiment can on same micro-nano sample measurement ＆ characterization conductance
Rate, thermal conductivity, heat absorption coefficient, Seebeck coefficient, temperature-coefficient of electrical resistance, specific heat, thermal diffusivity, the T-shaped method of the system of merit figue.
Wherein, DC source is loaded on sample, is referred to as the T-shaped submethod of four-wire system in the submethod of sample both ends measurement DC voltage；
DC source is loaded on hot line, is referred to as the T-shaped submethod of direct current in the submethod of hot line both ends measurement DC voltage；Loaded on hot line
Simple alternating current source, the submethod that fundamental component and frequency tripling composition are measured at hot line both ends are referred to as 3 ω-T-shaped submethod；In hot line
Upper loading simple alternating current source, turn into exchange heating-direct current in the submethod of sample both ends measurement flip-flop and detect T-shaped son side
Method.The T-shaped submethod of four-wire system can direct measurement obtain the electrical conductivity and temperature-coefficient of electrical resistance of sample；The T-shaped submethod energy of direct current
Enough direct measurements obtain the thermal conductivity of sample；3 ω-T-shaped submethod can direct measurement obtain the heat absorption coefficient and sample of sample
With the thermal contact resistance of hot line lap-joint；Exchange heating-direct current detect T-shaped submethod can direct measurement obtain sample
Seebeck coefficients；Specific heat, the thermal diffusivity merit figue of sample can be further extracted with reference to above-mentioned measurement result.
For example, in one embodiment of the present utility model, comprise the following steps：
Step S1, sensor and preparation of samples.
Before the T-shaped method of system, first have to prepare sample and sensor.For the sample of micro materials, sensor uses
The platinum filament that diameter does not wait from 10um to 100um.For the sample of nano material, sensor is using thickness at tens nanometers to hundreds of
Nanometer does not wait suspension platinum film.By sample overlap joint with after sensor, using slide measure, light microscope, SEM or TEM etc.
Technology, the length l of measurement sensorh, sensor diameter Dh, sample length lf, sample diameter Df。
Step S2, the T-shaped submethod of four-wire system.
The T-shaped method of four-wire system can measure the electrical conductivity and temperature-coefficient of electrical resistance of sample.During method T-shaped using four-wire system, sample
The DC voltage component of two sections of data collecting card is Vf, the DC voltage component of the data collecting card of standard resistor at two terminals is Vs,
The resistance of measuring resistance is Rs, then sample resistance be：
With reference to sample size, sample resistivity ρ can be calculatedf, conductivityσfFor：
Change environment temperature, measure sample resistivity using the T-shaped method of four-wire system at different ambient temperatures, obtain environment temperature
Degree series { T1,T2,T3,T4... } and corresponding temperature under resistivity sequence { σf,1,σf,2,σf,3,σf,4,……}.According to electricity
The definition of temperature coefficient is hindered, can be calculated in temperature TkPlace sample temperature-coefficient of electrical resistance β be：
Step S3, the T-shaped submethod of direct current.
The T-shaped method of direct current can measure the thermal conductivity of sample.During method T-shaped using direct current, lead to direct current at hot line both ends.Change
DC voltage, the DC component of the data collecting card at hot line both ends is sequence { Vh,1,Vh,2,Vh,3,Vh,4... ..., measuring resistance
The DC component of the data acquisition at both ends is sequence { Vs,1,Vs,2,Vs,3,Vs,4... }, the resistance of measuring resistance is Rs.It is then hot
The joule heat power of line is sequence { Ph,k}={ Vs,kVh,k/Rs, under different heat power, the resistance of hot line is designated as sequence
{Rh,k}={ Vh,kRs/Vs,k}.To sequence { Ph,k, { Rh,kLinear fit is done, obtain slope khWith intercept Rh,b.Then hot line is flat
Samming ascending chainIt can be expressed as：
In the case where hot line temperature rise is little, the resistance of hot line is linear change with the heating power of hot line.Its is linear
Variation relation can portray for：
Wherein β is the temperature-coefficient of electrical resistance of hot line, Rh,273.15It is resistance of the hot line under 273.15K environment temperature.It is right
Sequence { Ph,k, { Rh,kLinear fit is done, obtain slope kh, then the thermal conductivity λ of survey line is treatedfFor：
Step S4,3 ω-T-shaped submethod.
3 ω-T-shaped method can measure the thermal contact resistance between the heat absorption coefficient of sample and sample and hot line overlapped points.Use 3
During ω-T-shaped method, at hot line both ends, passband rate is ω sinusoidal ac.Change ac frequency is sequence { f1,f2,f3,
f4... ..., the ω component amplitudes of the data collecting card at hot line both ends are sequence { Vhω,1,Vhω,2,Vhω,3,Vh
ω,4... ..., the ω component amplitudes component of the data acquisition of standard resistor at two terminals is sequence { Vs,1,Vs,2,Vs,3,Vs,4,……},
The resistance of measuring resistance is Rs, 3 ω component amplitudes of the data collecting card at sample both ends are sequence { Vh3ω,1,Vh3ω, 2,Vh3
ω, 3,Vh3ω, 4,……}.Then dimensionless heat transfer coefficient Z meets：
The wherein relation of dimensionless heat transfer coefficient Z and test signal is：
Dimensionless frequency LhExpression formula be：
By formula (8), dimensionless thermal impedance χ, dimensionless can be calculated with fitted signal using nonlinear fitting instrument
Thermal impedance χ and sample heat absorption coefficient bf, thermal contact resistance RcRelational expression be：
Wherein, bhIt is the heat absorption coefficient of hot line, F is proportionality coefficient.The heat absorption system of sample can be obtained according to χ fitting results
Number bfThermal contact resistance R between sample and hot linec。
Step S5, exchange heating direct current detect T-shaped submethod.
Exchange heating direct current, which detects T-shaped method, can measure the Seebeck coefficient of sample.It is T-shaped using exchange heating direct current detection
During method, at hot line both ends, passband rate is ω sinusoidal ac.It is sequence { V to change alternating current voltage amplitude1,V2,V3,
V4... ..., the ω component amplitudes of the data collecting card at hot line both ends are sequence { Vh,1,Vh,2,Vh,3,Vh,4... ..., standard electric
The ω component amplitudes component for hindering the data acquisition at both ends is sequence { Vs,1,Vs,2,Vs,3,Vs,4... }, the resistance of measuring resistance is
Rs, the DC component of the data collecting card at sample both ends is sequence { Vf,1,Vf,2,Vf,3,Vf,4,……}.The then joule hair of hot line
Thermal power is sequence { Ph,k}={ Vs,kVh,k/2Rs, under different heat power, the resistance of hot line is designated as sequence { Rh,k}=
{Vh,kRs/Vs,k}.To sequence { Ph,kAnd sequence { Rh,kLinear fit is done, it is R to obtain intercepth,b.The then average temperature rising sequence of hot line
Row can be expressed as：
The hot line average temperature rising for not overlapping sample under identical heating power is：
Then the temperature rise steady-state quantity at sample overlapped joints is：
To sequence { Vf,kAnd sequence { θs,kLinear fit is done, its slope is the Seebeck coefficient S of sample.
Step S6, the conductivityσ of sample can be measured respectively in step 2~5f, temperature-coefficient of electrical resistance β, thermal conductivity λf、
Heat absorption coefficient bf, Seebeck coefficient S and thermal contact resistance Rc.Then the volume ratio hotlist of sample is shown as：
The thermal diffusivity of sample is expressed as：
The merit figue of sample is expressed as：
Further, in one particular embodiment of the present invention, as shown in figure 9,1 is vacuum constant temperature groove, 2,3 are respectively
Molecular pump and oil-sealed rotary pump, 4 be refrigeration compressor, and 5 be temperature control console, and 6 be matrix switch.4, hot line both ends binding post and
In the equal access matrix switch of 2 binding posts of sample tail end.7th, 8,9,10 be respectively power supply, measuring resistance and two pieces of data acquisitions
Card, the wiring of power supply, measuring resistance and data collecting card is also in equal access matrix switch.Switch different patrol in matrix switch
The switching of 4 kinds of different submethods in the T-shaped method of system can be realized by collecting circuit.11 be computer.Temperature control console, matrix switch, electricity
Source, data collecting card connect with computer, are controlled by computer, are communicated with computer.Can be with the cooperation of related software
Realize automatic measurement.
According to the thermoelectricity capability measuring system of nano material of the present utility model, by gathering the terminal voltage of hot line and to be measured
The terminal voltage of sample, so as to measure electricity, heat and the Thermoelectric Physicss property of nanotube sample on same sample, realize accurate survey
The purpose of calorimetric electrical property, the applicability of measuring system is improved, it is simple easily to realize.
In addition, term " first ", " second " are only used for describing purpose, and it is not intended that instruction or hint relative importance
Or the implicit quantity for indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can be expressed or
Implicitly include at least one this feature.In description of the present utility model, " multiple " are meant that at least two, such as two
It is individual, three etc., unless otherwise specifically defined.
In the utility model, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " Gu
It is fixed " etc. term should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integrally；Can be
Mechanically connect or electrically connect；Can be joined directly together, can also be indirectly connected by intermediary, can be two
The connection of element internal or the interaction relationship of two elements, limited unless otherwise clear and definite.For the common skill of this area
For art personnel, concrete meaning of the above-mentioned term in the utility model can be understood as the case may be.
In the utility model, unless otherwise clearly defined and limited, fisrt feature is "above" or "below" second feature
Can be that the first and second features directly contact, or the first and second features pass through intermediary mediate contact.Moreover, first is special
Sign second feature " on ", " top " and " above " can be fisrt feature directly over second feature or oblique upper, or only
Represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " lower section " and " below " can be with
Be fisrt feature immediately below second feature or obliquely downward, or be merely representative of fisrt feature level height and be less than second feature.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment or example of the present utility model.In this manual, to the schematic table of above-mentioned term
State and be necessarily directed to identical embodiment or example.Moreover, specific features, structure, material or the feature of description can be with
Combined in an appropriate manner in any one or more embodiments or example.In addition, in the case of not conflicting, this area
Technical staff the different embodiments or example and the feature of different embodiments or example described in this specification can be entered
Row combines and combination.
Although embodiment of the present utility model has been shown and described above, it is to be understood that above-described embodiment is
Exemplary, it is impossible to it is interpreted as to limitation of the present utility model, one of ordinary skill in the art is in the scope of the utility model
It is interior above-described embodiment to be changed, changed, replaced and modification.
Claims (10)
- A kind of 1. thermoelectricity capability measuring system of nano material, it is characterised in that including：Substrate；First be arranged in the substrate suspends to the 3rd and taken, and first suspension, which takes to suspend to take with described second, passes through hot line Suspend and be connected, and testing sample suspension is arranged at the 3rd suspension and taken between the central point of the hot line；AndHarvester, the harvester suspends to take with described first to the 3rd respectively to be connected, to gather the end of hot line electricity The terminal voltage of pressure and the testing sample.
- 2. the thermoelectricity capability measuring system of nano material according to claim 1, it is characterised in that also include：Controller, the controller are connected with the harvester, and the controller is used to control the harvester collection institute The terminal voltage of hot line and the terminal voltage of the testing sample are stated, and then obtains the electrical conductivity, thermal conductivity, heat absorption of the testing sample Coefficient and Seebeck coefficient, further to obtain the temperature-coefficient of electrical resistance of the testing sample, specific heat, thermal diffusivity, high-quality system Number and thermal contact resistance.
- 3. the thermoelectricity capability measuring system of nano material according to claim 1, it is characterised in that also include：Power supply, institute State power supply and suspend to take with described first to the 3rd according to default connected mode and be connected, wherein,It is described first suspend take including first it is heat sink take with second it is heat sink take, wherein, the described first heat sink cost is provided with first Electrode, the described second heat sink cost are provided with second electrode；It is described second suspend take including the 3rd it is heat sink take with the 4th it is heat sink take, wherein, the 3rd heat sink cost is provided with the 3rd Electrode, the described 4th heat sink cost are provided with the 4th electrode；It is described 3rd suspend take including the 5th it is heat sink take with the 6th it is heat sink take, wherein, the 5th heat sink cost is provided with the 5th Electrode, the described 6th heat sink cost are provided with the 6th electrode.
- 4. the thermoelectricity capability measuring system of nano material according to claim 3, it is characterised in that in the T-shaped son of four-wire system In method, the positive pole of the power supply is connected with the second electrode, and the negative pole of the power supply passes through first resistor and the described 6th Electrode is connected, wherein, the power supply is dc source.
- 5. the thermoelectricity capability measuring system of nano material according to claim 3, it is characterised in that in the T-shaped son side of direct current In method, the positive pole of the power supply is connected with the 3rd electrode, and the negative pole of the power supply passes through second resistance and the described second electricity Extremely it is connected, wherein, the power supply is dc source.
- 6. the thermoelectricity capability measuring system of nano material according to claim 3, it is characterised in that in 3 ω-T-shaped son side In method, the positive pole of the power supply is connected with the 3rd electrode, and the negative pole of the power supply passes through 3rd resistor and the described second electricity Extremely it is connected, wherein, the power supply is AC power.
- 7. the thermoelectricity capability measuring system of nano material according to claim 3, it is characterised in that in exchange heating-straight In stream detection submethod, the positive pole of the power supply is connected with the 3rd electrode, the negative pole of the power supply by the 4th resistance and The second electrode is connected, wherein, the power supply is AC power.
- 8. the thermoelectricity capability measuring system of nano material according to claim 1, it is characterised in that the harvester bag Include multiple collection DC voltages or the data collecting card of alternating voltage sequence.
- 9. the thermoelectricity capability measuring system of nano material according to claim 1, it is characterised in that the hot line is platinum Silk.
- 10. the thermoelectricity capability measuring system of the nano material according to claim any one of 1-9, it is characterised in that described Testing sample is one-dimensional line sample, and the one-dimensional line sample includes nanotube sample and mum sample.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109142433A (en) * | 2018-09-05 | 2019-01-04 | 中国科学院工程热物理研究所 | A method of low-dimensional micro-nano material thermal conductivity is measured based on alternating current method |
| CN109187628A (en) * | 2018-08-30 | 2019-01-11 | 桂林电子科技大学 | The test method of thermal contact resistance between micro-/ nano thin material is measured based on 3 ω methods |
| CN109975348A (en) * | 2019-03-07 | 2019-07-05 | 北京工业大学 | A kind of in-situ heat electric performance testing device, preparation method and system |
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| CN112816520A (en) * | 2020-12-30 | 2021-05-18 | 华中科技大学 | Method for testing film contact thermal resistance |
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- 2017-04-26 CN CN201720450926.XU patent/CN206990487U/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109187628A (en) * | 2018-08-30 | 2019-01-11 | 桂林电子科技大学 | The test method of thermal contact resistance between micro-/ nano thin material is measured based on 3 ω methods |
| CN109142433A (en) * | 2018-09-05 | 2019-01-04 | 中国科学院工程热物理研究所 | A method of low-dimensional micro-nano material thermal conductivity is measured based on alternating current method |
| CN109142433B (en) * | 2018-09-05 | 2021-01-12 | 中国科学院工程热物理研究所 | Method for measuring thermal conductivity of low-dimensional micro-nano material based on alternating current method |
| CN109975348A (en) * | 2019-03-07 | 2019-07-05 | 北京工业大学 | A kind of in-situ heat electric performance testing device, preparation method and system |
| CN110108770A (en) * | 2019-05-10 | 2019-08-09 | 北京科技大学 | High-flux electric card test system based on space thermal imaging |
| CN112816520A (en) * | 2020-12-30 | 2021-05-18 | 华中科技大学 | Method for testing film contact thermal resistance |
| CN112881464A (en) * | 2021-01-20 | 2021-06-01 | 中国科学院工程热物理研究所 | Method and device for directly and comprehensively measuring thermoelectric performance of micro-nano material in situ |
| WO2022156740A1 (en) * | 2021-01-20 | 2022-07-28 | 中国科学院工程热物理研究所 | Method and device for direct in-situ comprehensive measurement of thermoelectric properties of micro-nano material |
| CN112881464B (en) * | 2021-01-20 | 2022-12-09 | 中国科学院工程热物理研究所 | Method and device for directly and comprehensively measuring thermoelectric performance of micro-nano material in situ |
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