CN102692427B - Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope - Google Patents
Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope Download PDFInfo
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Abstract
The invention relates to a nano-thermoelectric energy material multi-parameter in-situ quantitative characterization device based on an atomic force microscope, which is used for detecting a micro-area heat conduction coefficient, a Seebeck coefficient and other thermoelectric property parameters of a detected nano-thermoelectric material sample. The device comprises a nano-thermoelectric multi-parameter atomic force microscope in-situ excitation platform and a nano-thermoelectric multi-parameter in-situ detection platform, wherein the nano-thermoelectric multi-parameter atomic force microscope in-situ excitation platform is used for providing a basic hardware platform required in nano-thermoelectric multi-parameter excitation and realizing in-situ simultaneous excitation of a micro-area frequency-tripled heat conduction signal and a micro-area stable-state Seebeck direct current voltage signal of a nano-thermoelectric material; and the nano-thermoelectric multi-parameter in-situ detection platform is used for realizing in-situ real-time detection and data processing of micro-area heat conduction and Seebeck voltage of the nano-thermoelectric material and realizing real-time display of the quantitative characterization results of the micro-area heat conduction coefficient and the Seebeck coefficient. According to the device disclosed by the invention, the nano-detection function of the atomic force microscope, the frequency tripling detection principle of macro-heat conductivity and the test principle of the macro-Seebeck coefficient are combined for establishing a nano in-situ evaluation device which is based on the commercial atomic force microscope and combines the properties of nano-scale heat excitation and thermoelectric multi-parameter detection.
Description
Technical field
The application relates to a kind of nano pyroelectric material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope, belongs to input instrument field.
Background technology
Thermoelectric material, as a kind of important strategic energy and material, has very wide application prospect at numerous key areas such as microelectronics, photoelectron, survey of deep space, defence and military and energy-conserving and environment-protective.Current, the main obstacle of restriction thermoelectric material widespread use is exactly that its conversion efficiency of thermoelectric is low, and nanometer technology has been opened up a new way for developing high performance thermoelectric material.Thus, nano pyroelectric material has become the research field that current international thermoelectricity circle is the most active, be hopeful to make a breakthrough most, and the measurement of nanometer thermoelectric performance and sign also become the challenge subjects that solution is badly in need of in this field day by day.
Thermal conductivity and Seebeck coefficient are two important physical parameters in thermoelectric material physical property, it characterizes conventional art and the method still continued to use at present, the method has following limitation: (1) its thermal excitation or heat detect the macro property that has only reflected sample, reach far away nanoscale level; (2) its method of testing is in static state, only adopts the thermal excitation mode of stable state to realize single-point and detects, cannot reflect heat electric material dynamic property and continuously the detected parameter of reflection with the variable condition of locus; (3) test of the thermoelectricity such as thermal conductance, Seebeck coefficient many reference amounts adopts many cover discrete devices to complete, and cannot reach in real time, synchronously detect.Thereby the conventional test methodologies of thermoelectric material physical property is difficult to realize the original position of the comprehensive physical property of nano pyroelectric material, real-time, integrated sign.For above limitation, the application wishes that foundation can realize the original position of nano pyroelectric material many reference amounts physical property, harmless, real-time, dynamic, quantitative, nanometer characterization system, to meet the urgent need of the nano pyroelectric material physical property sign of current fast development.
Atomic force microscope (AFM) is one of current important tool of carrying out nano science research, it has the distinct advantages such as high precision control, nanometer resolution, become a kind of nanometer detection platform of maturation, and for developing on its basis new technology, expand new function Important Platform basis be provided.
The active demand that the application characterizes for current nanometer thermoelectric physical property, the features such as the detection maturity based on AFM nanometer platform, multiple functional property and structural integrity, set up the in situ quantitation characterization apparatus of nanometer thermoelectric many reference amounts, realize the original position of nano pyroelectric material thermal conductivity and Seebeck coefficient, real-time, dynamic, quantitative test, for furtheing investigate the deep development of thermoelectricity transport theory, nano pyroelectric material and the device thereof of nano pyroelectric material, provide important in situ quantitation nanometer characterizing method.There is no at present report in this respect both at home and abroad.
Summary of the invention
The application's object is to provide the thermoelectricity many reference amounts such as a kind of nanometer thermal conductivity coefficient that can be used in nanometer thermoelectric energy and material, nano-plug seebeck coefficient to characterize the in situ quantitation nanometer characterization apparatus of use.The frequency tripling of atomic force microscope nanometer measuring ability and macroscopical thermal conductivity is detected to principle to this technology and macroscopical Seebeck coefficient test philosophy is combined together, based on commercial AFM nanometer detection platform, set up the nanometer in situ assessment technique that has nanoscale thermal excitation and thermoelectricity many reference amounts detection characteristic concurrently, efficiently solve thermoelectric material nanometer thermoelectric performance in-situ and detect this gordian technique difficult point.This novel nano technology not only has the unique function that nanometer thermoelectric many reference amounts original position excites simultaneously, in-situ synchronization characterizes, and has the advantages such as high resolving power, high sensitivity, high s/n ratio.Gordian technique apparatus structure described in the application is simple, compatible strong, and fit and combine from different commercial AFM systems, be a new technology that is easy to promotion and application.
The application has adopted a kind of nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope, for detection of thermoelectricity Physical Parameters such as the microcell thermal conductivity coefficient of a tested nano pyroelectric material sample and Seebeck coefficients, it is characterized in that, comprise: the atomic force microscope original position stimulating platform of nanometer thermoelectric many reference amounts, for providing nanometer thermoelectric many reference amounts to excite required basic hardware platform, and realize original position excitation nano thermoelectric material microcell frequency tripling thermal conductance signal and microcell stable state Seebeck d. c. voltage signal simultaneously; One nanometer thermoelectric many reference amounts in situ detection platform, detects and data processing in real time for realizing the original position of nano pyroelectric material microcell thermal conductance and Seebeck voltage, shows in real time the quantitatively characterizing result of microcell thermal conductivity coefficient and Seebeck coefficient.
Reasonablely be, the atomic force microscope original position stimulating platform of described nanometer thermoelectric many reference amounts further comprises: an atomic force microscope platform, one thermoelectricity detector probe, one thermoelectricity reference probe, two adjustable resistance networks, one signal generator, one thermoelectric material, one ceramic insulating layer, one magnetic bases, one signal transmission ends, one microcell thermal conductance signal output port, one microcell Seebeck voltage signal output port, described tested thermoelectric material sample is placed on described magnetic bases by ceramic insulation described in underlay, described thermoelectricity detector probe, thermoelectricity reference probe, two adjustable resistance networks and signal generator form a Wheatstone bridge, described thermoelectricity detector probe is placed on described tested thermoelectric material sample and contact, to detect the voltage of described tested thermoelectric material sample point of excitation, the first end of described microcell Seebeck voltage signal output port receives the voltage signal in another region of described tested thermoelectric material sample by described signal transmission ends, the second end of described microcell Seebeck voltage signal output port is connected with described Wheatstone bridge earth terminal, the first end of described microcell thermal conductance signal output port connects the described thermoelectricity detector probe end that is connected with described Wheatstone bridge, and its second end connects the described thermoelectricity reference probe end that is connected with described Wheatstone bridge.
Reasonable, the mode of operation of described atomic force microscope platform is contact mode.
Reasonable, described thermoelectricity detector probe is the probe of a tool thermistor characteristic, has the function of microcell driving source, signal transducer and detection resources simultaneously; The mode of operation of described thermoelectricity detector probe is AFM contact mode, and its micro-cantilever deformation quantity as feedback parameters is 0.1-5nm, with the diameter of described tested thermoelectric material sample interaction contact area be 30-100nm.
Reasonable, the operating frequency range of described thermoelectricity probe is 100Hz-10kHz, and current margin is 1mA-100mA.
Reasonable, the described thermoelectricity detector probe in described Wheatstone bridge and described thermoelectricity reference probe adopt differential input mode to be connected to form two probe structures.
Reasonable, its adjustment mode of described thermoelectricity loop comprises that the adjustment of thermoelectricity probe recommended current, thermoelectricity loop fundamental signal suppress to adjust, harmonic signal sensitivity increases the three kinds of patterns of adjusting.
Reasonablely be, described nanometer thermoelectric many reference amounts in situ detection platform comprises a front end loop processing module, one high sensitivity lock-in amplifier, one high accuracy number voltmeter, one data processing and display system, detect, process and show the in-situ characterization result of the thermoelectricity many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient in real time for realizing the original position of faint frequency tripling thermal conductance signal and Seebeck voltage signal.
The nanometer thermoelectric many reference amounts in situ quantitation characterization apparatus that adopts said structure to set up has solved nano pyroelectric material many reference amounts thermoelectricity physical property original position and has excited and synchronously detected this great technical barrier.The original position that this novel nano characterization apparatus has been realized nanometer thermoelectric many reference amounts excites simultaneously, in-situ synchronization detects, expand the nanometer thermoelectric evaluation of physical property function that existing commercial atomic force microscope does not have, for furtheing investigate the thermoelectricity transport theory of nano pyroelectric material and the deep development of nano pyroelectric material and device thereof, provide important original position, quantitative, nanometer characterization apparatus.
Accompanying drawing explanation
Below, with reference to accompanying drawing, for those skilled in the art, to the application's detailed description, the application's above and other object, feature and advantage will be apparent.
Fig. 1 illustrates the structured flowchart of the application's nanometer thermoelectric many reference amounts in situ quantitation characterization apparatus;
Fig. 2 illustrates the structured flowchart of atomic force microscope (AFM) the original position stimulating platform of the many reference amounts of nanometer thermoelectric described in Fig. 1;
Fig. 3 illustrates the structured flowchart of Fig. 2 Atom force microscope platform (AFM);
Fig. 4 illustrates the structured flowchart of nanometer thermoelectric many reference amounts in situ detection platform in Fig. 1;
The structured flowchart of end loop processing module before Fig. 5 illustrates in Fig. 4;
Fig. 6 (a) has provided the AFM picture of nanometer thermoelectric film surface appearance;
Fig. 6 (b) has provided thin film micro-zone thermal conductance frequency tripling signal (U
3 ω) and excitation frequency logarithm (ln ω) between relation, can calculate accordingly microcell thermal conductance quantitatively characterizing result;
Fig. 7 (a) has provided probe voltage (U under different exciting voltages
probe) test result;
Fig. 7 (b) is the Seebeck voltage (U under different exciting voltages
seebeck) test result;
Fig. 7 (c) has provided Seebeck voltage (U under different temperatures
seebeck-Δ T
probe) test result, can calculate microcell Seebeck coefficient accordingly.
Embodiment
Following instance is all quantitatively characterizing results to thermoelectricity many reference amounts such as nanometer thermoelectric membraneous material microcell thermal conductivity coefficient and microcell Seebeck coefficients of nanometer thermoelectric many reference amounts in situ quantitation characterization technique of application the application, to further illustrate the application's effect, but be not limited only to following embodiment.
The application has set up a kind of in situ quantitation characterization apparatus of the nanometer thermoelectric many reference amounts based on atomic force microscope, its principle of work structure as shown in Figure 1, by two parts, formed: the AFM original position stimulating platform 1 of nanometer thermoelectric many reference amounts, nanometer thermoelectric many reference amounts in situ detection platform 2.The AFM original position stimulating platform 1 of nanometer thermoelectric many reference amounts wherein, in order to the AFM platform base of development nanometer thermoelectric many reference amounts in-situ characterization new technology to be provided, and this original position that realizes the thermoelectricity many reference amounts signals such as nano pyroelectric material microcell thermal conductance, microcell Seebeck voltage of base excites simultaneously; Its nanometer thermoelectric many reference amounts in situ detection platform 2, in order to realize the original position of nano pyroelectric material microcell thermal conductance signal and Seebeck voltage signal, detect in real time and process, showing the in-situ characterization result of the thermoelectricity many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient.
The work structuring of the AFM original position stimulating platform 1 of nanometer thermoelectric many reference amounts as shown in Figure 2, mainly comprise atomic force microscope platform 11, thermoelectricity detector probe 12, thermoelectricity reference probe 13, two adjustable resistance networks 14, 15, signal generator 16, tested thermoelectric material sample 17, ceramic insulating layer 18, magnetic bases 19, signal transmission ends 110, microcell thermal conductance signal output port 111, microcell Seebeck voltage signal output port 112 etc., wherein, tested thermoelectric material sample 17 is placed on the magnetic bases 19 of atomic force microscope platform 11 by underlay ceramic insulating layer 18, thermoelectricity detector probe 12, thermoelectricity reference probe 13, two adjustable resistance networks 14, 15, signal generator 16 forms Wheatstone bridge (Wheat stone bri dge), thermoelectricity detector probe 12 is placed on tested thermoelectric material sample 17 and contact, to detect the voltage of sample point of excitation.The first end of microcell Seebeck voltage signal output port 112 receives the voltage signal in tested thermoelectric material sample 17 another regions by signal transmission ends 110, the second end of microcell Seebeck voltage signal output port 112 is connected with electric bridge earth terminal.In addition, the first end of microcell thermal conductance signal output port 111 connects thermoelectricity detector probe 12 end that is connected with electric bridge, its second end connection thermoelectricity reference probe 13 end that is connected with electric bridge.
The AFM original position stimulating platform 1 of the nanometer thermoelectric many reference amounts of said structure is in order to provide nanometer thermoelectric many reference amounts to excite required basic hardware platform, and realizes original position and excite microcell thermal conductance signal and microcell Seebeck voltage signal simultaneously.
Why the AFM original position stimulating platform 1 of nanometer thermoelectric many reference amounts has heat interchange interaction and the peculiar Seebeck physical influence of thermoelectric material that original position while excitation nano thermoelectricity many reference amounts function mainly comes from thermal probe and sample.For microcell thermal conductance, its physical process exciting can be expressed as follows: when signal generator 16 applies periodic activation signals and acts on thermoelectricity detector probe 12, thermoelectricity detector probe 12 temperature raise (higher than room temperature), causes the resistance of probe 12 to increase.Now, when thermoelectricity detector probe 12 contacts with tested thermoelectric material sample 17, due to the existence of both temperature difference, thermoelectricity detector probe 12 will produce heat exchange action with tested thermoelectric material sample 17.This heat interchange effect has induced the surface temperature of thermoelectricity detector probe 12 and thermally sensitive resistance thereof to change, because thermoelectricity detector probe 12 is one end of electric bridge brachium pontis, the variation of the resistance of thermoelectricity detector probe 12 will cause Gai Qiao road uneven, produced frequency tripling higher harmonic voltage output signal and exported by microcell thermal conductance signal output port 111, this output signal is directly related with tested microcell thermal conductance.Thus, the original position that has realized microcell thermal conductance excites.Meanwhile, between the sample point of excitation (temperature end) that the heat interchange effect between above-mentioned thermal probe-sample also can contact in thermoelectricity detector probe 12 and signal transmission ends 110 neighboring area of living in (low-temperature end, room temperature), induced a temperature difference source.Based on the peculiar Seebeck effect of thermoelectric material, this temperature difference source will produce Seebeck voltage signal in tested thermoelectric material sample 17.Because thermal probe exciting power is in stable state, therefore, the Seebeck voltage signal of generation is the d. c. voltage signal of a stable state.Thus, the original position that has also simultaneously realized microcell Seebeck voltage signal excites.Thereby, in thermoelectric material, utilize pyroelectric signal driver unit original position to excite microcell frequency tripling thermal conductance signal and microcell Seebeck DC Steady voltage signal simultaneously.
Fig. 3 has provided the further structured flowchart of Fig. 2 Atom force microscope platform 11, and this microscope stage 11 is commercial atomic force microscope (AFM), has high precision control, nano level high resolution rate imaging characteristic.Mainly comprise sweep unit 11a, power detection part 11b, position detection component 11c, FEEDBACK CONTROL parts 11d etc., in order to provide nanometer thermoelectric to detect required basic hardware platform.AFM mode of operation is contact mode, and its feedback parameters (micro-cantilever deformation quantity) is 0.1-5nm, and in order to realize, nanoscale good between thermoelectricity probe and sample contacts and effectively signal excitation and transmission.
Return in Fig. 2, thermoelectricity detector probe 12, thermoelectricity reference probe 13, two adjustable resistance networks 14,15 and signal generator 16 form thermoelectricity loop, realize thermoelectricity many reference amounts frequency tripling signal excitation.This thermoelectricity loop adopts the bridge structure with high detection sensitivity feature, and this bridge structure is significantly different from the general bridge structure that only can detect single one physical amount.Wherein thermoelectricity loop Qiao road integrally closed is in can, to shield undesired signal; And two adjustable resistance networks 14,15 are selected accurate noninductive resistance, to avoid the distribution parameter of electronic component to affect accuracy of detection.
Thermoelectricity loop signal comprises fundamental signal and frequency tripling harmonic signal, and wherein harmonic signal reflection is detected thermoelectric material microcell thermal conductance signal, and the duty of this thermal conductance signal and thermal probe is closely related.In thermoelectricity loop, the adjustment mode of thermoelectricity detector probe duty comprises that the adjustment of thermoelectricity probe recommended current, thermoelectricity loop fundamental signal suppress to adjust, harmonic signal sensitivity increases three kinds of patterns such as adjustment.Two adjustable resistance networks 14,15 in thermoelectricity bridge circuit, one of them adjustable resistance network 14 is in order to adjust bridge balancing, thus the output of Fundamental wave suppression signal; Another adjustable resistance network 15, in order to regulate the working current of thermoelectricity detector probe 12, is realized thermoelectricity detector probe 12 in optimum Working.Meanwhile, in this thermoelectricity loop, adopt nonlinear element to adjust the frequency tripling harmonic component relevant with detected thermoelectric material microcell thermal conductance signal, thereby improve harmonic signal sensitivity.
Thermoelectricity detector probe 12 is the core component of system in this thermoelectricity loop.It is different significantly that thermoelectricity detector probe 12 and commercial AFM probe have, and its structure is V-structure, by Pt/Rh material, is made, tool thermistor characteristic, and its resistance will change and change with probe temperature.This probe has three kinds of functions such as microcell thermal source, micro-area temperature sensor and microcell Seebeck voltage extension line simultaneously, and structure is single, easy to use.Its mode of operation is AFM contact mode, with the diameter of tested thermoelectric material sample 17 interaction contacts area be 30-100nm, realized effective excitation and the output of nanoscale microcell signal.Thermoelectricity detector probe 12 produces harmonic effect under cyclical signal excitation, detects the frequency tripling higher hamonic wave signal directly related with tested thermoelectric material sample 17 thermal conductances, can be in order to reflect the microcell thermal conductivity of tested thermoelectric material sample 17.The frequency of operation of thermoelectricity detector probe 12 must be taken into account the required periodicity thermal source of tested microcell thermal conductance and the required stable state thermal source of Seebeck coefficient simultaneously, and its operating frequency range is 100Hz-10kHz.Meanwhile, working current is set must take into account the optimum Working of thermoelectricity detector probe 12 and effective output of frequency tripling signal, and its current margin is 1mA-100mA.
Thermoelectricity detector probe 12 forms two probe structures with thermoelectricity reference probe 13, adopt differential input mode to be connected with system, so effectively overcome the impact that environment temperature is disturbed, improved the detection sensitivity of tested microcell thermal conductivity coefficient, guarantee the accuracy of test data, reduced test job condition.
Signal generator 16 provides the working power in thermoelectricity detector probe 12, thermoelectricity reference probe 13, two thermoelectricity loops that adjustable resistance network 14,15 forms, and its signal amplitude and frequency are all adjustable.Signal amplitude is taken into account the working current of thermoelectricity detector probe 12, and signal frequency is taken into account microcell thermal conductance simultaneously and detected the pumping signal that required periodic activation signals and microcell Seebeck coefficient detect required steady state thermal power.
Thermoelectricity sample 17, ceramic insulating layer 18, magnetic bases 19, form thermoelectricity sample stage, adopt each other conducting resinl bonding, have effectively guaranteed the mechanical stability of sample and effective transmission of signal.
Signal transmission ends 110, for being bonded at tested thermoelectric material sample 17 upper surface copper sheets and drawing conductor wire, forms microcell Seebeck voltage signal transmission one end.Wherein copper sheet bonds with welding manner, has not only guaranteed the microhm contact of Seebeck voltage lead-in wire; The firm stability of test condition and the reliability of data of having guaranteed goes between simultaneously.
Microcell thermal conductance signal output port 111, realizes institute's nano pyroelectric material microcell thermal conductance frequency tripling signal that detects and exports.Its signal two ends lead-in wire comes from thermoelectricity detector probe 12 one end and thermoelectricity reference probe 13 one end lead-in wires.
Microcell Seebeck voltage signal output port 112, realizes institute's nano pyroelectric material Seebeck voltage signal that detects and exports.Its signal lead one end comes from thermoelectricity detector probe 12, and the other end comes from the copper sheet 110 that is bonded at tested thermoelectric material sample 17 upper surfaces and is welded with conductor wire.
Nanometer thermoelectric many reference amounts signal output procedure not only relates to the multiple physical parameters such as nanoscale region calorifics, electricity, also relate to the signal with different type such as dynamic and stable state simultaneously, and its signal amplitude is faint.Therefore, must guarantee that signal effectively transmits links and all wants reliable, comprise the Ohmic contact of parts shielding, electrical grounding, probe and sample nanoscale contact area.For this reason, insulator is set below tested thermoelectricity sample with by the electrical isolation of system; Adopt multiple shielding mode to comprise the shielding between thermoelectricity probe-sample stage and Outdoor Space simultaneously, and the individual screen of the vitals such as thermoelectricity loop; And various parts electrical equipment is carried out to common ground.Realize signal effectively aspect transmission, must solve thermal probe in nano measurement and the Ohmic contact of thermoelectricity sample.Utilize AFM to differentiate by the detection of power and the test of impedance the Ohmic contact that whether reaches good, thus guarantee faint thermoelectricity many reference amounts signal effectively, accurately transmission.
The work structuring figure of nanometer thermoelectric many reference amounts in situ detection platform 2 as shown in Figure 4, comprise front end loop processing module 21, high sensitivity lock-in amplifier 22, high accuracy number voltmeter 23, data processing and display module 24 etc., detect, process and show the in-situ characterization result of the thermoelectricity many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient in real time in order to realize the original position of faint frequency tripling thermal conductance signal and Seebeck voltage signal.
The work structuring principle of front end loop processing module 21 as shown in Figure 5; comprise front end circuit 211; amplifying circuit 212; holding circuit 213; power supply 214; so that the output signal in thermoelectricity loop is realized to impedance transformation, have simultaneously and improve signal amplitude and defencive function, while preventing the unbalance or signal distortion of electric bridge, produce overload and damage next stage circuit and instrument.
High sensitivity lockin signal amplifier 22 has to be measured highly sensitive, strong interference immunity and tool linearity and non-linear detection function, meets the advantages such as system works requirement, can realize the high-sensitivity detection of faint thermal conductance signal.High accuracy number voltmeter 23 can be realized the high-sensitivity detection of faint Seebeck voltage signal.
Data processing and display module 24 comprise signal processing module and the result display module based on computer platform.Linear relationship based on microcell frequency tripling calorifics signal and excitation signal modulation frequency logarithm, can calculate and obtain microcell thermal conductivity coefficient; Relation between thermistor characteristic based on thermoelectricity probe, thermoelectric material Seebeck voltage and the temperature difference, can calculate and obtain microcell Seebeck coefficient.
Embodiment 1
The nanometer thermoelectric many reference amounts in situ quantitation characterization technique that application the application sets up is tested the microcell thermal conductance of Bi-Sb-Te thermal electric film, and Fig. 6 has shown test result.Wherein Fig. 6 (a) is the AFM picture of sample surface morphology, and Fig. 6 (b) is the microcell frequency tripling thermal conductance signal of three measuring points obtaining in sample corresponding region original position of the nanometer thermoelectric many reference amounts in situ quantitation characterization technique set up and the relation between stimulating frequency logarithm.According to relevant near field calorifics image-forming condition, can calculate and obtain its microcosmic thermal conductivity coefficient is λ=1.668W/ (mK).Because film macroscopic view thermal conductance measuring technology is satisfactorily resolved so far, therefore, this microcell thermal conductance value macroscopic view value corresponding with it cannot be compared.But this value is in close proximity to this thermal conductivity coefficient λ=1.7W/ (mK) that forms corresponding monocrystal material, shows the feasibility of microcell thermal conductance quantitatively characterizing technology and the accuracy of result.
Embodiment 2
The nanometer thermoelectric many reference amounts in situ quantitation characterization technique that application the application sets up is tested the microcell Seebeck coefficient of Bi-Sb-Te thermal electric film, Fig. 7 has shown test result, it must be noted that, this result is the result that in-situ synchronization obtains while characterizing with Fig. 8 microcell thermoelectricity.Fig. 7 (a) is the test result of probe voltage under different exciting voltages, and Fig. 7 (b) is the Seebeck voltage test result under different exciting voltages.According to the peculiar thermistor characteristic of thermal probe and thermoelectricity loop bridge balancing characteristic, can calculate and obtain probe temperature under different exciting voltages by Fig. 7 (a), this temperature is corresponding thermal electric film micro-area temperature.Thus, according to the Seebeck voltage test result shown in calculated micro-area temperature result and Fig. 7 (b), can obtain the test result of Seebeck voltage under the different temperatures shown in Fig. 7 (c).Linear relationship based between thermoelectric material Seebeck voltage and the temperature difference, can calculate and obtain microcell Seebeck coefficient is S=135.54 μ V/K.This value is in close proximity to the macro-test result S=138 μ V/K of this film, shows the feasibility of microcell Seebeck quantitatively characterizing technology and the accuracy of result.
Above-mentioned example table understands that the nanometer thermoelectric many reference amounts in situ quantitation characterization technique of setting up based on atomic force microscope has solved nano pyroelectric material many reference amounts thermoelectricity physical property original position and excited and synchronously detect this great technical barrier.The original position that this novel nano characterization technique has realized nanometer thermoelectric many reference amounts excites simultaneously, in-situ synchronization characterizes, expand the nanometer thermoelectric evaluation of physical property function that existing commercial atomic force microscope does not have, for furtheing investigate the thermoelectricity transport theory of nano pyroelectric material and the deep development of nano pyroelectric material and device thereof, provide important original position, quantitative, nanometer characterizing method.
In sum, the application's outstanding advantages is atomic force microscope nanometer measuring ability, the frequency tripling of macroscopic view thermal conductivity detects principle and macroscopical Seebeck coefficient test philosophy combines, set up based on commercial atomic force microscope and have nanoscale thermal excitation concurrently and the nanometer in situ evaluating apparatus of thermoelectricity many reference amounts detection characteristic, this novel nano characterization apparatus not only has nanometer thermoelectric many reference amounts original position and excites simultaneously, the unique function that in-situ synchronization characterizes, and there is high resolving power, high sensitivity, the advantages such as high s/n ratio, and it is simple in structure, compatible strong, suitable extensive promotion and application.Thus, the original position that the application has solved nanometer thermoelectric many reference amounts in thermoelectric power source material excites and synchronously detects this great technical barrier, can in the strategic brand-new materials such as nano material, energy and material and industry thereof, obtain important application.
Before the description to preferred embodiment is provided so that any technician in this area can use or utilize the application.Various modifications to these embodiment are evident for personnel skilled in the art, and total application of principle described here can not used to creativeness to other embodiment.Thereby the application is the embodiment shown in being not limited to here, and should be according to meeting the principle that disclosed and the wide region of new feature here.
Claims (6)
1. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope, microcell thermal conductivity coefficient and Seebeck coefficient for detection of a tested nano pyroelectric material sample, is characterized in that, comprising:
The atomic force microscope original position stimulating platform of one nanometer thermoelectric many reference amounts, for providing nanometer thermoelectric many reference amounts to excite required basic hardware platform, and realize original position excitation nano thermoelectric material microcell frequency tripling thermal conductance signal and microcell stable state Seebeck d. c. voltage signal simultaneously;
One nanometer thermoelectric many reference amounts in situ detection platform, detects and data processing in real time for realizing the original position of nano pyroelectric material microcell thermal conductance and Seebeck voltage, shows in real time the quantitatively characterizing result of microcell thermal conductivity coefficient and Seebeck coefficient;
Wherein, the atomic force microscope original position stimulating platform of described nanometer thermoelectric many reference amounts further comprises:
One atomic force microscope platform, one thermoelectricity detector probe, one thermoelectricity reference probe, two adjustable resistance networks, one signal generator, one thermoelectric material, one ceramic insulating layer, one magnetic bases, one signal transmission ends, one microcell thermal conductance signal output port, one microcell Seebeck voltage signal output port, described tested nano pyroelectric material sample is placed on described magnetic bases by ceramic insulation described in underlay, described thermoelectricity detector probe, thermoelectricity reference probe, two adjustable resistance networks and signal generator form a thermoelectricity loop, described thermoelectricity detector probe is placed on described tested nano pyroelectric material sample and contact, to detect the voltage of described tested nano pyroelectric material sample point of excitation, the first end of described microcell Seebeck voltage signal output port receives the voltage signal in another region of described tested nano pyroelectric material sample by described signal transmission ends, the second end of described microcell Seebeck voltage signal output port is connected with described thermoelectricity loop earth terminal, the first end of described microcell thermal conductance signal output port connects the described thermoelectricity detector probe end that is connected with described thermoelectricity loop, and its second end connects the described thermoelectricity reference probe end that is connected with described thermoelectricity loop,
Described nanometer thermoelectric many reference amounts in situ detection platform comprises a front end loop processing module, one high sensitivity lock-in amplifier, one high accuracy number voltmeter, one data processing and display system, detect, process and show the in-situ characterization result of microcell thermal conductivity coefficient and Seebeck coefficient in real time for realizing the original position of faint frequency tripling thermal conductance signal and Seebeck voltage signal.
2. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 1, is characterized in that,
The mode of operation of described atomic force microscope platform is contact mode.
3. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 1, is characterized in that,
Described thermoelectricity detector probe is the probe of a tool thermistor characteristic, has the function of microcell driving source, signal transducer and detection resources simultaneously; The mode of operation of described thermoelectricity detector probe is AFM contact mode, and its micro-cantilever deformation quantity as feedback parameters is 0.1-5nm, with the diameter of described tested nano pyroelectric material sample interaction contact area be 30-100nm.
4. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 3, is characterized in that,
The operating frequency range of described thermoelectricity probe is 100Hz-10kHz, and current margin is 1mA-100mA.
5. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 1, is characterized in that,
Described thermoelectricity detector probe in described thermoelectricity loop and described thermoelectricity reference probe adopt differential input mode to be connected to form two probe structures.
6. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 5, is characterized in that,
Its adjustment mode of described thermoelectricity loop comprises that the adjustment of thermoelectricity probe recommended current, thermoelectricity loop fundamental signal suppress to adjust, harmonic signal sensitivity increases the three kinds of patterns of adjusting.
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| CN201210205677.XA CN102692427B (en) | 2012-06-20 | 2012-06-20 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
| PCT/CN2012/079079 WO2013189112A1 (en) | 2012-06-20 | 2012-07-24 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
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| CN103336149B (en) * | 2013-06-25 | 2015-07-29 | 苏州新锐博纳米科技有限公司 | Based on atomic force microscopy micro-cantilever and the application of nano particle dot array Quantum Transport |
| CN103344790B (en) * | 2013-07-08 | 2015-08-19 | 中国科学院上海硅酸盐研究所 | A kind of device based on scanning calorifics microscope in-situ characterization nanometer thermoelectric Seebeck coefficient |
| CN103412150B (en) * | 2013-08-30 | 2015-04-22 | 哈尔滨工业大学 | Double-probe atomic power microscope and method for realizing nanometer structure operation by adopting microscope |
| CN104111268B (en) * | 2014-05-12 | 2016-09-07 | 中国科学院上海硅酸盐研究所 | A kind of AFM conducting probe In Situ Heating, the device of in-situ characterization nano-plug seebeck coefficient |
| CN105510637B (en) * | 2014-09-24 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | Micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy and detection method |
| CN105510639B (en) * | 2014-09-24 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | Probe, preparation method and detection method in a kind of scanning probe microscopy |
| CN104614557B (en) * | 2015-02-02 | 2017-07-18 | 国家纳米科学中心 | A kind of material domain conductance and the measurement apparatus of thermoelectric property, measuring method and application thereof |
| CN106771372A (en) * | 2017-01-18 | 2017-05-31 | 中国科学院深圳先进技术研究院 | Thermoelectricity detecting system and thermoelectricity detection method |
| CN106770445A (en) * | 2017-01-18 | 2017-05-31 | 中国科学院深圳先进技术研究院 | Thermoelectricity detecting system and thermoelectricity detection method |
| CN110579628B (en) * | 2018-06-11 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | In-situ characterization device for nanoscale extremely-low thermal conductance |
| CN111693565B (en) * | 2019-03-12 | 2024-05-14 | 湘潭大学 | Dynamic detection system and detection method for electrothermal performance |
| CN110907489A (en) * | 2019-11-13 | 2020-03-24 | 中国科学院上海硅酸盐研究所 | Nanoscale thermal conductivity-electric domain in-situ characterization device based on atomic force microscope |
| CN111912813B (en) * | 2020-07-13 | 2023-07-18 | 中国科学院上海硅酸盐研究所 | Nanometer thermal infrared microscopy device |
| CN111948250B (en) * | 2020-08-13 | 2023-01-13 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN113092825B (en) * | 2021-03-05 | 2022-12-30 | 中山大学 | Atomic force microscope system and current detection method thereof |
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