CN102692427A - 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
- Publication number
- CN102692427A CN102692427A CN201210205677XA CN201210205677A CN102692427A CN 102692427 A CN102692427 A CN 102692427A CN 201210205677X A CN201210205677X A CN 201210205677XA CN 201210205677 A CN201210205677 A CN 201210205677A CN 102692427 A CN102692427 A CN 102692427A
- Authority
- CN
- China
- Prior art keywords
- thermoelectric
- nano
- atomic force
- force microscope
- situ
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/58—SThM [Scanning Thermal Microscopy] or apparatus therefor, e.g. SThM probes
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 has very wide application prospect as a kind of important strategic performance source material 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 the development high performance thermoelectric material.Thus, nano pyroelectric material has become the research field that thermoelectric boundary, the current world is the most active, be hopeful to make a breakthrough most, and the measurement of nanometer thermoelectric performance and sign also become the challenge problem that solution is badly in need of in this field day by day.
Thermal conductivity and Seebeck coefficient are two important physical parameters in the thermoelectric material rerum natura; It characterizes conventional art and the method still continued to use at present; This method has following limitation: (1) its thermal excitation or heat detect the macro property that has only reflected sample, reach the nanoscale level far away; (2) its method of testing is in static state, only adopts the thermal excitation mode of stable state to realize that single-point detects, and can't reflect heat electric material dynamic property reach continuously reflection parameter to be detected with the variable condition of locus; (3) test of thermoelectric many reference amounts such as thermal conductance, Seebeck coefficient is to adopt many cover discrete devices to accomplish, and can't reach real-time, synchronous detection.Thereby the conventional test methodologies of thermoelectric material rerum natura is difficult to realize the original position of the comprehensive rerum natura of nano pyroelectric material, real-time, integrated sign.To above limitation, the application hope to set up the original position that can realize nano pyroelectric material many reference amounts rerum natura, harmless, in real time, dynamically, quantitatively, the nanometer characterization system, with the urgent need of the nano pyroelectric material rerum natura sign that satisfies current fast development.
Atomic force microscope (AFM) is one of current important tool of carrying out nano science research; It has distinct advantages such as High Accuracy Control, nanometer resolution; Become a kind of nanometer detection platform of maturation, and on its basis, developing new technology, expanding new function important platform base is provided.
The active demand that the application characterizes to present nanometer thermoelectric physical property; Based on characteristics such as the detection maturity of AFM nanometer platform, multiple functional property and structural integrity; Set up the in situ quantitation characterization apparatus of nanometer thermoelectric many reference amounts; Realized the original position of nano pyroelectric material thermal conductivity and Seebeck coefficient, in real time, dynamically, quantitative test, for the deep development of thermoelectric transport theory, nano pyroelectric material and the device thereof of further investigation nano pyroelectric material provides important in situ quantitation nanometer characterizing method.Still there is not report in this respect at present both at home and abroad.
Summary of the invention
The application's purpose is to provide thermoelectric many reference amounts such as a kind of nanometer thermal conductivity coefficient that can be used in the nanometer thermoelectric energy and material, nanometer Seebeck coefficient to characterize the in situ quantitation nanometer characterization apparatus of usefulness.The atomic force microscope nanometer measuring ability is detected principle with the frequency tripling of macroscopical thermal conductivity to this technology and macroscopical Seebeck coefficient test philosophy combines; Based on commercial AFM nanometer detection platform; Set up the nanometer original position assessment technique that has nanoscale thermal excitation and thermoelectric 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 advantages such as high resolving power, high sensitivity, high s/n ratio.The described gordian technique apparatus structure of the application is simple, compatible strong, fits and different commercial AFM system combines, and 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; Be used to detect the thermoelectric Physical Parameters such as microcell thermal conductivity coefficient and Seebeck coefficient of a tested nano pyroelectric material sample; It is characterized in that; Comprise: the atomic force microscope original position stimulating platform of nanometer thermoelectric many reference amounts; Be used to provide the 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 is used to realize that the original position of nano pyroelectric material microcell thermal conductance and Seebeck voltage detects and data processing in real time, shows the quantitatively characterizing result of microcell thermal conductivity coefficient and Seebeck coefficient in real time.
Reasonable is that the atomic force microscope original position stimulating platform of said nanometer thermoelectric many reference amounts further comprises: an atomic force microscope platform, a thermoelectric detector probe; One thermoelectric reference probe, two adjustable resistance networks, a signal generator; One thermoelectric material, a ceramic insulating layer, magnetic bases; One signal transmission ends, a microcell thermal conductance signal output port, a microcell Seebeck voltage signal output end mouth; Said tested thermoelectric material sample is placed on the said magnetic bases through the said ceramic insulation of underlay; Said thermoelectric detector probe, thermoelectric reference probe, two adjustable resistance networks and signal generator are formed a Wheatstone bridge, and said thermoelectric detector probe places on the said tested thermoelectric material sample and contact, to detect the voltage of said tested thermoelectric material sample point of excitation; First end of said microcell Seebeck voltage signal output end mouth receives said another regional voltage signal of tested thermoelectric material sample through said signal transmission ends, and second end of said microcell Seebeck voltage signal output end mouth links to each other with said Wheatstone bridge earth terminal; First end of said microcell thermal conductance signal output port connects the said thermoelectric detector probe end that links to each other with said Wheatstone bridge, and its second end connects the said thermoelectric reference probe end that links to each other with said Wheatstone bridge.
Reasonable is that the mode of operation of said atomic force microscope platform is a contact mode.
Reasonable is that said thermoelectric 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 said thermoelectric detector probe is the AFM contact mode, and its micro-cantilever deformation quantity as feedback parameters is 0.1-5nm, with the diameter of said tested thermoelectric material sample interaction contact area be 30-100nm.
Reasonablely be, the operating frequency range of said thermoelectric probe is 100Hz-10kHz, and current margin is 1mA-100mA.
Reasonablely be that the said thermoelectric detector probe in the said Wheatstone bridge adopts differential input mode to link to each other with said thermoelectric reference probe to constitute two probe structures.
Reasonable is that its adjustment mode of said thermoelectric loop comprises that thermoelectric probe recommended current adjustment, thermoelectric loop fundamental signal suppress adjustment, harmonic signal sensitivity increases three kinds of patterns of adjustment.
Reasonablely be; End loop processing module before said nanometer thermoelectric many reference amounts in situ detection platform comprises one; One high sensitivity lock-in amplifier; One high accuracy number voltmeter, a data processing and display system, the original position that is used to realize faint frequency tripling thermal conductance signal and Seebeck voltage signal detects, handles and show the in-situ characterization result of thermoelectric many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient in real time.
The nanometer thermoelectric many reference amounts in situ quantitation characterization apparatus that adopts said structure to set up has solved the thermoelectric rerum natura original position of nano pyroelectric material many reference amounts and has excited and this great technical barrier of synchronous detection.This novel nano characterization apparatus has realized that the original position of nanometer thermoelectric many reference amounts excites simultaneously, in-situ synchronization detects; Expanded the nanometer thermoelectric evaluation of physical property function that existing commercial atomic force microscope did not have, for the deep development of thermoelectric transport theory and the nano pyroelectric material and the device thereof of further investigation nano pyroelectric material provide important original position, quantitatively, the nanometer characterization apparatus.
Description of drawings
Below, with reference to accompanying drawing, for those skilled in the art that, from the detailed description to the application, above-mentioned and other purposes of the application, feature and advantage will be obvious.
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 atomic force microscope platform (AFM) among Fig. 2;
Fig. 4 illustrates the structured flowchart of nanometer thermoelectric many reference amounts in situ detection platform among Fig. 1;
The structured flowchart of end loop processing module before Fig. 5 illustrates among 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 microcell thermal conductance quantitatively characterizing result in view of the above;
Fig. 7 (a) has provided probe voltage (U under the different exciting voltages
Probe) test result;
Fig. 7 (b) is the Seebeck voltage (U under the different exciting voltages
Seebeck) test result;
Fig. 7 (c) has provided Seebeck voltage (U under the different temperatures
Seebeck-Δ T
Probe) test result, can calculate the microcell Seebeck coefficient in view of the above.
Embodiment
Following instance all is to use the quantitatively characterizing result of the application's nanometer thermoelectric many reference amounts in situ quantitation characterization technique to thermoelectric many reference amounts such as nanometer thermoelectric membraneous material microcell thermal conductivity coefficient and microcell Seebeck coefficients; Further specifying 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 is as shown in Figure 1; Form by two parts: 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 thermoelectric 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; Detect in real time and handle in order to the original position that realizes nano pyroelectric material microcell thermal conductance signal and Seebeck voltage signal, show the in-situ characterization result of thermoelectric 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 is as shown in Figure 2, mainly comprises atomic force microscope platform 11, thermoelectric detector probe 12; 13, two adjustable resistance networks of thermoelectric reference probe 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 end mouth 112 etc.; Wherein, tested thermoelectric material sample 17 places through underlay ceramic insulating layer 18 on the magnetic bases 19 of atomic force microscope platform 11, thermoelectric detector probe 12; 13, two adjustable resistance networks of thermoelectric reference probe 14,15, signal generator 16 is formed Wheatstone bridge (Wheat stone bri dge); Thermoelectric detector probe 12 places on the tested thermoelectric material sample 17 and contact, with the voltage of test sample point of excitation.First end of microcell Seebeck voltage signal output end mouth 112 receives tested thermoelectric material sample 17 another regional voltage signals through signal transmission ends 110, and second end of microcell Seebeck voltage signal output end mouth 112 links to each other with the electric bridge earth terminal.In addition, first end of microcell thermal conductance signal output port 111 connects thermoelectric detector probe 12 end that links to each other with electric bridge, and its second end connects thermoelectric reference probe 13 end that links to each other with electric bridge.
The AFM original position stimulating platform 1 of the nanometer thermoelectric many reference amounts of said structure excites required basic hardware platform in order to the nanometer thermoelectric many reference amounts to be provided, and realizes that original position excites 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 the thermoelectric many reference amounts function of original position while excitation nano mainly comes from thermal probe and sample.For the microcell thermal conductance, its physical process that excites can be explained as follows: when signal generator 16 applied periodic activation signals and acts on thermoelectric detector probe 12, thermoelectric detector probe 12 temperature raise (being higher than room temperature), cause the resistance of probe 12 to increase.This moment is when thermoelectric detector probe 12 contacts with tested thermoelectric material sample 17, because the existence of both temperature difference, thermoelectric detector probe 12 will produce heat exchange action with tested thermoelectric material sample 17.This heat interchange effect has induced the surface temperature of thermoelectric detector probe 12 and thermally sensitive resistance thereof to change; Because thermoelectric detector probe 12 is ends of electric bridge brachium pontis; The variation of the resistance of thermoelectric detector probe 12 will cause this bridge circuit uneven; Produced frequency tripling higher harmonic voltage output signal and passed through 111 outputs of microcell thermal conductance signal output port, this output signal is directly related with tested microcell thermal conductance.Thus, the original position that has realized the microcell thermal conductance excites.Simultaneously, the heat interchange effect between above-mentioned thermal probe-sample also can have been induced a temperature difference source between sample point of excitation (temperature end) that thermoelectric detector probe 12 is contacted and signal transmission ends 110 neighboring areas of living in (low-temperature end, room temperature).Based on the peculiar Seebeck effect of thermoelectric material, this temperature difference source will produce the Seebeck voltage signal in tested thermoelectric material sample 17.Because the 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 realized microcell Seebeck voltage signal simultaneously excites.Thereby, in thermoelectric material, but utilize pyroelectric signal driver unit original position to excite microcell frequency tripling thermal conductance signal and microcell Seebeck direct current steady state voltage signal simultaneously.
Fig. 3 has provided the further structured flowchart of atomic force microscope platform 11 among Fig. 2, and this microscope stage 11 is commercial atomic force microscope (AFM), has High Accuracy 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. detect required basic hardware platform in order to nanometer thermoelectric to be provided.The AFM mode of operation is a contact mode, and its feedback parameters (micro-cantilever deformation quantity) is 0.1-5nm, in order to realize that good nanoscale contacts and effective signal excitation and transmission between thermoelectric probe and the sample.
Return among Fig. 2, thermoelectric detector probe 12, thermoelectric reference probe 13, two adjustable resistance networks 14,15 and signal generator 16 constitute thermoelectric loop, realize thermoelectric many reference amounts frequency tripling signal excitation.The bridge structure with high detection sensitivity characteristics is adopted in this thermoelectricity loop, and this bridge structure is significantly different with the general bridge structure that only can detect the single one physical amount.Wherein the bridge circuit integrally closed in thermoelectric loop is in can, with the shielding undesired signal; And two adjustable resistance networks 14,15 are selected accurate noninductive resistance for use, influence accuracy of detection with the distribution parameter of avoiding electronic component.
Thermoelectric loop signal comprises fundamental signal and frequency tripling harmonic signal, and wherein harmonic signal reflects thermoelectric material microcell thermal conductance signal to be detected, and the duty of this thermal conductance signal and thermal probe is closely related.The adjustment mode of thermoelectric detector probe duty comprises that thermoelectric probe recommended current adjustment, thermoelectric loop fundamental signal suppress adjustment, harmonic signal sensitivity increases three kinds of patterns such as adjustment in the thermoelectric loop.Two adjustable resistance networks 14,15 in the thermoelectric bridge circuit, one of them adjustable resistance network 14 are in order to the adjustment bridge balancing, thus the output of inhibition fundamental signal; Another adjustable resistance network 15 realizes that in order to regulate the working current of thermoelectric detector probe 12 thermoelectric detector probe 12 is in optimum Working.Simultaneously, adopt nonlinear element with adjustment and the relevant frequency tripling harmonic component of thermoelectric material microcell thermal conductance signal to be detected in this thermoelectricity loop, thereby improve harmonic signal sensitivity.
Signal transmission ends 110 for being bonded at tested thermoelectric material sample 17 upper surface copper sheets and drawing conductor wire, constitutes microcell Seebeck voltage signal and transmits an end.Wherein copper sheet bonds with welding manner, has not only guaranteed the microhm contact of Seebeck voltage lead; The firm stability of test condition and the reliability of data of having guaranteed simultaneously goes between.
Microcell thermal conductance signal output port 111 realizes that institute's nano pyroelectric material microcell thermal conductance frequency tripling signal that detects exports.Its signal two ends lead-in wire comes from thermoelectric detector probe 12 1 ends and thermoelectric reference probe 13 1 ends lead-in wire.
Microcell Seebeck voltage signal output end mouth 112 realizes that institute's nano pyroelectric material Seebeck voltage signal that detects exports.Its signal lead one end comes from thermoelectric 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 multiple physical parameters such as nanoscale zone calorifics, electricity, also relate to signal with different type such as dynamic and stable state simultaneously, and its signal amplitude is faint.Therefore, must guarantee that signal effectively transmits each link and all wants reliable, comprise the Ohmic contact of parts shielding, electrical grounding, probe and sample nanoscale contact area.For this reason, below tested thermoelectric sample, insulator is set with electrical isolation with system; Adopt multiple shielding mode to comprise the shielding between thermoelectric probe-sample stage and the external environment condition space simultaneously, and the individual screen of vitals such as thermoelectric loop; And each parts electrical equipment of system is carried out common ground.Realize signal effectively aspect the transmission, must solve thermal probe and the Ohmic contact of thermoelectric sample in the nano measurement.Utilize AFM to differentiate whether reach good Ohmic contact, thereby guarantee effective, the accurately transmission of faint thermoelectric many reference amounts signal through the detection of power and the test of impedance.
The work structuring figure of nanometer thermoelectric many reference amounts in situ detection platform 2 is as shown in Figure 4; End loop processing module 21 before comprising; High sensitivity lock-in amplifier 22; High accuracy number voltmeter 23, data processing and display module 24 etc. detect, handle and show the in-situ characterization result of thermoelectric many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient in real time in order to the original position that realizes faint frequency tripling thermal conductance signal and Seebeck voltage signal.
The work structuring principle of preceding end loop processing module 21 is 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 thermoelectric loop is realized impedance conversion, have the signal amplitude of raising and defencive function simultaneously, produce overload when preventing the unbalance or signal distortion of electric bridge 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, satisfies advantage 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 based on the signal processing module of computer platform and display module as a result.Based on the linear relationship of microcell frequency tripling calorifics signal and excitation signal modulation frequency logarithm, can calculate and obtain the microcell thermal conductivity coefficient; Based on the relation between thermistor characteristic, thermoelectric material Seebeck voltage and the temperature difference of thermoelectric probe, can calculate and obtain the microcell Seebeck coefficient.
Use the nanometer thermoelectric many reference amounts in situ quantitation characterization technique of the application's foundation the microcell thermal conductance of Bi-Sb-Te thermal electric film is tested, Fig. 6 has shown test result.Wherein Fig. 6 (a) is the AFM picture of sample surfaces pattern, the microcell frequency tripling thermal conductance signal of Fig. 6 (b) three measuring points that to be the nanometer thermoelectric many reference amounts in situ quantitation characterization technique set up obtain in sample corresponding region original position and the relation between the 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, can't the macroscopic view value that this microcell thermal conductance value is corresponding with it compare.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 result's accuracy.
Using the nanometer thermoelectric many reference amounts in situ quantitation characterization technique of the application's foundation tests 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 when characterizing with Fig. 8 microcell is thermoelectric.Fig. 7 (a) is the test result of probe voltage under the different exciting voltages, and Fig. 7 (b) is the Seebeck voltage tester result under the different exciting voltages.According to peculiar thermistor characteristic of thermal probe and thermoelectric loop bridge balancing characteristic, can calculate by Fig. 7 (a) and obtain probe temperature under the different exciting voltages, this temperature is corresponding thermal electric film micro-area temperature.Thus, according to the Seebeck voltage tester result shown in the micro-area temperature result who is calculated and Fig. 7 (b), can obtain the test result of Seebeck voltage under the different temperatures shown in Fig. 7 (c).Based on the linear relationship between the thermoelectric material Seebeck voltage and the temperature difference, can calculate and obtain the microcell Seebeck coefficient is S=135.54 μ V/K.The macro-test that this value is in close proximity to this film is S=138 μ V/K as a result, shows the feasibility of microcell Seebeck quantitatively characterizing technology and result's accuracy.
The clear nanometer thermoelectric many reference amounts in situ quantitation characterization technique of setting up based on atomic force microscope of above-mentioned example table has solved the thermoelectric rerum natura original position of nano pyroelectric material many reference amounts and has excited and this great technical barrier of synchronous detection.This novel nano characterization technique has realized that the original position of nanometer thermoelectric many reference amounts excites simultaneously, in-situ synchronization characterizes; Expanded the nanometer thermoelectric evaluation of physical property function that existing commercial atomic force microscope did not have, for the deep development of thermoelectric transport theory and the nano pyroelectric material and the device thereof of further investigation nano pyroelectric material provide important original position, quantitatively, the nanometer characterizing method.
In sum; The outstanding advantage of the application is frequency tripling detection principle and macroscopical Seebeck coefficient test philosophy of atomic force microscope nanometer measuring ability, macroscopical thermal conductivity are combined; Set up based on commercial atomic force microscope and have the nanoscale thermal excitation concurrently and thermoelectric many reference amounts detect the nanometer original position evaluating apparatus of characteristic; This novel nano characterization apparatus not only has the unique function that nanometer thermoelectric many reference amounts original position excites simultaneously, in-situ synchronization characterizes; And have advantages such as high resolving power, high sensitivity, 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 the thermoelectric power source material excites and this great technical barrier of synchronous detection, can in strategic brand-new materials such as nano material, energy and material and industry thereof, obtain important application.
The front provides the description to preferred embodiment, so that any technician in this area can use or utilize the application.Various modifications to these embodiment are conspicuous to those skilled in the art, can be applied to other embodiment to total principle described here and not use creativeness.Thereby, the embodiment shown in the application will be not limited to here, and the wide region of principle that should disclose and new feature according to meeting here.
Claims (8)
1. nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope is used to detect the thermoelectric Physical Parameters such as microcell thermal conductivity coefficient and Seebeck coefficient of a tested nano pyroelectric material sample, it is characterized in that, comprising:
The atomic force microscope original position stimulating platform of one nanometer thermoelectric many reference amounts; Be used to provide the 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 is used to realize that the original position of nano pyroelectric material microcell thermal conductance and Seebeck voltage detects and data processing in real time, shows the quantitatively characterizing result of microcell thermal conductivity coefficient and Seebeck coefficient in real time.
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 atomic force microscope original position stimulating platform of said nanometer thermoelectric many reference amounts further comprises:
One atomic force microscope platform, a thermoelectric detector probe, a thermoelectric reference probe; Two adjustable resistance networks, a signal generator, a thermoelectric material; One ceramic insulating layer, magnetic bases, a signal transmission ends; One microcell thermal conductance signal output port; One microcell Seebeck voltage signal output end mouth, said tested thermoelectric material sample is placed on the said magnetic bases through the said ceramic insulation of underlay, and said thermoelectric detector probe, thermoelectric reference probe, two adjustable resistance networks and signal generator are formed a Wheatstone bridge; Said thermoelectric detector probe places on the said tested thermoelectric material sample and contact, to detect the voltage of said tested thermoelectric material sample point of excitation; First end of said microcell Seebeck voltage signal output end mouth receives said another regional voltage signal of tested thermoelectric material sample through said signal transmission ends, and second end of said microcell Seebeck voltage signal output end mouth links to each other with said Wheatstone bridge earth terminal; First end of said microcell thermal conductance signal output port connects the said thermoelectric detector probe end that links to each other with said Wheatstone bridge, and its second end connects the said thermoelectric reference probe end that links to each other with said Wheatstone bridge.
3. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 2 is characterized in that,
The mode of operation of said atomic force microscope platform is a contact mode.
4. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 2 is characterized in that,
Said thermoelectric 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 said thermoelectric detector probe is the AFM contact mode, and its micro-cantilever deformation quantity as feedback parameters is 0.1-5nm, with the diameter of said tested thermoelectric material sample interaction contact area be 30-100nm.
5. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 4 is characterized in that,
The operating frequency range of said thermoelectric probe is 100Hz-10kHz, and current margin is 1mA-100mA.
6. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 2 is characterized in that,
Said thermoelectric detector probe in the said Wheatstone bridge and said thermoelectric reference probe adopt differential input mode to link to each other to constitute two probe structures.
7. the nanometer thermoelectric energy and material many reference amounts in situ quantitation characterization apparatus based on atomic force microscope according to claim 6 is characterized in that,
Its adjustment mode of said thermoelectric loop comprises that thermoelectric probe recommended current adjustment, thermoelectric loop fundamental signal suppress adjustment, harmonic signal sensitivity increases three kinds of patterns of adjustment.
8. 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,
End loop processing module before said nanometer thermoelectric many reference amounts in situ detection platform comprises one; One high sensitivity lock-in amplifier; One high accuracy number voltmeter; One data processing and display system, the original position that is used to realize faint frequency tripling thermal conductance signal and Seebeck voltage signal detects, handles and show the in-situ characterization result of thermoelectric many reference amounts physical parameters such as microcell thermal conductivity coefficient and Seebeck coefficient in real time.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210205677.XA CN102692427B (en) | 2012-06-20 | 2012-06-20 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102692427A true CN102692427A (en) | 2012-09-26 |
| CN102692427B CN102692427B (en) | 2014-07-16 |
Family
ID=46858024
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210205677.XA Active CN102692427B (en) | 2012-06-20 | 2012-06-20 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN102692427B (en) |
| WO (1) | WO2013189112A1 (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103336149A (en) * | 2013-06-25 | 2013-10-02 | 苏州新锐博纳米科技有限公司 | Atomic force microscopy micro cantilever and application based on nanometer particle lattice quantum transportation |
| CN103344790A (en) * | 2013-07-08 | 2013-10-09 | 中国科学院上海硅酸盐研究所 | Nano thermoelectrical Seebeck coefficient in-situ characterization device based on scanning thermal microscope |
| CN103412150A (en) * | 2013-08-30 | 2013-11-27 | 哈尔滨工业大学 | Double-probe atomic power microscope and method for realizing nanometer structure operation by adopting microscope |
| CN104111268A (en) * | 2014-05-12 | 2014-10-22 | 中国科学院上海硅酸盐研究所 | Device for in-situ heating of atomic force microscope conducting probe and in-situ characterization of nanometer Seebeck coefficient |
| CN104614557A (en) * | 2015-02-02 | 2015-05-13 | 国家纳米科学中心 | Device and method for measuring micro-zone electric conductance and thermoelectric properties of material and application thereof |
| CN105510637A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Micro-nano thermoelectric in-situ detection device and method based on scanning probe microscope |
| CN105510639A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe |
| 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 |
| 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 |
| CN110579628A (en) * | 2018-06-11 | 2019-12-17 | 中国科学院上海硅酸盐研究所 | In-situ characterization device for nanoscale extremely-low thermal conductance |
| 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 |
| CN111912813A (en) * | 2020-07-13 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Nano thermal infrared microscopy device |
| CN111948250A (en) * | 2020-08-13 | 2020-11-17 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN113092825A (en) * | 2021-03-05 | 2021-07-09 | 中山大学 | Atomic force microscope system and current detection method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6467951B1 (en) * | 2000-08-18 | 2002-10-22 | International Business Machines Corporation | Probe apparatus and method for measuring thermoelectric properties of materials |
| CN102305807A (en) * | 2011-05-25 | 2012-01-04 | 清华大学 | Method for measuring Seebeck coefficient of micro/nano thermoelectric materials or devices |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6487515B1 (en) * | 2000-08-18 | 2002-11-26 | International Business Machines Corporation | Method and apparatus for measuring thermal and electrical properties of thermoelectric materials |
| US6679625B2 (en) * | 2001-12-17 | 2004-01-20 | International Business Machines Corporation | Scanning heat flow probe |
| CN1975372A (en) * | 2006-12-01 | 2007-06-06 | 中山大学 | Scanning samples electric heating device used for atomic force microscope |
| CN102053170B (en) * | 2009-11-09 | 2012-06-06 | 中国科学院上海硅酸盐研究所 | Micro/nano-scale thermal detection-based nonlinear amplifier |
| CN102053171B (en) * | 2009-11-09 | 2012-06-06 | 中国科学院上海硅酸盐研究所 | Micron-nano thermal detecting and sensing component |
-
2012
- 2012-06-20 CN CN201210205677.XA patent/CN102692427B/en active Active
- 2012-07-24 WO PCT/CN2012/079079 patent/WO2013189112A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6467951B1 (en) * | 2000-08-18 | 2002-10-22 | International Business Machines Corporation | Probe apparatus and method for measuring thermoelectric properties of materials |
| CN102305807A (en) * | 2011-05-25 | 2012-01-04 | 清华大学 | Method for measuring Seebeck coefficient of micro/nano thermoelectric materials or devices |
Non-Patent Citations (2)
| Title |
|---|
| S. LEFEVRE ET AL.: "《Probe calibration of the scanning thermal microscope in the AC mode》", 《SUPERLATTICES AND MICROSTRUCTURES》 * |
| 王照亮: "《微纳米尺度材料热物性表征与热输运机理研究》", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103336149A (en) * | 2013-06-25 | 2013-10-02 | 苏州新锐博纳米科技有限公司 | Atomic force microscopy micro cantilever and application based on nanometer particle lattice quantum transportation |
| 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 |
| CN103344790A (en) * | 2013-07-08 | 2013-10-09 | 中国科学院上海硅酸盐研究所 | Nano thermoelectrical Seebeck coefficient in-situ characterization device based on scanning thermal microscope |
| 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 |
| CN103412150A (en) * | 2013-08-30 | 2013-11-27 | 哈尔滨工业大学 | Double-probe atomic power microscope and method for realizing nanometer structure operation by adopting microscope |
| 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 |
| CN104111268A (en) * | 2014-05-12 | 2014-10-22 | 中国科学院上海硅酸盐研究所 | Device for in-situ heating of atomic force microscope conducting probe and in-situ characterization of nanometer Seebeck coefficient |
| 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 |
| 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 |
| CN105510637A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Micro-nano thermoelectric in-situ detection device and method based on scanning probe microscope |
| CN105510639A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe |
| 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 |
| CN104614557A (en) * | 2015-02-02 | 2015-05-13 | 国家纳米科学中心 | Device and method for measuring micro-zone electric conductance and thermoelectric properties of material 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 |
| CN110579628A (en) * | 2018-06-11 | 2019-12-17 | 中国科学院上海硅酸盐研究所 | In-situ characterization device for nanoscale extremely-low thermal conductance |
| 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 |
| 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 |
| CN111912813A (en) * | 2020-07-13 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Nano thermal infrared microscopy device |
| CN111948250A (en) * | 2020-08-13 | 2020-11-17 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN111948250B (en) * | 2020-08-13 | 2023-01-13 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN113092825A (en) * | 2021-03-05 | 2021-07-09 | 中山大学 | Atomic force microscope system and current detection method thereof |
| CN113092825B (en) * | 2021-03-05 | 2022-12-30 | 中山大学 | Atomic force microscope system and current detection method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102692427B (en) | 2014-07-16 |
| WO2013189112A1 (en) | 2013-12-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102692427B (en) | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope | |
| CN103344790B (en) | A kind of device based on scanning calorifics microscope in-situ characterization nanometer thermoelectric Seebeck coefficient | |
| CN102692524B (en) | A kind of nano thermoelectric seebeck coefficient in-situ quantitative characterization device based on atomic force microscope | |
| CN102760727B (en) | Testing device and method of electromigration of interconnection line | |
| CN110579628B (en) | In-situ characterization device for nanoscale extremely-low thermal conductance | |
| CN107430148B (en) | Using scanning probe microscopy to the method for characteristic imaging | |
| Bhatia et al. | Pyroelectric current measurements on PbZr0. 2Ti0. 8O3 epitaxial layers | |
| CN106770445A (en) | Thermoelectricity detecting system and thermoelectricity detection method | |
| Park et al. | Wireless guided wave and impedance measurement using laser and piezoelectric transducers | |
| Mesalam et al. | Towards a comprehensive model for characterising and assessing thermoelectric modules by impedance spectroscopy | |
| CN104111268A (en) | Device for in-situ heating of atomic force microscope conducting probe and in-situ characterization of nanometer Seebeck coefficient | |
| Notingher et al. | An insight into space charge measurements | |
| Nguyen et al. | Study for the non-contact characterization of metallization ageing of power electronic semiconductor devices using the eddy current technique | |
| CN103901234A (en) | In-situ integration representation device of multiferroic material nanoscale domain structure | |
| CN102053171A (en) | Micron-nano thermal detecting and sensing component | |
| CN209745854U (en) | dynamic detection system for electric heating performance | |
| CN111766264B (en) | Device for in-situ characterization of nanoscale thermal conductivity by controlling excitation through thermal wave hopping for atomic force microscope | |
| Bodzenta et al. | Reduced thermal quadrupole heat transport modeling in harmonic and transient regime scanning thermal microscopy using nanofabricated thermal probes | |
| CN206489103U (en) | Thermoelectricity detecting system | |
| Hou et al. | Nonintrusive near-field characterization of spatially distributed effects in large-periphery high-power GaN HEMTs | |
| Borca-Tasciuc et al. | Experimental techniques for thin-film thermal conductivity characterization | |
| Cho et al. | Nanoscale mapping of molecular vibrational modes via vibrational noise spectroscopy | |
| CN110907489A (en) | Nanoscale thermal conductivity-electric domain in-situ characterization device based on atomic force microscope | |
| Jakoby et al. | A novel microacoustic viscosity sensor providing integrated sample temperature control | |
| JP4265606B2 (en) | Non-contact conductivity measuring device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211222 Address after: 215400 No.6 Liangfu Road, Taicang City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Institute of advanced inorganic materials Address before: 200050 No. 1295 Dingxi Road, Shanghai, Changning District Patentee before: SHANGHAI INSTITUTE OF CERAMICS, CHINESE ACADEMY OF SCIENCES |
|
| TR01 | Transfer of patent right |