CN106771372A - Thermoelectricity detecting system and thermoelectricity detection method - Google Patents
Thermoelectricity detecting system and thermoelectricity detection method Download PDFInfo
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- CN106771372A CN106771372A CN201710034720.3A CN201710034720A CN106771372A CN 106771372 A CN106771372 A CN 106771372A CN 201710034720 A CN201710034720 A CN 201710034720A CN 106771372 A CN106771372 A CN 106771372A
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- 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
Abstract
The present invention provides a kind of thermoelectricity detecting system and thermoelectricity detection method.The thermoelectricity detecting system is used to detect the thermoelectricity capability of material nano yardstick, the thermoelectricity detecting system includes scanning probe, sample stage, heater element, detection circuit and controller, the sample stage is used to carry sample, the scanning probe is used to that sample to be heated and detected under probe excitation pattern, the heater element is used to heat sample under non-probe excitation pattern, the scanning probe is additionally operable to detect sample under non-probe excitation pattern, the detection circuit is used for the change in electric detected on the scanning probe and exports detection signal, the controller is used for the thermoelectricity capability for being controlled and receiving the detection signal of the detection circuit output with output to the input of signal and the sample is analyzed based on the detection signal.
Description
Technical field
The present invention relates to electronic technology field, more particularly to a kind of thermoelectricity detecting system and thermoelectricity detection method.
Background technology
With the low-dimensional and miniaturization of material and device, electricity, thermotransport problem on nanoscale become increasingly conspicuous, to receiving
Rice material has a huge impact with the performance of device, and it is studied also has turned into material science, Condensed Matter Physics and micro-nano
The forward position focus of the crossing domains such as device.Carrier in semi-conducting material can be sent out under the driving of external electric field and thermograde
Raw displacement, causes intercoupling between electricity, heat transfer, and this migration can also be subject to impurity, defect, boundary in material
Face and the scattering of lattice vibration.These factors are competed with one another for, and material is finally reached the nonequilibrium condition of stable state.It is multiple in nanometer
In condensation material, this effect is the most obvious.
Due to introducing nano particle, shortwave phonon is consumingly scattered, therefore the total thermal conductivity of material can be by regulation
The characteristic size of nano-particle is realized.For example, introducing Si nano particles in SiGe alloys, its thermal conductivity can be made significantly to drop
It is low.And for low-dimension nano material and structure, because phonon is in constrained state, its transport mechanism is also considerably complicated, with nanometer
The shape of structure, size, surface and border are closely relevant.Currently, in theory, the steady test bench for near-equilibrium state shows
As that can be analyzed using linear irreversible thermodynamics, and transport coefficient is obtained by solving Boltzmann equation.So
And, in order to further investigate electric, the hot microcosmic transport mechanics of low-dimensional materials and nanostructured, we must experimentally, particularly
In nanoscale, its transport coefficient is measured, so as to accurately hold impurities of materials, defect and interface to transport property
Influence, and be compared with theoretical calculation.At present, also this target is realized without reliable laboratory facilities.Asked for this
Topic, the present invention wishes a kind of material nano yardstick thermoelectricity detecting system based on scanning probe of development, realizes to electricity, thermotransport
The Effective Regulation of journey, so as to deepen and promote people to electricity, the understanding of thermotransport microcosmic mechanism, tool has very important significance.
The content of the invention
The urgent premise of difficult, instrument demand is characterized based on current low dimensional physical property, the present invention proposes one kind
Thermoelectricity detecting system and thermoelectricity detection method, for the detection of material nano yardstick thermoelectricity capability.
A kind of thermoelectricity detecting system, the thermoelectricity capability for detecting material nano yardstick, the thermoelectricity detecting system includes
Scanning probe, sample stage, detection circuit and controller, the sample stage are used to carry sample, and the scanning probe is used to visit
Pin incentive mode contacts sample to heat sample and further in the probe excitation pattern examine the carrying out of sample
Survey, it is described detection circuit be used for electrically connect it is described scanning probe with detect it is described scanning probe under the probe excitation pattern
To export first detection signal, the controller is used to receive the first detection signal of the detection circuit output to change in electric
And the thermoelectricity capability of the sample is analyzed based on the first detection signal, the thermoelectricity detecting system also includes heater element,
The heater element is used to heat sample under non-probe excitation pattern, so that the scanning probe is further described
Non- probe excitation pattern is detected to the carrying out of sample, and then scanning probe described in the detection circuit detecting swashs in the non-probe
Encourage the change in electric under pattern and export the detection signal, the controller is used to receive the inspection of the detection circuit output
Survey signal and the thermoelectricity capability of sample is analyzed based on the detection signal.
In one embodiment, the heater element includes the heater strip in matrix and embedded described matrix.
In one embodiment, the tolerable temperature of the heater strip is more than or equal to 1000 degrees Celsius.
In one embodiment, the material of described matrix is boron nitride ceramics, and the material of the heater strip includes metal
The alloy of nickel, crome metal or metallic nickel and crome metal.
In one embodiment, the thermoelectricity detecting system also includes the first thermocouple and the second thermocouple, described the
One thermocouple is arranged at the top of described matrix and near one end of the sample, and second thermocouple is arranged at the scanning
It is used to contact the sample via the scanning probe on probe, first thermocouple is monitored jointly with second thermocouple
The temperature of the sample.
In one embodiment, the heater element is arranged on the sample stage, and the non-probe excitation pattern is
Sample stage incentive mode.
In one embodiment, the sample stage also includes water-cooled base, and the heater element is arranged at the water-cooled
On pedestal, the water-cooled base is used to keep the peripheral temperature of the sample stage within the scope of predetermined temperature.
In one embodiment, the material of the water-cooled base includes aluminium alloy.
In one embodiment, the sample stage also includes heat radiation cover, and the heat radiation cover is used to cover the sample
Sample platform it is at least part of, with keep the peripheral temperature of the sample stage within the scope of predetermined temperature and reduce heat diffusion.
In one embodiment, the detection circuit includes Wheatstone bridge and amplifier, the Wheatstone bridge bag
First resistor device, second resistance device and 3rd resistor device are included, the first resistor device is variable resistance, the first resistor device
One end connection it is described scanning probe one end, have between one end of the first resistor device and one end of the scanning probe
First node, the first node ground connection, the other end of the scanning probe connects one end of the second resistance device, described to sweep
The other end and one end of the second resistance device for retouching probe have Section Point, and the Section Point connects the amplifier
First input end, the other end of the first resistor device connects one end of the 3rd resistor device, the first resistor device it is another
One end has the 3rd node with one end of the 3rd resistor device, and the 3rd node connects the second input of the amplifier
End, the other end of the 3rd resistor device connects the other end of the second resistance device, the other end of the 3rd resistor device with
There is fourth node, the fourth node connects respectively with the output end of the amplifier between the other end of the second resistance device
Connect the controller.
In one embodiment, it is additionally operable to connect measurement apparatus between the Section Point and the 3rd node, for leading to
The voltage change crossed between the Section Point and the 3rd node knows the change in electric on the scanning probe and knows sample
The thermoelectricity capability of product.
In one embodiment, the controller includes sensor, signal processing module and high-speed, multi-path data acquisition
Module, the sensor is used to for the detection signal to be converted to conversion signal, and the signal processing module is used for described turn
Change signal and carry out denoising, amplification, filtering process and be changed into the high-speed, multi-path data acquisition module energy with by the conversion signal
The standard signal of enough identification, the high-speed, multi-path data acquisition module is used for standard signal record in computer system
In.
In one embodiment, the controller includes double frequency lock-in amplifier, and the double frequency lock-in amplifier is used for
The measurement of a frequency multiplication and frequency tripling is carried out to the detection signal and the detection signal of a frequency multiplication and the detection letter of frequency tripling is obtained
Number subsequent analysis are supplied, wherein the detection signal of the frequency tripling embodies the thermal conductivity of sample.
In one embodiment, the thermoelectricity detecting system also includes excitation module, and the controller also controls described
Excitation module applies the exchange electric excitation signal of a frequency multiplication so that the scanning under probe excitation pattern to the scanning probe
Probe is heated to sample.
A kind of thermoelectricity detection method, it comprises the following steps：
Under probe excitation pattern, scanning probe is heated and detected to sample, detects the telecommunications of the scanning probe
Number change obtains first detection signal, and the thermoelectricity capability of the sample is analyzed based on the first detection signal；And
Under non-probe excitation pattern, heater element is heated to sample, and the scanning probe is carried out to the sample
Detection, the change in electric for detecting the scanning probe obtains the second detection signal, and institute is analyzed based on second detection signal
State the thermoelectricity capability of sample.
In one embodiment, under probe excitation pattern with non-probe excitation pattern, by electrically connecting the scanning
The change in electric of the Wheatstone bridge detecting scanning probe of probe simultaneously obtains corresponding detection signal.
In one embodiment, the thermoelectricity detection method also includes：Described first and second detection signal is carried out
After conversion, denoising, amplification, filtering process and it is changed into standard signal, and by standard signal record in computer system
In step.
In one embodiment, the thermoelectricity detection method also includes：It is used for described using double frequency lock-in amplifier
First and second detection signal carry out the measurement of a frequency multiplication and frequency tripling and obtain first and second detection signal of a frequency multiplication with
The step of first and second detection signal of frequency tripling supplies subsequent analysis, wherein first and second detection signal of the frequency tripling
Embody the thermal conductivity of sample.
In one embodiment, the thermoelectricity detection method also includes：Under probe excitation pattern, visited to the scanning
Pin applies the exchange electric excitation signal of a frequency multiplication so that the step of scanning probe is heated to sample.
In one embodiment, include under non-probe excitation pattern, the step of heater element is heated to sample：
Heated to sample by the heater element being arranged on the sample stage for carrying sample.
Compared to prior art, the thermoelectricity detecting system for material nano yardstick of the invention and thermoelectricity detection method,
The two kinds of incentive modes heated using probe heating, sample stage, can be actually needed the suitable excitation of selection for user's foundation
Pattern, reaches the purpose of the thermoelectricity capability of accurate detection sample.Additionally, the apparatus structure of thermoelectricity detecting system of the present invention it is simple,
It is compatible strong, it is suitable to be combined with different commercial scanning probe systems, it is easy to spread and application a new technology.
In addition, the thermoelectricity detecting system for material nano yardstick of the invention need to only directly heat by direct detection material
Material nanoscale thermoelectricity capability.Material nano yardstick thermoelectricity capability not available for the existing scanning probe system of the technique extension
The physical property function of characterizing and evaluate, is deep development and the low dimensional material correlation nanometer chi of relevant Scanning probe technique
The research of degree physical property provides important sign new method.
Brief description of the drawings
In order to illustrate more clearly of embodiment of the present invention or technical scheme of the prior art, below will be to implementation method
Or the accompanying drawing to be used needed for description of the prior art is briefly described, it should be apparent that, drawings in the following description are only
It is some embodiments of the present invention, for those of ordinary skill in the art, on the premise of not paying creative work,
Other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of the thermoelectricity detecting system of a better embodiment of the invention, wherein the thermoelectricity is detected
System includes scanning probe and sample stage.
Fig. 2 is the structural representation of the sample stage of thermoelectricity detecting system shown in Fig. 1.
Fig. 3 is the structural representation of the thermoelectricity detection method of a better embodiment of the invention.
Fig. 4 is graph of relation of the heating voltage with the resistor of the scanning probe for putting on the scanning probe.
Fig. 5 is the temperature and resistor graph of relation of the scanning probe.
Fig. 6 is heat, the schematic diagram data of electric excitation probe sign material part heat conduction property under a kind of example.
Fig. 7 is the two-dimensional material Pyroelectric response figure under a kind of example.
Main element symbol description
Thermoelectricity detecting system 100
Scanning probe 110
Needle point 111
First linking arm 112
Second linking arm 113
Sample stage 120
Water-cooled base 121
Heater element 122
Heat radiation cover 123
Matrix 124
Heater strip 125
First thermocouple 126
Second thermocouple 127
Detection circuit 130
Controller 140
Wheatstone bridge 150
First resistor device 151
Second resistance device 152
3rd resistor device 153
First node 154
Section Point 155
3rd node 156
Fourth node 157
Lock-in amplifier 160
First input end 161
Second input 162
Output end 163
Sample 200
Step S1, S2
Following specific embodiment will further illustrate the present invention with reference to above-mentioned accompanying drawing.
Specific embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is carried out clearly
Chu, it is fully described by, it is clear that described implementation method is only a part of implementation method of the invention, rather than whole realities
Apply mode.Based on the implementation method in the present invention, those of ordinary skill in the art institute under the premise of creative work is not paid
The every other implementation method for obtaining, belongs to the scope of protection of the invention.
It should be noted that the term for using in embodiments of the present invention be only merely for description particular implementation
Purpose, and it is not intended to be limiting the present invention.Singulative used in embodiment of the present invention and appended claims
" one kind ", " described " and " being somebody's turn to do " is also intended to include most forms, unless context clearly shows that other implications.Should also manage
Solution, term "and/or" used herein refers to and can comprising one or more associated any or all of project listed
Can combination.In addition, term " first ", " second " in description and claims of this specification and above-mentioned accompanying drawing etc. be for
Different objects are distinguished, rather than for describing particular order.Additionally, term " comprising " and " having " and their any deformations,
It is intended to cover non-exclusive including.For example contain the process of series of steps or unit, method, system, product or set
It is standby to be not limited to the step of having listed or unit, but alternatively also include the step of not listing or unit, or alternatively
Also include for these processes, method, product or other intrinsic steps of equipment or unit.
Fig. 1 is referred to, Fig. 1 is the structural representation of the thermoelectricity detecting system 100 of a better embodiment of the invention.It is described
Thermoelectricity detecting system 100 is used to detect the thermoelectricity capability of material nano yardstick, and it includes scanning probe 110, sample stage 120, inspection
Slowdown monitoring circuit 130 and controller 140, the sample stage 120 are used to carry sample 200, and the scanning probe 110 is used to swash in probe
Pattern contact sample 200 is encouraged to be heated and further in probe excitation pattern the entering to sample 200 with to sample 200
Row detection, the detection circuit 130 is used to electrically connect the scanning probe 110 to detect the scanning probe 110 in the spy
The change in electric caused by the temperature change of sample 200 under pin incentive mode is to export first detection signal, the controller 140
The sample is analyzed for receiving the first detection signal of detection circuit 130 output and being based on the first detection signal
200 thermoelectricity capability.
Specifically, Fig. 2 is referred to, Fig. 2 is the structural representation of the sample stage 120 of thermoelectricity detecting system shown in Fig. 1 100.
In present embodiment, the sample stage 120 can include pedestal 121, heater element 122 and heat radiation cover 123.The pedestal
121 is water-cooled base, for carrying the heater element 122, and for keeping the peripheral temperature of the sample stage 120 predetermined
Within the temperature range of, the temperature of sample stage 120 is in (25 degrees Celsius) Zuo You of room temperature as described in keeping, and prevents to the sample
Other devices beyond platform 120 are damaged.It is appreciated that the predetermined temperature range can according to user the need for from
Row setting.Further, the pedestal 121 can include aluminum alloy materials, i.e., be processed into by aluminum alloy materials, and it can also
Storage tank including being arranged at the surface of pedestal 121, for housing the heater element 122.
The heater element 122 is arranged on the pedestal 121, for contacting the sample 200 and in non-probe excitation
Sample 200 is heated under pattern, so that the scanning probe 110 is further in the non-probe excitation pattern to sample
200 carrying out detect, and then the detection circuit 130 detects the scanning probe 110 under the non-probe excitation pattern
Change in electric simultaneously exports the detection signal, and the controller 140 is used to receive the detection letter of detection circuit 130 output
Number and based on the detection signal analyze sample 200 thermoelectricity capability.The heater element 122 includes matrix 124 and is embedded at
Heater strip 125 inside described matrix 124.Preferably, the tolerable temperature of the heater strip 125 is more than or equal to 1000 degrees Celsius.
The material of described matrix 124 is boron nitride ceramics but is not limited to boron nitride ceramics, and the material of the heater strip 125 includes metal
The alloy of nickel, crome metal or metallic nickel and crome metal but it is not limited to the conjunction of metallic nickel, crome metal or metallic nickel and crome metal
Gold.It is appreciated that in present embodiment, the heater element 122 is arranged on the sample stage 120, in change implementation method
In, the heater element 122 can also be independently disposed to outside the sample stage 120, however it is not limited to above-mentioned.
The heat radiation cover 123 is used to cover at least part of of the sample stage 120, to keep the sample stage 120
Peripheral temperature is within the scope of predetermined temperature and reduces the heat diffusion of the sample stage 120 so that the energy of the heater element 122
It is enough that the target temperature heated to the sample 200 is reached with minimum electric energy.Specifically, the heat radiation cover 123 can be set
In on the pedestal 121 of the sample stage, and cover the top in the heater element 122 with the sample 200.It is appreciated that
In one embodiment, the heat radiation cover 123 can include opening so that the scanning probe 110 can be opened via described
The mouth contact sample 200.
The thermoelectricity detecting system 100 can also include the first thermocouple 126 and the second thermocouple 127, first heat
Galvanic couple 126 is arranged at the top of described matrix 124 and near one end of the sample 200, and second thermocouple 127 is arranged on
Surface temperature on the scanning probe 110 for contacting the surface of the sample 200 to monitor the sample 200.Wherein, institute
It is the built-in thermocouple on the sample stage 120 to state the first thermocouple 126, and second thermocouple 127 is to be arranged on
State the external flexible thermocouple on scanning probe 110.Can be accurate with the second thermocouple 127 by first thermocouple 126
Position the temperature range on the surface of the sample 200.Specifically, can to position the sample 200 neighbouring for first thermocouple 126
The temperature of the side of the heater element 122, so as to know 122 pairs of heating-up temperatures of the sample 200 of the heater element.It is described
Scanning probe 110 is slided successively on the surface of the sample 200, and then second thermocouple 127 is in the scanning probe 110
The lower temperature that can successively monitor the surface of the sample 200 is driven, so as to be informed in the table of the sample 200 under excitation heated condition
The temperature of face diverse location, the thermoelectricity capability of the sample 200 is known eventually through analysis.
Wherein, 122 pairs of heating of the sample 200 of the heater element of the sample stage 120 can be added using resistor silk
Pyrogen reason, proportion of utilization-integral-derivative controller (PID) and pulse-width modulation method (PWM) carry out high-precision anti-to temperature
Feedback control.Particularly, by K-type thermocouple measurement, certainty of measurement is higher than 0.01 degree to the temperature of the sample stage 120.
The scanning probe 110 is thermal sensitivity resistor probe, when the two ends to the scanning thermal probe 110 apply heating
During voltage, the temperature of the scanning probe 110 can change with the change of voltage, and the resistor for scanning probe 110
Change also with the change of temperature.Specifically, the scanning probe 110 can include needle point 111, the first linking arm 112 with
Second linking arm 113, first linking arm 112 is connected and general alignment forming V-shape with second linking arm 113, described
The substantially vertical summit for being connected to the V-arrangement of needle point 111.Wherein described needle point 111 be used for contacted with the sample 200, with
The sample 200 carries out heat exchange.
The two ends (such as the first linking arm 112 and the second linking arm 113) of the scanning probe 110 are additionally operable to and the detection
Circuit 130 is electrically connected.Specifically, as under probe excitation pattern, the controller 140 can be controlled to the scanning probe 110
The heating voltage is applied in, and is heated up with the applying of heating voltage, the needle point 111 carries out heat with the sample 200
Exchange passes to the sample 200 with by thermal excitation.Further, due to the thermal excitation of the transmission of the needle point 111, the sample
200 surface temperature changes, and the sample 200 causes the scanning probe because there is heat exchange with the needle point 111
110 resistance changes, so as to cause the electric signal (such as voltage or electric current) on scanning probe 110 two ends to become
Change, the electric signal at scanning probe 110 two ends is detected and be further transmitted to the controller by the detection circuit 130
140。
Specifically, the heating to the scanning probe 110 can quickly be heated by Joule heating principle, and in fact
Existing microcell heat regulation and control, wherein for microcell local temperature, the characteristic that can be varied with temperature by the resistance of the scanning probe 110
Demarcated and real-time monitoring.When the temperature of needle point 111 of the scanning probe 110 occurs faint change, described sweeping can be caused
The resistance variations of probe 110 are retouched, so as to be detected by the detection circuit 130, and then the accurate measurement of micro-area temperature is realized.
It is appreciated that under the probe excitation pattern, the scanning probe 110 while as heating element heater (in other words
Thermal excitation element) and detecting element, and the measurement of horizontal electrical signal can also be entered to the sample 200 while heating, have
Body ground, in the course of the work, when heating voltage is applied to the scanning thermal probe 110, the scanning probe 110 can be with institute
State heating voltage to apply and heat up, thermal excitation is passed to by the sample 200 by the needle point 111, further detection is described
Change in electric on scanning probe 110, so as to realize the detection of the thermoelectricity capability of the sample 200.
Under non-probe excitation pattern (such as sample wants incentive mode), entered by 120 pairs of samples 200 of the sample stage
During row heating, the scanning probe 110 can be used only as detecting element, i.e., described sample stage 120 passes through heater element 122
Thermal excitation is carried out to the sample 200, the sample stage 120 directly has heat exchange with the sample 200, then by the sample
Product 200 cause the resistance of the scanning probe 110 to change with the scanning heat exchange of probe 110, cause change in electric,
So as to realize the sign of the thermoelectric material nanoscale thermoelectricity capability of the sample.
The detection circuit 130 includes Wheatstone bridge 150 and amplifier 160.The Wheatstone bridge 150 includes first
Resistor 151, second resistance device 152 and 3rd resistor device 153.The first resistor device 151 is variable resistance, described first
One end (such as the first linking arm 112) of one end connection scanning probe 110 of resistor 151, the first resistor device 151
There is first node 154, the first node 154 is grounded between one end of one end and the scanning probe 110, the scanning is visited
The other end (such as the second linking arm 113) of pin 110 connects one end of the second resistance device 152, the scanning probe 110 it is another
One end has Section Point 155 with one end of the second resistance device 152, and the Section Point 155 connects the amplifier 160
First input end 161, the other end of the first resistor device 151 connects one end of the 3rd resistor device 153, described first
The other end of resistor 151 has the 3rd node 156 with one end of the 3rd resistor device 153, and the 3rd node 156 is connected
Second input 162 of the amplifier 160, the other end of the 3rd resistor device 153 connects the second resistance device 152
There is fourth node between the other end of the other end, the other end of the 3rd resistor device 153 and the second resistance device 152
157, the fourth node 157 is connected the controller 140 respectively with the output end 163 of the amplifier 160.It is appreciated that
Can be connected with measurement apparatus between the node 156 of the Section Point 155 and the 3rd, for by the Section Point 155 with
Voltage change between 3rd node 160 knows the change in electric on the scanning probe 110 and knows the thermoelectricity of sample 200
Performance.
In present embodiment, the first resistor device 151 can be variable resistance, the second resistance device 152 and institute
State 3rd resistor device 153 and be fixed resistance, and the two resistance such as can be 1 kilo-ohm of fixed resistance with equal.
It is appreciated that the first resistor device 151, second resistance device 152,3rd resistor device 153, scanning probe 110 and
The sample 200 constitutes a Wheatstone bridge loop, when the surface temperature of the sample 200 changes, causes described
The resistance for scanning probe 110 changes, so as to the balance for causing the Wheatstone bridge loop changes, from the detection
Circuit 130 is exported to the detection signal of the controller 140 and changed, using the change between temperature and the detection signal
Relation, you can know the thermoelectricity capability result of the material nano yardstick of the sample 200.
It is appreciated that can be carried out using the heating voltage of the exchange of 1 ω (frequency multiplication chain) to the scanning probe 110
Exchange electric excitation, specifically can carry out quantitative measurement point to the thermal conductivity of the sample 200 by 3 ω (frequency tripling passage)
Analysis, specifically, the thermoelectricity detecting system 100 can also include excitation module, and the controller 140 can control the excitation
Module can apply the ac signal of 1 ω frequencies as heating voltage to the scanning probe 110.Meanwhile, implement in one kind
In mode, the controller 140 can also include double frequency lock-in amplifier, and the double frequency lock-in amplifier is to detection circuit 130
Output detection signal carries out 1 ω and the signal of 3 two frequencies of ω is measured, wherein the detection signal embodiment of 1 ω is measurement
Voltage, the detection signal of 3 ω embodies the local thermal conductivity of the material of sample 200.It will be appreciated, of course, that the double frequency lock phase
Amplifier can also be placed on outside the controller 140, detected between circuit 130 and the controller 140 as described in being connected to.
The controller 140 is used to be analyzed based on the detection signal thermoelectricity capability of the sample 200, and it can be with meter
Calculation machine system is connected, and is presented with result with carrying out auxiliary operation by the computer system, after analyzing the detection signal
Would know that the thermoelectricity capability image of the sample 200.Specifically, the controller can obtain local and global response
After time-domain signal, pre-processed by signal, demodulated, the signal processing flow such as FFT, obtain containing base
The local of the frequency contents such as ripple, second harmonic, triple-frequency harmonics and the space of global response spectrum and CF local acknowledgement
Distribution.
In present embodiment, the controller 140 can be AFM controller (AFM Controller), its
Sensor, signal processing module and high-speed, multi-path data acquisition module can be included, the sensor is used to believe the detection
Conversion signal number is converted to, the signal processing module is used to carry out the conversion signal denoising, amplifications, filtering process with general
The conversion signal is changed into the standard signal that the high-speed, multi-path data acquisition module is capable of identify that, the high-speed, multi-path data
Acquisition module is used for standard signal record in computer systems.Specifically, the main performance ginseng of the controller 140
Number can set as follows：Efficiently sampling rate：400MS/S；Average noise density：148dbm/HZ；Data output channel：4 passages.
It will be appreciated, of course, that the controller 140 can also be further used for the control hot detecting system 100 working
Input, output and switching of correlation timing and control different mode of required number control signal etc., and be not limited to
The thermoelectricity capability for analyzing the sample is stated, such as controls to apply heating voltage and control probe excitation to the scanning probe 110
Pattern and switching of non-probe excitation pattern etc., herein to the other functions of the controller 140 with regard to no longer repeating.In addition,
Specific module is also not necessarily limited to foregoing description with thermoelectricity capability analysis principle in the controller 140, such as can be using other analyses
Mode is based on the thermoelectricity capability that the detection signal knows the sample.
Refer to Fig. 3, the flow chart of Fig. 3 thermoelectricity detection methods of the present invention.The thermoelectricity detection method can use above-mentioned
Thermoelectricity detecting system 100.The thermoelectricity detection method includes step S1 and S2.
Step S1, under probe excitation pattern, scanning probe 110 is heated and detected to sample 200, is swept described in detecting
The change in electric for retouching probe 100 obtains first detection signal, and the heat of the sample 200 is analyzed based on the first detection signal
Electrical property.
Step S2, under non-probe excitation pattern, heater element 122 is heated to sample 200, the scanning probe
110 pairs of samples 200 detect that the change in electric for detecting the scanning probe 110 obtains the second detection signal, is based on
Second detection signal analyzes the thermoelectricity capability of the sample 200.
Specifically, in above-mentioned steps S1 and S2, can be by electrically connecting the Wheatstone bridge for scanning probe 110
The change in electric of the 150 detectings scanning probe 110 simultaneously obtains corresponding detection signal.
Include in step S2, the step of heated to sample by heater element：The sample of sample is carried by being arranged at
Heater element in sample platform is heated to sample.
The thermoelectricity detection method can also comprise the following steps：Described first and second detection signal is changed,
After denoising, amplification, filtering process and it is changed into standard signal, and the step by standard signal record in computer systems
Suddenly.Wherein above-mentioned steps can be by the sensor in the controller 140, signal processing module and high-speed, multi-path data acquisition module
Block etc. is completed.
The thermoelectricity detection method can also comprise the following steps：Be used for described first using double frequency lock-in amplifier and
Second detection signal carries out the measurement of a frequency multiplication and frequency tripling and obtains first and second detection signal and frequency tripling of a frequency multiplication
First and second detection signal supply subsequent analysis the step of, wherein the frequency tripling first and second detection signal embody sample
The thermal conductivity of product.During wherein double frequency lock-in amplifier may be located at the controller 140.
The thermoelectricity detection method can also comprise the following steps：Under probe excitation pattern, to the scanning probe 110
Apply the exchange electric excitation signal of a frequency multiplication so that the step of scanning probe 110 is heated to sample 200.
Refer to Fig. 4 and the graph of relation of resistance that Fig. 5, Fig. 4 are the heating voltage and the scanning probe 110.
Fig. 5 is the graph of relation of the temperature with the resistance of the scanning probe 110 of the scanning probe 110.From fig. 4, it can be seen that
With the increase of the heating voltage of the scanning probe 110, the resistance of the scanning probe 110 increases, with reference to Fig. 5, you can obtain
Know the relation between the temperature of the heating voltage and the scanning probe 110.
The thermoelectricity detecting system 100 that the present invention is developed is illustrated with reference to instantiation, it will be understood that below
The thermoelectricity capability detecting system developed of the invention is based primarily upon for the sample comprising CoSb3 and the Yb0.7Co4Sb12 of YbSb2
Product have carried out thermoelectricity detection imaging, and to further illustrate effect of the invention, and the scope of the present invention is not limited only to following realities
Example.
Example 1：Yb0.7Co4Sb12 is a kind of typical filling skutterudite thermoelectric material, and thermoelectric material is in the energy and environmental protection
Field has a wide range of applications.Miniaturization and Highgrade integration due to device, the hot physical property of its micro-structural and the work of device
Reliability is closely related with service life, the report of hot physical property detection microcosmic to this kind of material that so far there are no.Fig. 6 shows that it is swept
Retouch probe excitation and characterize material part heat conduction property.Wherein (a) figure is the scanning electron microscope (SEM) photograph of sample, analysis in display base material
Go out two kinds of different impurities, its chemical composition also by Accurate Calibration, however, ESEM cannot determine the heat biography of substrate and impurity
Lead property.C () figure is the atomic force scanning shape appearance figure of the same area, display material surface is smooth, and cannot be distinguished by impurity and base
Bottom.
Fig. 6 (b) figures are then the same area heat transfer distribution map that the device invented using us is obtained, and show thermal conductivity point
Cloth and Electronic Speculum microscopic structure corresponding relation completely, it is thus possible to determine the difference of substrate and the heat conduction property of impurity.(d) figure
Pattern and surface potential imaging when being scanned for the line of sample.
Example 2：Thermoelectricity sign has been carried out to two-dimensional material SnO2 using the present invention.Fig. 7 shows the pattern of two-dimensional material
Figure and thermoelectricity image.A () figure shows the complicated appearance structure of two-dimensional material.B () figure shows its corresponding thermoelectricity imaging
Figure.Confirm application function of the thermoelectricity detecting system 100 in material nano yardstick thermal imaging well.
Examples detailed above indicates the thermoelectricity detecting system 100 and is solving thermoelectric material nanoscale without direct measurement
Temperature change and can directly characterize the thermal conductivity distribution of material and thermoelectricity is imaged isoparametric important technology problem.The thermoelectricity
Detecting system 100 realize thermoelectric material nanoscale needed for multiple-frequency signal generation and collection, and synchro measure material
Thermal conductivity, extends the thermoelectric material nanoscale evaluation of physical property work(not available for existing commercial scanning probe microscopy
Can, for the further investigation of thermoelectric material nanoscale performance provides important instrument and characterizing method.
In sum, compared to prior art, the thermoelectricity of thermoelectricity detecting system 100 for material nano yardstick of the invention
Detection method, the two kinds of incentive modes heated using probe heating, sample stage can be closed for user according to selection is actually needed
Suitable incentive mode, reaches the purpose of the thermoelectricity capability of accurate detection sample.Additionally, the dress of thermoelectricity detecting system 100 of the present invention
Put simple structure, compatibility strong, it is suitable to be combined with different commercial scanning probe systems, it is easy to spread and application a new skill
Art.
In addition, 100 need of thermoelectricity detecting system for material nano yardstick of the invention are directly examined by directly heating
Measure and monitor the growth of standing timber and expect nanoscale thermoelectricity capability.Material nano yardstick thermoelectricity not available for the existing scanning probe system of the technique extension
Performance characterization and the physical property function of evaluating, are that the deep development of relevant Scanning probe technique and low dimensional material correlation are received
The research of metrical scale physical property provides important sign new method..
The description to preferred embodiments is above provided, so that scientific research technical staff in the art can be used and utilize this hair
It is bright.Various parameters modification to these examples is simply and easily to its research work.Therefore made according to the claims in the present invention
Equivalent variations, still belong to the scope that is covered of the present invention.
Claims (20)
1. a kind of thermoelectricity detecting system, it is characterised in that：The thermoelectricity detecting system includes scanning probe, sample stage, detection electricity
Road and controller, the sample stage are used to carry sample, and the scanning probe is used to contact sample with right in probe excitation pattern
Sample is heated and further in the probe excitation pattern the carrying out of sample detected, the detection circuit is used to be electrically connected
The scanning probe is connect to detect change in electric of the scanning probe under the probe excitation pattern to export the first inspection
Signal is surveyed, the controller is used to receive the first detection signal of the detection circuit output and based on the first detection signal
The thermoelectricity capability of the sample is analyzed, the thermoelectricity detecting system also includes heater element, and the heater element is used in non-spy
Sample is heated under pin incentive mode, so that the scanning probe is further in the non-probe excitation pattern to sample
Detected, and then change in electric of the scanning probe under the non-probe excitation pattern described in the detection circuit detecting is simultaneously
The detection signal is exported, the controller is used to receive the detection signal of the detection circuit output and based on the detection letter
Number analysis sample thermoelectricity capability.
2. thermoelectricity detecting system as claimed in claim 1, it is characterised in that：The heater element includes that matrix and insertion are described
Heater strip in matrix.
3. thermoelectricity detecting system as claimed in claim 2, it is characterised in that：The tolerable temperature of the heater strip is more than or equal to
1000 degrees Celsius.
4. thermoelectricity detecting system as claimed in claim 2, it is characterised in that：The material of described matrix is boron nitride ceramics, institute
Stating the material of heater strip includes the alloy of metallic nickel, crome metal or metallic nickel and crome metal.
5. thermoelectricity detecting system as claimed in claim 2, it is characterised in that：The thermoelectricity detecting system also includes the first thermoelectricity
It is even that first thermocouple is arranged at the top of described matrix and near one end of the sample with the second thermocouple, and described the
Two thermocouples are arranged on the scanning probe to be used to contact the sample via the scanning probe, first thermocouple with
Second thermocouple monitors the temperature of the sample jointly.
6. thermoelectricity detecting system as claimed in claim 1, it is characterised in that：The heater element is arranged at the sample stage
On, the non-probe excitation pattern is sample stage incentive mode.
7. thermoelectricity detecting system as claimed in claim 6, it is characterised in that：The sample stage also includes water-cooled base, described
Heater element is arranged in the water-cooled base, and the water-cooled base is used to keep the peripheral temperature of the sample stage predetermined
In temperature range.
8. thermoelectricity detecting system as claimed in claim 7, it is characterised in that：The material of the water-cooled base includes aluminium alloy.
9. thermoelectricity detecting system as claimed in claim 6, it is characterised in that：The sample stage also includes heat radiation cover, described
Heat radiation cover is used to cover at least part of of the sample stage, to keep the peripheral temperature of the sample stage in predetermined temperature model
Enclose interior and reduction heat diffusion.
10. thermoelectricity detecting system as claimed in claim 1, it is characterised in that：It is described detection circuit include Wheatstone bridge with
Amplifier, the Wheatstone bridge includes first resistor device, second resistance device and 3rd resistor device, and the first resistor device is can
Variohm, one end of one end connection scanning probe of the first resistor device, one end of the first resistor device and institute
Stating between one end of scanning probe has first node, first node ground connection, the other end connection institute of the scanning probe
One end of second resistance device is stated, the other end of the scanning probe has Section Point with one end of the second resistance device, institute
The first input end that Section Point connects the amplifier is stated, the other end of the first resistor device connects the 3rd resistor device
One end, one end of the other end of the first resistor device and the 3rd resistor device has the 3rd node, the 3rd node
The second input of the amplifier is connected, the other end of the 3rd resistor device connects the other end of the second resistance device,
Between the other end of the other end of the 3rd resistor device and the second resistance device have fourth node, the fourth node with
The output end of the amplifier connects the controller respectively.
11. thermoelectricity detecting systems as claimed in claim 10, it is characterised in that：Between the Section Point and the 3rd node also
For connecting measurement apparatus, for knowing the scanning probe by the voltage change between the Section Point and the 3rd node
On change in electric and know the thermoelectricity capability of sample.
12. thermoelectricity detecting systems as claimed in claim 1, it is characterised in that：The controller includes sensor, signal transacting
Module and high-speed, multi-path data acquisition module, the sensor are used to for the detection signal to be converted to conversion signal, the letter
Number processing module is used to carrying out the conversion signal denoising, amplifications, filtering process with described in the conversion signal is changed into
The standard signal that high-speed, multi-path data acquisition module is capable of identify that, the high-speed, multi-path data acquisition module is used for the standard
Signal record is in computer systems.
13. thermoelectricity detecting systems as claimed in claim 1, it is characterised in that：The controller includes double frequency lock-in amplifier,
The double frequency lock-in amplifier obtains the inspection of a frequency multiplication for carrying out the measurement of a frequency multiplication and frequency tripling to the detection signal
Survey signal and supply subsequent analysis with the detection signal of frequency tripling, wherein the detection signal of the frequency tripling embodies the thermal conductivity of sample.
14. thermoelectricity detecting systems as claimed in claim 1, it is characterised in that：The thermoelectricity detecting system also includes excited modes
Block, the controller also controls the excitation module to apply a frequency multiplication to the scanning probe under the probe excitation pattern
Exchange electric excitation signal is so that the scanning probe is heated to sample.
A kind of 15. thermoelectricity detection methods, it comprises the following steps：
Under probe excitation pattern, scanning probe is heated and detected to sample, and the electric signal for detecting the scanning probe becomes
Change and obtain first detection signal, the thermoelectricity capability of the sample is analyzed based on the first detection signal；And
Under non-probe excitation pattern, heater element is heated to sample, and the scanning probe is detected to the sample,
The change in electric of the detecting scanning probe obtains the second detection signal, and the sample is analyzed based on second detection signal
Thermoelectricity capability.
16. thermoelectricity detection methods as claimed in claim 15, it is characterised in that：In probe excitation pattern and non-probe excitation mould
Under formula, the change in electric of the scanning probe is detected by the Wheatstone bridge for electrically connecting the scanning probe and correspondence is obtained
Detection signal.
17. thermoelectricity detection methods as claimed in claim 15, it is characterised in that：The thermoelectricity detection method also includes：To institute
First and second detection signal is stated to be changed, denoising, amplification, after filtering process and be changed into standard signal, and will be described
The step of standard signal is recorded in computer systems.
18. thermoelectricity detection methods as claimed in claim 15, it is characterised in that：The thermoelectricity detection method also includes：Utilize
Double frequency lock-in amplifier is used to carry out the measurement of a frequency multiplication and frequency tripling to described first and second detection signal and obtain one times
The step of first and second detection signal of frequency supplies subsequent analysis with first and second detection signal of frequency tripling, wherein described three
First and second detection signal of frequency multiplication embodies the thermal conductivity of sample.
19. thermoelectricity detection methods as claimed in claim 15, it is characterised in that：The thermoelectricity detection method also includes：Visiting
Under pin incentive mode, the exchange electric excitation signal of a frequency multiplication is applied so that the scanning probe enters to sample to the scanning probe
The step of row heating.
20. thermoelectricity detection methods as claimed in claim 15, it is characterised in that：Under non-probe excitation pattern, heater element
The step of being heated to sample includes：Added to sample by the heater element being arranged on the sample stage for carrying sample
Heat.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111948250A (en) * | 2020-08-13 | 2020-11-17 | 上海大学 | Variable temperature measuring device for high-flux thermoelectric material |
| CN112857456A (en) * | 2021-02-04 | 2021-05-28 | 上海大学 | Device and method for integrally representing multiple parameters of block material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11183414A (en) * | 1997-12-19 | 1999-07-09 | Nikon Corp | Scanning heat transfer distribution measuring device |
| CN1344952A (en) * | 2000-09-29 | 2002-04-17 | 中国科学院低温技术实验中心 | Heatable sample platform for scanning probe microscope |
| CN102692427A (en) * | 2012-06-20 | 2012-09-26 | 中国科学院上海硅酸盐研究所 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
| CN105510636A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Nano-magnetism-electricity-heat multi-parameter coupling in situ detection system and detection method thereof |
| CN206684185U (en) * | 2017-01-18 | 2017-11-28 | 中国科学院深圳先进技术研究院 | Thermoelectricity detecting system |
-
2017
- 2017-01-18 CN CN201710034720.3A patent/CN106771372A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11183414A (en) * | 1997-12-19 | 1999-07-09 | Nikon Corp | Scanning heat transfer distribution measuring device |
| CN1344952A (en) * | 2000-09-29 | 2002-04-17 | 中国科学院低温技术实验中心 | Heatable sample platform for scanning probe microscope |
| CN102692427A (en) * | 2012-06-20 | 2012-09-26 | 中国科学院上海硅酸盐研究所 | Nano-thermoelectric multi-parameter in-situ quantitative characterization device based on atomic force microscope |
| CN105510636A (en) * | 2014-09-24 | 2016-04-20 | 中国科学院宁波材料技术与工程研究所 | Nano-magnetism-electricity-heat multi-parameter coupling in situ detection system and detection method thereof |
| CN206684185U (en) * | 2017-01-18 | 2017-11-28 | 中国科学院深圳先进技术研究院 | Thermoelectricity detecting system |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112857456A (en) * | 2021-02-04 | 2021-05-28 | 上海大学 | Device and method for integrally representing multiple parameters of block material |
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