CN106770445A - Thermoelectricity detecting system and thermoelectricity detection method - Google Patents
Thermoelectricity detecting system and thermoelectricity detection method Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 146
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- 239000000523 sample Substances 0.000 claims abstract description 296
- 238000005086 pumping Methods 0.000 claims abstract description 65
- 230000008859 change Effects 0.000 claims abstract description 33
- 238000004093 laser heating Methods 0.000 claims abstract description 7
- 230000005284 excitation Effects 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 24
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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 laser pumping module, scanning probe, sample stage, detection circuit and controller, the sample stage is used to carry sample, the laser pumping module is used to send LASER HEATING sample under laser pumping pattern, the scanning probe is used to detect sample, the detection circuit is used to detect the change in electric of the scanning probe to export detection signal, the controller is used for the thermoelectricity capability that output and input to signal etc. was controlled and received the detection signal of the detection circuit output 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
Laser pumping module, scanning probe, sample stage, detection circuit and controller, the sample stage are used to carry sample, the laser
Excitation module is used to send LASER HEATING sample under laser pumping pattern, and the scanning probe is used to examine the carrying out of sample
Survey, the detection circuit is used to detect the change in electric of the scanning probe to export detection signal, and the controller is used for
Receive the detection signal of the detection circuit output and the thermoelectricity capability of the sample is analyzed based on the detection signal.
In one embodiment, the laser pumping module includes the regulation of laser generator, laser detector and laser
Device, the laser generator is used to send LASER HEATING sample, and the laser detector is used to detect the laser generator hair
The laser that goes out simultaneously exports detection signal, and the laser modulation device is used for the detection signal based on laser detector output and sends
Control signal is to the laser generator adjusting the laser that the laser generator sends.
In one embodiment, the size of the laser generator is 100*40*40mm.
In one embodiment, the laser generator includes light source and optics episcotister, and the optics episcotister is used
In being switched or frequency modulation(PFM) to the light source.
In one embodiment, the controller includes lock-in amplifier, and the lock-in amplifier is used for the inspection
The detection signal of slowdown monitoring circuit output is acquired, and coordinates the switch of the optics episcotister to be carried out to sample based on time scale
Transient state characterize.
In one embodiment, the lock-in amplifier is double frequency lock-in amplifier, and the double frequency lock-in amplifier is used
The detection signal of a frequency multiplication and the detection of frequency tripling are obtained in the measurement of a frequency multiplication and frequency tripling is carried out to the detection signal
Signal supplies subsequent analysis, wherein the detection signal of the frequency tripling embodies the thermal conductivity of sample.
In one embodiment, the controller is also adopted including sensor, signal processing module and high-speed, multi-path data
Collection module, the sensor is used to for the detection signal that the lock-in amplifier is exported to be converted to conversion signal, at the signal
Reason module is used to carrying out the conversion signal denoising, amplification, filtering process being changed into the high speed with by the conversion signal
The standard signal that Multichannel 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.
In one embodiment, side of the laser pumping module from sample away from the sample stage sends laser pair
Sample is heated, the power of the laser pumping module in the range of 0.1mW to 10mW, the hair of the laser pumping module
Raw frequency within the 5kHz in the range of, the optical maser wavelength is 360nm-800nm.
In one embodiment, side of the laser pumping module from sample stage away from the sample sends laser,
The laser is heated to sample via being irradiated on the sample through the through hole of the sample stage, the laser pumping mould
The power of block is 250mW, the occurrence frequency of the laser pumping module within the 5kHz in the range of, the optical maser wavelength is
360nm-800nm。。
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 scanning probe is additionally operable to that sample is heated and examined under probe excitation pattern
Survey, the change in electric that the detection circuit is used to detect the scanning probe obtains detection signal, and the controller is based on institute
The detection signal for stating detection circuit output analyzes the thermoelectricity capability of sample.
In one embodiment, the thermoelectricity detecting system also includes probe excitation module, and the controller controls institute
State probe excitation module and apply the exchange electric excitation signal of a frequency multiplication so that institute to the scanning probe under probe excitation pattern
Scanning probe is stated to heat sample.
In one embodiment, the thermoelectricity detecting system also includes the first thermocouple and the second thermocouple, described the
One thermocouple is arranged on the sample stage and near one end of the sample, and second thermocouple is arranged at the scanning and visits
It is used to contact the sample via the scanning probe on pin, first thermocouple monitors institute jointly with second thermocouple
State the temperature of sample.
A kind of thermoelectricity detection method, it comprises the following steps:
Laser is provided to heat sample;
Sample is detected using probe is scanned;
The change in electric of the detecting scanning probe obtains detection signal;And
The thermoelectricity capability of the sample is analyzed based on the detection signal.
In one embodiment, the thermoelectricity detection method is further comprising the steps of:Detect the laser and according to inspection
Result is surveyed to be adjusted the laser being applied on sample.
In one embodiment, the thermoelectricity detection method is further comprising the steps of:Optics episcotister is provided for right
The light source for sending the laser is switched or frequency modulation(PFM).
In one embodiment, it is described the sample is analyzed based on the detection signal thermoelectricity capability the step of also wrap
Include:There is provided lock-in amplifier to be acquired the detection signal of the detection circuit output, and coordinate the optics episcotister
Switch the step of transient state based on time scale is carried out to sample characterizing.
In one embodiment, it is described the sample is analyzed based on the detection signal thermoelectricity capability the step of also wrap
Include:Using double frequency lock-in amplifier a frequency multiplication is obtained for carrying out the measurement of a frequency multiplication and frequency tripling to the detection signal
Detection signal supplies subsequent analysis with the detection signal of frequency tripling, wherein the detection signal of the frequency tripling embodies the thermal conductivity of sample
Rate.
In one embodiment, it is described the sample is analyzed based on the detection signal thermoelectricity capability the step of also wrap
Include:The detection signal of lock-in amplifier collection is changed, denoising, amplification, after filtering process and is changed into standard letter
Number, and by the standard signal record in computer systems the step of.
In one embodiment, there is provided the step of laser is heated to sample includes:In sample away from the sample
The side of platform sets laser pumping module, and the laser pumping module sends laser and sample is heated, wherein the laser
The power of module is encouraged in the range of 0.1mW to 10mW, the model of the occurrence frequency of the laser pumping module within 5kHz
In enclosing, the optical maser wavelength is 360nm-800nm.
In one embodiment, there is provided the step of laser is heated to sample includes:In sample stage away from the sample
The side of product sets laser pumping module, and the laser pumping module sends laser, and the laser is via through the sample stage
Through hole be irradiated on sample sample heated, the power of the laser pumping module is 250mW, the laser pumping mould
The occurrence frequency of block within the 5kHz in the range of, the optical maser wavelength is 360nm-800nm.
In one embodiment, the step of change in electric of the detecting scanning probe obtains detection signal is wrapped
Include:The change in electric of the scanning probe is detected by the Wheatstone bridge for electrically connecting the scanning probe and obtains corresponding
The step of detection signal.
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.
Compared to prior art, the excitation of the thermoelectricity detecting system LASER HEATING for material nano yardstick of the invention
Pattern, direct detection material nano yardstick thermoelectricity capability by need to only directly heating.The existing scanning probe system of the technique extension
The not available material nano yardstick thermoelectric property characterization of system and the physical property function of evaluating, are the depth of relevant Scanning probe technique
Enter development and the correlation nanoscale physical property research of low dimensional material provides important sign new method.Additionally, of the invention
The apparatus structure of thermoelectricity detecting system is simple, compatibility is strong, suitable to be combined with different commercial scanning probe systems, is one and is easy to
The new technology of promotion and application.
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.
Fig. 2 is a kind of structural representation of the thermoelectricity detecting system for changing implementation method of thermoelectricity detecting system shown in Fig. 1.
Fig. 3 is the structural representation of the laser pumping module of thermoelectricity detecting system shown in Fig. 1.
Fig. 4 is the flow chart of thermoelectricity detection method of the present invention.
Fig. 5 is applied to the heating voltage of scanning probe shown in Fig. 1 and the graph of relation of the resistor of scanning probe.
Fig. 6 is the temperature and resistor graph of relation of scanning probe shown in Fig. 1.
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
Through hole 121
First thermocouple 126
Second thermocouple 118
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
Amplifier 160
First input end 161
Second input 162
Output end 163
Laser pumping module 180
Laser generator 181
Laser detector 182
Laser modulation device 183
Light source 184
Optics episcotister 185
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, controller 140 and laser pumping module 180.The sample stage 120 is used to carry sample 200.The scanning is visited
Pin 110 is used to be heated and further in the probe excitation with to sample 200 in probe excitation pattern contact sample 200
Pattern detects that the detection circuit 130 is used to electrically connect the scanning probe 110 to detect described sweeping to the carrying out of sample 200
Change in electric that probe 110 causes by the temperature change of sample 200 under the probe excitation pattern is retouched to export the first detection
Signal, the controller 140 is used to receive the first detection signal of detection circuit 130 output and based on the described first detection
The thermoelectricity capability of sample 200 described in signal analysis.The laser pumping module 180 is used to send laser under laser pumping pattern
Heating sample 200, the carrying out that the scanning probe 110 is used for sample 200 under laser pumping pattern detects that the detection is electric
Road 130 is used to electrically connect the scanning probe 110 to detect the change in electric of the scanning probe 110 to export the second detection
Signal, the controller 140 is used to receive the second detection signal of detection circuit 130 output and based on the described second detection
The thermoelectricity capability of sample 200 described in signal analysis.
Specifically, as shown in figure 1, the laser pumping module 180 can be arranged on the sample 200 away from the sample
The side of platform 120, is added so as to send laser away from the side of the sample stage 120 from the sample 200 to sample 200
Heat.Preferably, the power of the laser pumping module 180 is in the range of 0.1mW to 10mW, the laser pumping module 180
Occurrence frequency within the 5kHz in the range of, the optical maser wavelength that the laser pumping module 180 sends is 360nm-800nm.
As shown in Fig. 2 in a kind of change implementation method of Fig. 1, the laser pumping module 180 can be arranged on described
Sample stage 120 away from the sample 200 side, so as to sending sharp away from the side of the sample 200 from the sample stage 120
Light, the laser is heated via the through hole 121 through the sample stage 120 to sample 200.Now, the laser pumping
The power of module is 250mW, the occurrence frequency of the laser pumping module within the 5kHz in the range of, the optical maser wavelength is
360nm-800nm。
Fig. 3 is referred to, Fig. 3 is the structural representation of the laser pumping module 180.The laser pumping module 180 is wrapped
Laser generator 181, laser detector 182 and laser modulation device 183 are included, the laser generator 181 adds for sending laser
Hot sample, the laser detector 182 is used to detecting the laser that the laser generator 181 sends and exports detection signal, institute
State laser modulation device 183 for based on the laser detector 182 export detection signal send control signal to the laser
Generator 181 is adjusting the laser that the laser generator 181 sends.Preferably, the size of the laser generator 181 is
100mm*40mm*40mm.The laser generator 181 can include light source 184 and optics episcotister 185, and the optics cuts light
Device 185 is used to switch the light source 184 or frequency modulation(PFM).
The controller 140 can include lock-in amplifier, and the lock-in amplifier is used for defeated to the detection circuit 130
The detection signal for going out is acquired, and coordinates the switch of the optics episcotister 185 to be carried out to sample 200 based on time scale
Transient state is characterized.It is appreciated that the controller 140 can also control the Laser emission sequential of the laser pumping module 180 with
And control to adjust the laser of the laser pumping module 180.
Further, the scanning probe 110 can be carried out using the heating voltage of the exchange of 1 ω (frequency multiplication chain)
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 140 can ring the local and overall situation is obtained
After the time-domain signal answered, pre-processed by signal, demodulated, the signal processing flow such as FFT, contained
There are local and global response spectrum and the CF local acknowledgement of the frequency contents such as fundamental wave, second harmonic, triple-frequency harmonics
Spatial 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 some required signals etc., and it is not limited to above-mentioned point
The thermoelectricity capability of the sample is analysed, such as controls to apply heating voltage and control probe excitation pattern to the scanning probe 110
With the switching of non-probe excitation pattern etc., herein to the other functions of the controller 140 with regard to no longer repeating.In addition, described
Specific module is also not necessarily limited to foregoing description with thermoelectricity capability analysis principle in controller 140, can such as use other analysis modes
The thermoelectricity capability of the sample is known based on the detection signal.
Further, in present embodiment, the thermoelectricity detecting system 100 can also include the first thermocouple 126 with
Second thermocouple 118, first thermocouple 126 is arranged at the top of the sample stage 120 and near the one of the sample 200
End, second thermocouple 118 is arranged on the scanning probe 110 for contacting the surface of the sample 200 to monitor
State the surface temperature of sample 200.Wherein, first thermocouple 126 is the built-in thermocouple on the sample stage 120,
Second thermocouple 118 is the external flexible thermocouple being arranged on the scanning probe 110.By first thermocouple
126 and second thermocouple 118 can be accurately positioned the temperature range on the surface of the sample 200.Specifically, first thermocouple
126 can position temperature of the sample 200 adjacent to the side of the heater element 122, so as to know the heater element 122 pairs
The heating-up temperature of the sample 200.The scanning probe 110 is slided successively on the surface of the sample 200, and then second heat
Galvanic couple 118 can successively monitor the temperature on the surface of the sample 200 under the drive of the scanning probe 110, so as to be informed in
The temperature of the surface diverse location of the sample 200, the thermoelectricity of the sample 200 is known eventually through analysis under excitation heated condition
Performance.
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, and detection signal is provided with to the detection circuit 130.Specifically, such as under probe excitation pattern, the control
Device processed 140 can control to be applied in the heating voltage to the scanning probe 110, and be risen with the applying of heating voltage
Temperature, the needle point 111 carries out heat exchange and passes to the sample 200 with by thermal excitation with the sample 200.Further, by
In the thermal excitation of the transmission of the needle point 111, the surface temperature of the sample 200 changes, the sample 200 because with the pin
There is heat exchange and cause that the resistor of the scanning probe 110 changes in point 111, so as to cause the scanning probe 110
Electric signal (such as voltage or electric current) on two ends changes, and the electric signal at scanning probe 110 two ends is by the detection electricity
Road 130 detects and is further transmitted to the controller 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 spy that can be varied with temperature by the resistor of the scanning probe 110
Property is demarcated and real-time monitoring.When the temperature of needle point 111 of the scanning probe 110 occurs faint change, can cause described
The resistor change of probe 110 is scanned, so as to be detected by the detection circuit 130, and then the accurate survey of micro-area temperature is realized
Amount.
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 that the thermoelectric material physical property of the sample 200 is detected.
Under non-probe excitation pattern (such as laser pumping pattern), by 180 pairs of samples of the laser pumping module
200 when being heated, and the scanning probe 110 can be used only as detecting element, i.e., described 180 pairs of institutes of laser pumping module
Stating sample 200 carries out thermal excitation, then causes the scanning to be visited with the scanning heat exchange of probe 110 by the sample 200
The resistor of pin 110 changes, and causes change in electric, so as to realize the thermoelectric material nanoscale pyroelectricity of the sample
The sign of energy.
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.
Refer to Fig. 4, the flow chart of Fig. 4 thermoelectricity detection methods of the present invention.The thermoelectricity detection method can use above-mentioned
Thermoelectricity detecting system 400.The thermoelectricity detection method includes step S1, S2, S3, S4.
Step S1:Laser is provided to heat sample 200.
Step S2:Sample 200 is detected using probe 110 is scanned.
Step S3:The change in electric of the detecting scanning probe 110 obtains first detection signal;And
Step S4:The thermoelectricity capability of the sample 200 is analyzed based on the first detection signal.
Further, the thermoelectricity detection method also includes:Under probe excitation pattern, in the control of controller 140
Under, apply the exchange electric excitation signal of a frequency multiplication so that the scanning probe 110 enters to sample 200 to the scanning probe 110
The step of row heating.
Specifically, in one embodiment, step S1 includes:Side from sample 200 away from the sample stage 126 sets
The step of laser pumping module 180 put sends laser and is heated to sample 200, wherein the laser pumping module 180
Power in the range of 0.1mW to 10mW, the occurrence frequency of the laser pumping module 180 within the 5kHz in the range of, institute
Optical maser wavelength is stated for 360nm-800nm.
In one embodiment, step S1 includes:From sample stage away from the side of the sample laser pumping module
The step of sending laser and heated to sample via the sample stage, the power of the laser pumping module is 250mW, institute
State the occurrence frequency of laser pumping module within the 5kHz in the range of, the optical maser wavelength is 360nm-800nm.
Further, step S1 also includes:The laser is detected using the laser pumping module 180 and tied according to detection
The step of fruit is adjusted to the laser being applied on sample 200.Further, step S1 also includes:Optics is provided and cuts light
Device 185 is used to switching the light source 184 that sends the laser or the step of frequency modulation(PFM).
In step S3, detected by the Wheatstone bridge 150 and amplifier 160 that electrically connect the scanning probe 110 described
Scan the change in electric of probe and obtain corresponding detection signal.
Step S4 can include:Lock-in amplifier is provided to be acquired the detection signal of detection circuit 130 output,
And the step of coordinate the switch of the optics episcotister 185 transient state based on time scale is carried out to sample 200 to characterize.More enter one
Step ground, the lock-in amplifier can be double frequency lock-in amplifier, and step S4 also includes, it is right to be used for using double frequency lock-in amplifier
Described first and second detection signal carries out the measurement of a frequency multiplication and frequency tripling and obtains first and second detection letter of a frequency multiplication
The step of number supplying subsequent analysis with first and second detection signal of frequency tripling, wherein first and second detection of the frequency tripling
Signal embodies the thermal conductivity of sample.
Further, step S4 also includes:To the lock-in amplifier collection detection signal changed, denoising,
Amplify, after filtering process and be changed into standard signal, and by standard signal record in computer systems the step of.
Refer to Fig. 5 and the graph of relation of resistance that Fig. 6, Fig. 5 are the heating voltage and the scanning probe 110.
Fig. 6 is the graph of relation of the temperature with the resistance of the scanning probe 110 of the scanning probe 110.From fig. 5, 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. 6, you can obtain
Know the relation between the temperature of the heating voltage and the scanning probe 110.
Compared to prior art, the thermoelectricity detecting system for material nano yardstick of the invention is swashed using LASER HEATING
Pattern is encouraged, direct detection material nano yardstick thermoelectricity capability by need to only directly heating.The existing scanning probe of the technique extension
Material nano yardstick thermoelectric property characterization and the physical property function of evaluating not available for system, are relevant Scanning probe technique
Deeply development and the correlation nanoscale physical property research of low dimensional material provides important sign new method.Additionally, this hair
The apparatus structure of bright thermoelectricity detecting system is simple, compatibility is strong, suitable to be combined with different commercial scanning probe systems, is one easy
In the new technology of promotion and application.
Further, the thermoelectricity detection method of thermoelectricity detecting system 100 for material nano yardstick of the invention, uses
Probe heating, two kinds of incentive modes of laser pumping heating, can be actually needed the suitable excited modes of selection for user's foundation
Formula, reaches the purpose of the thermoelectricity capability of accurate detection sample.
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 (24)
1. a kind of thermoelectricity detecting system, it is characterised in that the thermoelectricity detecting system include laser pumping module, scanning probe,
Sample stage, detection circuit and controller, the sample stage are used to carry sample, and the laser pumping module is used in laser pumping
LASER HEATING sample is sent under pattern, the scanning probe is used to detect sample, the detection circuit is used to detect institute
The change in electric of scanning probe is stated to export detection signal, the controller is used to receive the detection of the detection circuit output
Signal and the thermoelectricity capability based on the detection signal analysis sample.
2. thermoelectricity detecting system as claimed in claim 1, it is characterised in that the laser pumping module includes that laser occurs
Device, laser detector and laser modulation device, the laser generator are used to send LASER HEATING sample, and the laser detector is used
In detecting laser that the laser generator sends and exporting detection signal, the laser modulation device is used to be examined based on the laser
The detection signal for surveying device output sends control signal to the laser generator to adjust the laser that the laser generator sends.
3. thermoelectricity detecting system as claimed in claim 2, it is characterised in that the size of the laser generator is 100*40*
40mm。
4. thermoelectricity detecting system as claimed in claim 2, it is characterised in that the laser generator includes that light source cuts with optics
Light device, the optics episcotister is used to switch the light source or frequency modulation(PFM).
5. thermoelectricity detecting system as claimed in claim 4, it is characterised in that the controller includes lock-in amplifier, described
Lock-in amplifier is used to be acquired the detection signal of the detection circuit output, and coordinates the switch of the optics episcotister
The transient state based on time scale is carried out to sample to characterize.
6. thermoelectricity detecting system as claimed in claim 5, it is characterised in that the lock-in amplifier is that double frequency lock mutually amplifies
Device, the double frequency lock-in amplifier is used to carry out the measurement of a frequency multiplication and frequency tripling to the detection signal and obtain a frequency multiplication
Detection signal supplies subsequent analysis with the detection signal of frequency tripling, wherein the detection signal of the frequency tripling embodies the thermal conductivity of sample
Rate.
7. thermoelectricity detecting system as claimed in claim 5, it is characterised in that the controller also includes at sensor, signal
Reason module and high-speed, multi-path data acquisition module, the sensor are used for the detection signal conversion for exporting the lock-in amplifier
It is conversion signal, the signal processing module is used to carry out the conversion signal denoising, amplification, filtering process that described will turn
Change signal and be 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
Block is used for standard signal record in computer systems.
8. thermoelectricity detecting system as claimed in claim 1, it is characterised in that the laser pumping module is from sample away from described
The side of sample stage sends laser and sample is heated, the scope of the power of the laser pumping module in 0.1mW to 10mW
It is interior, the occurrence frequency of the laser pumping module within the 5kHz in the range of, the optical maser wavelength is 360nm-800nm.
9. thermoelectricity detecting system as claimed in claim 1, it is characterised in that the laser pumping module is from sample stage away from institute
The side for stating sample sends laser, and the laser is irradiated on the sample to enter sample via through the through hole of the sample stage
Row heating, the power of the laser pumping module is 250mW, the model of the occurrence frequency of the laser pumping module within 5kHz
In enclosing, the optical maser wavelength is 360nm-800nm.
10. thermoelectricity detecting system as claimed in claim 1, it is characterised in that the 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 scanning probe is additionally operable in probe excitation
Sample is heated and detected under pattern, the change in electric that the detection circuit is used to detect the scanning probe is examined
Signal is surveyed, the controller is based on the thermoelectricity capability of the detection signal analysis sample of the detection circuit output.
13. thermoelectricity detecting systems as claimed in claim 12, it is characterised in that the thermoelectricity detecting system also swashs including probe
Module is encouraged, the controller controls the probe excitation module to apply a frequency multiplication to the scanning probe under probe excitation pattern
Exchange electric excitation signal so that the scanning probe is heated to sample.
14. thermoelectricity detecting systems as claimed in claim 1, it is characterised in that the thermoelectricity detecting system also includes the first heat
Galvanic couple and the second thermocouple, first thermocouple are arranged on the sample stage and near one end of the sample, 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.
A kind of 15. thermoelectricity detection methods, it comprises the following steps:
Laser is provided to heat sample;
Sample is detected using probe is scanned;
The change in electric of the detecting scanning probe obtains detection signal;And
The thermoelectricity capability of the sample is analyzed based on the detection signal.
16. thermoelectricity detection methods as claimed in claim 15, it is characterised in that the thermoelectricity detection method also includes following step
Suddenly:Detect the laser and the laser being applied on sample is adjusted according to testing result.
17. thermoelectricity detection methods as claimed in claim 15, it is characterised in that the thermoelectricity detection method also includes following step
Suddenly:There is provided optics episcotister is used to switch or frequency modulation(PFM) the light source for sending the laser.
18. thermoelectricity detecting systems as claimed in claim 16, it is characterised in that described described based on detection signal analysis
The step of thermoelectricity capability of sample, also includes:Lock-in amplifier is provided to adopt the detection signal of the detection circuit output
Collection, and the step of coordinate the switch of the optics episcotister transient state based on time scale is carried out to sample to characterize.
19. thermoelectricity detecting systems as claimed in claim 18, it is characterised in that described described based on detection signal analysis
The step of thermoelectricity capability of sample, also includes:It is used to carry out a frequency multiplication and three to the detection signal using double frequency lock-in amplifier
The measurement of frequency multiplication and the detection signal of the detection signal and frequency tripling that obtain a frequency multiplication supplies subsequent analysis, wherein the frequency tripling
Detection signal embodies the thermal conductivity of sample.
20. thermoelectricity detection methods as claimed in claim 18, it is characterised in that described described based on detection signal analysis
The step of thermoelectricity capability of sample, also includes:To the lock-in amplifier collection detection signal changed, denoising, amplification,
After filtering process and be changed into standard signal, and by standard signal record in computer systems the step of.
21. thermoelectricity detection methods as claimed in claim 15, it is characterised in that the step of offer laser is heated to sample
Including:Laser pumping module is set away from the side of the sample stage in sample, the laser pumping module sends laser to sample
Product are heated, wherein the power of the laser pumping module is in the range of 0.1mW to 10mW, the laser pumping module
Occurrence frequency within the 5kHz in the range of, the optical maser wavelength is 360nm-800nm.
22. thermoelectricity detection methods as claimed in claim 15, it is characterised in that the step of offer laser is heated to sample
Including:Laser pumping module is set away from the side of the sample in sample stage, the laser pumping module sends laser, described
Laser is irradiated on sample via the through hole through the sample stage and sample is heated, the power of the laser pumping module
Be 250mW, the occurrence frequency of the laser pumping module within the 5kHz in the range of, the optical maser wavelength is 360nm-
800nm。
23. thermoelectricity detection methods as claimed in claim 15, it is characterised in that the electric signal of the detecting scanning probe
The step of change obtains detection signal includes:The scanning probe is detected by the Wheatstone bridge for electrically connecting the scanning probe
Change in electric and the step of obtain corresponding detection signal.
24. 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.
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