CN105510637B - Micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy and detection method - Google Patents
Micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy and detection method Download PDFInfo
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- CN105510637B CN105510637B CN201410495722.9A CN201410495722A CN105510637B CN 105510637 B CN105510637 B CN 105510637B CN 201410495722 A CN201410495722 A CN 201410495722A CN 105510637 B CN105510637 B CN 105510637B
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Abstract
The present invention provides a kind of micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy.The apparatus system is used with conductive, thermal conductivity probe, it is capable of providing the surface topography detection, electric signal detection and thermal signal detection mode of sample, by controlling displacement or the oscillation trajectory of probe, can in situ, synchronous, detection sample in real time electricity, hot property.Therefore, which, which overcomes existing scanning probe microscopy only, has the limitation of the electrically or thermally single detective function of signal；Simultaneously, can in situ, synchronous, detection material in real time temperature be distributed with thermal conductivity, electrical property and its Dynamic Evolution, to the Coupling Rule and mechanism between the intuitively magnetic heat of research material, help to reduce the power consumption of micro-/nano parts, improve its stability and integrated level, promote significantly it is micro-/receive the development of scale science of heat.
Description
Technical field
The application belongs to signal detection technical field more particularly to a kind of micro-/ nano heat based on scanning probe microscopy
Electric in-situ detector and detection method, can in situ, synchronous, real-time detection microcell electric conductivity and thermal property.
Background technology
Binning in 1981 et al. has invented scanning tunneling microscope (STM), and Nobel's physics thereby is achieved
Prize.STM is theoretical based on the tunnel-effect in quantum mechanics, when metal probe and sample surfaces with good conductivity close to when,
Tunnelling current is will produce under bias effect between metal probe and sample, which can accurately react probe and sample
The distance between, therefore STM can be imaged the sample of atomic scale, lateral resolution is up to 0.1nm.
But require sample surfaces that there is certain electric conductivity when being characterized to sample characteristics of for example using STM, therefore limit
Its application field.Bing et al. then develops scanning probe microscopy (SPM) technology, the technology by detect sample and
Interaction between SPM probe tips and under micro/nano-scale study sample corresponding properties, therefore promote micro-nano material
The performance characterization of material.
When being characterized to sample characteristics of for example using SPM, according to the phase interaction between the property and probe and sample of probe
With and obtain the characterization of sample different characteristics.For example, when characterization sample electric conductivity, detecting probe surface is needed to be coated with metal conducting layer
And electric current can be read under applied voltage；And when characterizing sample magnetic property, it is desirable that detecting probe surface is coated with thin magnetic film, relies on
Interaction between the magnetic moment and sample magnetic moment of the thin magnetic film characterizes sample magnetic property.Therefore, largely
The performance of probe determines the accuracy and reliability that sample characteristics of for example obtains.
With the miniaturization of electronic device and integrated, device size and device spacing have reached it is micro-/receive scale, hair
Heat becomes with heat dissipation problem restricts further highly integrated bottleneck.It is micro-/receive under scale, the microstructure of material and domain structure
Influence to thermal property is particularly important, and a micro-crack, hole, crystal boundary or even a domain wall may all influence material
Thermal property.By taking multi-iron material as an example, magnetic/electricdomain overturning (or domain wall drift) and leakage current in the case where outfield drives can all cause
Microcell generates heat.Therefore, it is micro-/receive characterization and the relevant physical property of heat under scale, understand the physical process of fever and heat dissipation at
For a brand-new branch in modern science of heat-it is micro-/to receive scale science of heat.
Therefore, mutual between the surface topography of research associated materials, especially micro Nano material, hot property and electrical property
Relationship is for understanding its intrinsic properties, fever and the physical mechanism of heat dissipation, and the related multifunctional material of development with extremely heavy
The meaning wanted.
But major part SPM at present, for example, conducting atomic force microscopy can only individually, it is real-time, characterize sample to ex situ
The shape characteristic and/or electrical property of product, and pattern, electric conductivity and thermal property cannot be characterized simultaneously.Therefore, how former
Position, synchronous, pattern, electric conductivity and thermal property of characterization micro Nano material in real time are the projects of scientific worker's research
One of.
Invention content
In view of the above technical problems, the present invention provides the signal detecting device under a kind of micro-/ nano scale, which can
For synchronizing, it is in situ, in real time to it is micro-/receive surface topography, thermal property and the electric conductivity of material under scale and detect.
Technical solution is used by the present invention realizes above-mentioned technical purpose：It is a kind of based on scanning probe microscopy it is micro-/
Nanometer thermoelectric in-situ detector, the detection device include as follows：
(1) scanning probe microscopy platform, probe, probe control unit
Probe control unit：Displacement and/or vibration are carried out for driving or controlling probe；
Probe：Conductive and thermal conductivity；
The probe includes feeler arm and needle point；
(2) Shape measure platform
Including displacement or vibration signals collecting unit, displacement signal or vibration signal for receiving probe；
Probe carries out transversal orientation scanning from initial position to sample surfaces, and probe tip and sample are controlled in scanning process
Makes point contact or vibration point contact, displacement or vibration signals collecting unit receive length travel signal or the vibration of probe tip
Signal, acquired analysis obtain the topography signal of sample；
(3) thermal signal detection platform
Including calorifics circuit and thermal signal collecting unit；
Electric signal, the electric signal is encouraged to flow into probe and carried out to probe by electric signal applying unit in the calorifics circuit
Heating, probe carry out heat exchange with sample, so that the voltage signal in calorifics circuit is changed, the variation of acquired voltage signal
Obtain the thermal signal of sample；
(4) electrical signal detection platform
Including electrical return and electrical signal collection unit；
The electrical return encourages electric signal, the electric signal to flow into probe, sample successively by electric signal applying unit, passes through
Electrical signal collection unit obtains the electric signal of sample；
(5) centralized control unit
For initializing system each unit, control system each unit receives after the pattern of sample, heat, electric signal, analysis
To the pattern of sample, heat, electric signal image.
Preferably, resistance heating platform is arranged in the scanning probe microscopy platform, for providing varying temperature environment.
The present invention also provides a kind of preferred probe structures, and as shown in Figure 1, 2, probe includes feeler arm 1 and needle point 2,
Needle point 2 is made of needle point ontology 3 with coating, and coating is by the film 1 positioned at 3 surface of needle point ontology, film one surface
Film 25, two surface of film film 36 form；Film 1 is conductive, film 25 has electrical insulating property, film 36
Conductive, film 1 is different from the material of film 36；Also, film 1, film 25 and film 36 constitute thermocouple
Structure, i.e.,：At the tip position of needle point ontology, one 4 surface of film is film 36, remaining position in addition to body tip is thin
Film 25 is between film 1 and film 36.
One 4 material of film is unlimited, includes a kind of material in metal and semiconductor with excellent conductive performance
Or metals and its alloy such as two or more combined materials, such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), graphite, stone
At least one of semiconductors such as black alkene.
25 material of film is unlimited, includes semiconductor, inorganic material or organic material with certain insulation performance
Material, such as zinc oxide (ZnO), bismuth ferrite (BiFeO3), cobalt acid lithium (LiCoO2), nickel oxide (NiO), cobalt oxide (Co2O3), oxygen
Change copper (CuxO), silica (SiO2), silicon nitride (SiNx), titanium dioxide (TiO2), tantalum pentoxide (Ta2O5), five oxidation
Two niobium (Nb2O5), tungsten oxide (WOx), hafnium oxide (HfO2), aluminium oxide (Al2O3), carbon nanotube, graphene, graphite oxide
Alkene, amorphous carbon, copper sulfide (CuxS), silver sulfide (Ag2S), non-crystalline silicon, titanium nitride (TiN), polyimides (PI), polyamide
(PAI), at least one of poly- Schiff base (PA), polysulfones (PS) etc..
36 material of film is unlimited, includes a kind of material in metal and semiconductor with excellent conductive performance
Or two or more combined material.Described metal and semiconductor with excellent conductive performance include but not limited to bismuth, nickel,
The metals such as cobalt, potassium and its alloy, at least one of semiconductors such as graphite, graphene.
The thermocouple structure that film one, film two and the film three is constituted may be used to be obtained following preparation method
It arrives：
Step 1 prepares film 1 using the method for plated film in needle point body surface；
Step 2 prepares film 25 using the method for plated film on the surface of film 1；
Step 3 removes the film 25 at needle point body tip using the method for etching, exposes film 1；
Step 4, one surface of film exposed described in step 3 using the method for plated film prepare film 36, make film 1
It is connect at needle point tip position with film 36, forms thermocouple structure.
In above-mentioned preparation method, the method for the plated film in the step 1,2,4 includes but not limited to various solution spin coatings
One or more kinds of combinations in the methods of method, inkjet printing, solid sputtering, thermal evaporation, electron beam evaporation；It is described
Step 3 in except the method for needle point tip film two includes but not limited to the methods of dry etching, wet etching, such as it is ion etching, anti-
Answer ion etching, chemical etching etc..
As shown in figure 3, the thermocouple structure that the film 1, film 25 and film 36 are constituted can also use
Following another kind preparation method obtains：
Step 1, the method using plated film prepare film 1, film 25 and film 36 on 3 surface of needle point ontology successively；
Step 2 applies voltage between film 36 and electrode layer 7, using point discharge principle, by adjusting film 36
The distance between electrode layer 7 makes the film 36 of needle point point melt, and exposes film 25, and other position films 36 do not have
Melting；
Step 3：The film 25 exposed described in removal step 2 exposes film 1；
Step 4：Using the method for plated film, material identical with film 36 is plated in the extending part, make film 1 and
Film 36 connects at needle point tip position, forms thermocouple structure.
In above-mentioned preparation method, the method for the plated film in the step 1,4 includes but not limited to various solution spin coating sides
One or more kinds of combinations in the methods of method, inkjet printing, solid sputtering, thermal evaporation or electron beam evaporation.
When using above-mentioned probe with thermocouple structure, it is former that the present invention is based on the nanometer thermoelectrics of scanning probe microscopy
The operating mode of position detection device includes the following two kinds, is respectively used to detect the pattern of sample and electric signal and thermal signal：
(1) pattern one：Surface topography and electric signal for detecting sample
Probe actuation unit driving probe is moved to sample surfaces initial position, and probe is transversely right from the initial position
Sample surfaces are oriented scanning, probe tip and sample surfaces point contact or vibration point contact are controlled in scanning process, simultaneously
Electric signal applying unit, film one, film three and sample form the electrical return being closed；Displacement or vibration signals collecting unit
The length travel signal or vibration signal for receiving probe tip, analyze to obtain the topography signal of sample through centralized control unit；Together
When, electric signal applying unit applies electric signal to needle point, which flows into film one, film three and sample, forms voltage
Signal obtains the electric signal of sample through electrical signal collection unit, analyzes to obtain the electric signal image of sample through centralized control unit.
(2) pattern two：Thermal signal for detecting sample
Electric signal applying unit, film one, film three form the electrothermal circuit being closed；Probe actuation unit drives probe position
Sample surfaces position is moved to, needle point is made to be in contact with sample surfaces, electric signal applying unit applies electric signal, electric current to needle point
It flows into needle point and it is heated, needle point carries out heat exchange with sample, makes to generate voltage signal in calorifics circuit, believe through calorifics
Number collecting unit obtains the thermal signal of sample, analyzes to obtain the thermal signal image of sample through centralized control unit.
When using the probe of above-mentioned thermocouple structure, using the present invention is based on the nanometer thermoelectric of scanning probe microscopy originals
Position detection device is in situ to pattern, electrical property and the hot property progress of sample, synchronous, the method for real-time detection is as follows：
Step 1：Sample is fixed on scanning probe microscopy platform, and using above-mentioned detection mode one, probe is moved to just
Beginning position is transversely oriented scanning to sample surfaces, obtains the feature image and electric signal image of sample；
Step 2：Probe is moved to the initial position in step 1, using above-mentioned detection mode two, is walked to sample surfaces
Transversal orientation scanning described in rapid 1, obtains the thermal signal image of sample.
The invention also provides another preferred probe structures.In the structure, as shown in Figure 1, probe includes feeler arm 1
With needle point 2.Needle point 2 is as shown in figure 4, including needle point ontology 3, thermal resistance material layer 8, the first conductive layer 9 and the second conductive layer
10；Thermal resistance material layer 8 is located at 3 surface of needle point ontology, and the second conductive layer 10 is located at thermal resistance material surface；First conductive layer
9 are connected with thermal resistance material layer 8；Thermal resistance material layer 8 is made of thermal resistance material, for detecting sample temperature variation and heat
It leads；First conductive layer 9 is constructed from a material that be electrically conducting, and is connect with thermal resistance material, the variation for detecting thermal resistance material resistance value；The
Two conductive layers 10 are constructed from a material that be electrically conducting.
8 material of thermal resistance material layer is unlimited, includes with low-doped silicon, semiconductor and metallic resistance material
Deng.
First conductive layer, 9 material is unlimited, includes one kind in metal and semiconductor with excellent conductive performance
Metals and its alloy such as material or two or more combined materials, such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), stone
At least one of semiconductors such as ink, graphene.
Second conductive layer, 10 material is unlimited, includes one kind in metal and semiconductor with excellent conductive performance
Metals and its alloy such as material or two or more combined materials, such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), stone
At least one of semiconductors such as ink, graphene.
The preparation method of above-mentioned probe is as follows：
Step 1 prepares thermal resistance material layer 8 using the method for plated film in needle point body surface；
Step 2 prepares the first conductive layer 9 using the method for plated film in needle point body surface；
Step 3 prepares the second conductive layer 10 using the method for plated film on 8 surface of thermal resistance material layer.
In above-mentioned preparation method, the method for the plated film in the step 1,2,3 includes but not limited to various solution spin coatings
One or more kinds of groups in the methods of method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporation
It closes.
Preferably, the thickness of the thermal resistance material layer 8 is 0.1 μm~10 μm.
Preferably, the thickness of first conductive layer 9 is 0.1 μm~1 μm.
When using above-mentioned probe with thermal resistance structure, it is former that the present invention is based on the nanometer thermoelectrics of scanning probe microscopy
The operating mode of position detection device includes the following two kinds, is respectively used to detect the pattern of sample and electric signal and thermal signal：
(1) pattern one：Surface topography and electric signal for detecting sample
Probe actuation unit driving probe is moved to sample surfaces initial position, and probe is transversely right from the initial position
Sample surfaces are oriented scanning, probe tip and sample surfaces point contact or vibration point contact are controlled in scanning process, simultaneously
Electric signal applying unit, the first conductive layer, thermal resistance material layer and the second conductive layer form the electrical return being closed；Displacement or
Vibration signals collecting unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain sample through centralized control unit
The topography signal of product；Meanwhile electric signal applying unit applies electric signal to needle point, which flows into the first conductive layer, thermoelectricity
Material layer, the second conductive layer and sample are hindered, voltage signal is formed, the electric signal of sample is obtained through electrical signal collection unit, is passed through
Centralized control unit is analyzed to obtain the electric signal image of sample；
(2) pattern two：Thermal signal for detecting sample
Electric signal applying unit, the first conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit pair
Thermal resistance material layer is heated, and then is heated to probe tip so that the temperature of probe tip is different from the temperature of sample
It spends (being typically chosen the temperature higher than sample)；Probe actuation unit driving probe tip is in contact with sample, sample and probe needle
Heat exchange occurs for point, and then influences the temperature of thermal resistance material layer, due to thermal resistance effect so that the resistance of thermal resistance material layer
Value changes, and is analyzed through centralized control unit after the acquisition of thermal signal collecting unit, obtains the thermal signal image of sample.
In above structure, thermal resistance material layer and the second conductive layer are in stacked arrangement at the tip position of needle point ontology,
In view of in actual fabrication process, since the tip location cross section of needle point ontology is smaller, coating prepares difficulty, especially
It is more difficult when preparing the multilayer laminate constructions, therefore preferably, second conductive layer is integrated in thermal resistance material
In layer.
As another preferred structure, insulating layer is set between the resistance elements and the second conductive layer, makes resistance
Material layer is mutually electrically insulated with the second conductive layer, and first conductive layer is electrically connected with the second conductive layer.In the structure, when adopting
When detecting the electric signal of sample with above-mentioned pattern one, electric signal applying unit, the first conductive layer and the formation of the second conductive layer are closed
The electrical return of conjunction, electric signal applying unit apply electric signal to needle point, which flows into the first conductive layer, the second conductive layer
And sample, voltage signal is formed, the electric signal of sample is obtained through electrical signal collection unit, analyzes to obtain through centralized control unit
The electric signal image of sample.
When using the probe of above-mentioned thermal resistance structure, using the present invention is based on the nanometer thermoelectric of scanning probe microscopy originals
Position detection device carries out the electricity of sample, hot property that in situ, synchronous, the method for real-time detection is as follows：
Step 1：Sample is fixed on scanning probe microscopy platform, and using above-mentioned detection mode one, probe is moved to just
Beginning position is transversely oriented scanning to sample surfaces, obtains the feature image and electric signal image of sample；
Step 2：Probe is moved to the initial position in step 1, using above-mentioned detection mode two, is walked to sample surfaces
Transversal orientation scanning described in rapid 1, obtains the thermal signal image of sample.
The present invention also provides a kind of preferred probe control unit structure, as shown in figure 5, the probe control unit be with
The piezoelectric actuator that probe is connected.At this point, the displacement signal acquisition unit include light source, photoelectricity four-quadrant detector with
And signal processor；When working condition, sample is placed in scanning probe microscopy platform, and probe carries out under piezoelectric actuator effect
Vibration, light source irradiate feeler arm, and reflection signal is collected by photoelectricity four-quadrant detector, then after signal processor processes
It is connected with centralized control unit.
As a kind of realization method, as shown in figure 5, the signal processor includes front-end amplifier, integrator, high pressure
Amplifier, delayer, lock-in amplifier and backend amplifier.Photoelectricity four-quadrant detector passes through front-end amplifier and integrator phase
Connection, integrator are connected with high-voltage amplifier, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, constitutes closed loop control
System, another way signal are connected with delayer, and (frequency tripling is logical by 1 ω (frequency multiplication chain) of delayer and lock-in amplifier and 3 ω
Road) channel is connected, and lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with control centre.
As a kind of realization method, as shown in figure 5, the thermal signal collecting unit includes delayer, lock-in amplifier
With backend amplifier.
In conclusion the nanometer thermoelectric in-situ detector provided by the invention based on scanning probe microscopy is with as follows
Advantage：
(1) the existing detection device based on scanning probe microscopy only has the function of electrically or thermally signal detection, the present invention
The detecting function limitation is breached, the detecting function of electric signal and thermal signal is provided；
(2) apply electric field and temperature field by situ, practical usage environment can be simulated, realize swashing in multiple physical field
Encourage or act on lower excitation heat in situ/electricdomain overturning, introduce leakage current etc., realize temperature that is in situ, synchronous, detecting material in real time
Degree and thermal conductivity distribution and its Dynamic Evolution, thus can in situ, the intuitively Coupling Rule between the electric-thermal of research material
With mechanism.
Therefore, the present invention has expanded the function of scanning probe microscopy, not the only research of thermoelectricity functional material and device
Advanced test platform is provided, to reduce the power consumption of micro-/nano parts, improve its stability and integrated level provides side
Help, at the same will also promote significantly it is micro-/receive the development of scale science of heat.
Description of the drawings
Fig. 1 is that have thermocouple structure in the nanometer thermoelectric in-situ detector the present invention is based on scanning probe microscopy
The overlooking structure diagram of probe；
Fig. 2 is the enlarged drawing with thermocouple structure probe tip in Fig. 1；
Fig. 3 is to prepare the schematic diagram with thermocouple structure probe tip in Fig. 1 using point discharge fusion method；
Fig. 4 is that have thermal resistance structure in the nanometer thermoelectric in-situ detector the present invention is based on scanning probe microscopy
Probe tip structural schematic diagram；
Fig. 5 is a kind of preferred function knot of the nanometer thermoelectric in-situ detector the present invention is based on scanning probe microscopy
Structure schematic diagram.
Specific implementation mode
Below in conjunction with attached drawing, embodiment, invention is further described in detail, it should be pointed out that implementation as described below
Example is intended to be convenient for the understanding of the present invention, and does not play any restriction effect to it.
Wherein：1- feeler arms, 2- needle points, 3- needle point ontologies, 4- films one, 5- films two, 6- films three, 7- electrode layers,
8- thermal resistance material layers, the first conductive layers of 9-, the second conductive layers of 10-.
Embodiment 1：
In the present embodiment, the nanometer thermoelectric in-situ detector based on scanning probe microscopy includes scanning probe microscopy
Platform, probe, probe control unit, topography signal detection platform, electric signal monitoring platform, thermal signal detection platform, Yi Jizhong
Heart control unit.
Probe control unit carries out displacement and/or vibration for driving or controlling probe；
Topography signal detection platform includes displacement or vibration signals collecting unit, displacement signal for receiving probe or is shaken
Dynamic signal；
Electrical signal detection platform includes electrical return and electrical signal collection unit；Electrical return is swashed by electric signal applying unit
Electric signal is encouraged, which flows into probe, sample successively, and the electric signal of sample is obtained through electrical signal collection unit；
Thermal signal detection platform includes calorifics circuit and thermal signal collecting unit；Swashed by electric signal applying unit in calorifics circuit
Electric signal is encouraged, which flows into probe and heated to probe, and probe carries out heat exchange with sample, makes in calorifics circuit
Voltage signal changes, acquired to obtain the thermal signal of sample；
Centralized control unit is for initializing system each unit, control system each unit, receive the pattern of sample, electricity and
The pattern, electricity, thermal signal image of sample are obtained after thermal signal, analysis.
As shown in Figure 1, probe includes feeler arm 1 and needle point 2.
The structure of needle point 2 as shown in Fig. 2, be made of with surface coating needle point ontology 3, surface coating by film 1,
One 4 surface of film covers film 25,25 surface of film covers film 36.Film 1 is conductive, film 25 has electricity
Insulating properties, film 36 are conductive, and film 1 is different from the material of film 36；Also, film 1, film 25 and thin
Film 36 constitutes thermocouple structure, i.e.,：In the tip location of needle point ontology 3, one 4 surface of film covers film 36, and needle point sheet
Remaining position of body 3 in addition to tip, film 25 is between film 1 and film 36.
The probe tip with thermocouple structure may be used following method and prepare, and this method comprises the following steps：
Step 1, the method using plated film, such as the sputtering of solution spin coating method, inkjet printing, solid, thermal evaporation, person's electronics
The methods of beam evaporation prepares film 1 on 3 surface of needle point ontology；
Step 2, the method using plated film, such as the sputtering of solution spin coating method, inkjet printing, solid, thermal evaporation, person's electronics
The methods of beam evaporation prepares film 25 on 3 surface of needle point ontology；
Step 3 is gone using the methods of dry etching, wet etching, such as the methods of ion etching, reactive ion etching, chemical etching
Except the film 25 at 3 tip of needle point ontology, expose film 1；
Step 4, the method using plated film, such as the sputtering of solution spin coating method, inkjet printing, solid, thermal evaporation, person's electronics
The methods of beam evaporation prepares film 36 on 3 surface of needle point ontology, and one 4 surface of film at 3 tip of needle point ontology is made to cover film
36, remaining position in addition to tip, film 25 is between film 1 and 36.
The material of film 1 is conductive metal Pt, and the material of thickness 100nm, film 25 are insulating layer Al2O3, thickness
Material for 200nm, film 36 is conductive metal Ni, thickness 100nm.
Probe control unit uses the piezoelectric actuator being connected with probe.The piezoelectric actuator selects U.S. Asylum
The MFP-3D-SA-SCANNER scanners of Research companies production, scanning range X × Y=90 × 90 μm2。
As shown in figure 5, displacement or vibration signals collecting unit include light source, photoelectricity four-quadrant detector and signal processing
Device.Signal processor is by front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier and backend amplifier group
At.When working condition, sample is placed in scanning probe microscopy platform, and probe is vibrated under piezoelectric actuator effect, light source
Feeler arm is irradiated, reflection signal is collected by photoelectricity four-quadrant detector, is then connected with integrator by front-end amplifier,
Integrator is connected with high-voltage amplifier, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, constitutes closed-loop control, separately
Signal is connected with delayer all the way, and 1 ω (frequency multiplication chain) and 3 ω (frequency tripling channel) of delayer and lock-in amplifier are logical
Road is connected, and lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with control centre.
Control centre is made of computer, initialization module, control module.
Thermal signal collecting unit is made of delayer, lock-in amplifier and backend amplifier.Electrical signal collection unit is by prolonging
When device, lock-in amplifier and backend amplifier form.In the present embodiment, the thermal signal collecting unit, electrical signal collection unit with
Signal processor is integrated.
Electric signal applying unit in calorifics circuit is current source.
Electrical return is voltage source by electric signal applying unit.
In the present embodiment, it is study sample to select the Fe films grown on ferroelectric substrate PMN-PT, and the thickness of the sample is
90nm。
Using the above-mentioned nanometer thermoelectric in-situ detector based on scanning probe microscopy, at room temperature to the hot of sample
Energy progress is in situ, synchronous, the method for real-time detection is as follows：
(1) sample is fixed on scanning probe microscopy platform, passes through initialization module initialization system each unit initial parameter；
(2) under control module effect, piezoelectric actuator driving probe is moved to sample surfaces initial position, and light source shines
Feeler arm is penetrated, reflection signal is collected by photoelectricity four-quadrant detector；Probe from the initial position transversely to sample surfaces into
Row direct scan, the film 36 on 2 surface of control probe tip and sample surfaces point contact or vibration point contact in scanning process；
Meanwhile current source, film 1, film 36 and sample form the electrical return being closed；
Reflection signal is collected by photoelectricity four-quadrant detector, is then connected with integrator by front-end amplifier, product
Device is divided to be connected with high-voltage amplifier, the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, constitutes closed-loop control, another
Road signal is connected with delayer, 1 ω (frequency multiplication chain) of delayer and lock-in amplifier and 3 ω (frequency tripling channel) channel
It is connected, lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with computer, is obtained after analyzing processing
The topography signal image of sample；Meanwhile current source to probe apply electric signal, the electric signal flow into film 1, film 36 with
And after sample, the earth is flowed into, voltage signal is formed, acquires the signal, through delayer, lock-in amplifier and backend amplifier, with
Computer is connected, and the electric signal image of the position sample is obtained after analyzing processing；
(3) piezoelectric actuator driving probe is back to the initial position described in step (2) and raises a spacing upwards
From, sample surfaces are scanned again according to the transversal orientation described in step (2), in scanning process control 2 table of probe tip
The film 36 in face carries out length travel or vibration, displacement or vibration signals collecting unit along the feature image that step (2) obtains
The length travel signal or vibration signal of probe tip are received, reflection signal is collected by photoelectricity four-quadrant detector, then such as
Step (1) is described, by front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier, backend amplifier, with
Computer is connected, and the electric signal image of sample is obtained after analyzing processing；
(4) piezoelectric actuator driving probe is back to the initial position described in step (2)；
(5) film 36 on 2 surface of needle point is made to be in contact with sample surfaces；Current source, film 1 and the formation of film 36
The electrothermal circuit of closure；Current source applies electric signal to probe, and electric current flows into needle point 2 and heated to it, needle point 2 and sample
Carry out heat exchange, so that the voltage signal in the calorifics circuit is changed, acquire the signal, through delayer, lock-in amplifier with
Backend amplifier is connected with computer, and the thermal signal image of the position sample is obtained after analyzing processing；
(6) according to the horizontal direction described in step (2), piezoelectric actuator drives probe to the next position；
(7) every bit repeats step (5) and (6), until point-by-point to sample surfaces according to the horizontal direction described in step (2)
It is scanned.
Embodiment 2：
In the present embodiment, the nanometer thermoelectric in-situ detector based on scanning probe microscopy and complete phase in embodiment 1
Together.
It is alternatively prepared except that should be adopted with the probe tip of thermocouple structure, this method includes as follows
Step：
Step 1, the method using plated film prepare film 1, film 25 and film 36 on 3 surface of needle point ontology successively；
Step 2 applies voltage between film 36 and electrode layer 7, using point discharge principle, by adjusting film 36
The distance between electrode layer 7 makes the film 36 of needle point point melt, and exposes film 25, and other position films 36 do not have
Melting；
Step 3：The film 25 exposed described in removal step 2 exposes film 1；
Step 4：Using the method for plated film, material identical with film 36 is plated in the extending part, make film 1 and
Film 36 connects at needle point tip position, forms thermocouple structure.
Using the nanometer thermoelectric in-situ detector based on scanning probe microscopy at room temperature to the electric, hot of sample
Energy progress is in situ, synchronous, the method for real-time detection is identical with embodiment 1.
Embodiment 3：
In the present embodiment, in the structure and embodiment 1 of the nanometer thermoelectric in-situ detector based on scanning probe microscopy
It is essentially identical, except that using the probe with thermal resistance structure.
As shown in Figure 1, the probe includes feeler arm 1 and needle point 2.Needle point 2 is as shown in figure 4, including needle point ontology 3, thermoelectricity
Hinder material layer 8, the first conductive layer 9 and the second conductive layer 10；Thermal resistance material layer 8 is located at 3 surface of needle point ontology, and second is conductive
Layer 10 is located at thermal resistance material surface；Conductive layer 9 is electrically connected with 8 phase of thermal resistance material layer.
8 material of thermal resistance material layer is low-doped silicon, and thickness 2m, 9 material of conductive layer is bismuth (Bi), nickel (Ni), cobalt
(Co), one kind in potassium (K), graphite, graphene, thickness are 1 μm, and 10 material of the second conductive layer is bismuth (Bi), nickel (Ni), cobalt
(Co), one kind in potassium (K), graphite, graphene, thickness are 0.1 μm.
The preparation method of above-mentioned probe is as follows：
Step 1, using plated films such as solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporations
Method prepare thermal resistance material layer 8 in needle point body surface；
Step 2, using plated films such as solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporations
Method prepare the first conductive layer 9 in needle point body surface, which is connected with thermal resistance material layer 8；
Step 3, using plated films such as solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporations
Method 8 surface of thermal resistance material layer prepare the second conductive layer 10.
Using the above-mentioned nanometer thermoelectric in-situ detector based on scanning probe microscopy, at room temperature to the electricity of sample,
Hot property progress is in situ, synchronous, the method for real-time detection is as follows：
(1) sample is fixed on scanning probe microscopy platform, passes through initialization module initialization system each unit initial parameter；
(2) under control module effect, piezoelectric actuator driving probe is moved to sample surfaces initial position, and light source shines
Feeler arm is penetrated, reflection signal is collected by photoelectricity four-quadrant detector；Probe from the initial position transversely to sample surfaces into
Row direct scan, second conductive layer 10 on 2 surface of control probe tip and sample surfaces point contact or oscillation point in scanning process
Contact；Meanwhile current source, the first conductive layer 9, thermal resistance material layer 8, the second conductive layer 10 and sample form the electricity being closed
Circuit；
Reflection signal is collected by photoelectricity four-quadrant detector, is then connected with integrator by front-end amplifier, product
Device is divided to be connected with high-voltage amplifier, the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, constitutes closed-loop control, another
Road signal is connected with delayer, 1 ω (frequency multiplication chain) of delayer and lock-in amplifier and 3 ω (frequency tripling channel) channel
It is connected, lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with computer, is obtained after analyzing processing
The topography signal image of sample；Meanwhile current source applies electric signal to probe, which flows into the first conductive layer 9, thermal resistance
After material layer 8, the second conductive layer 10 and sample, the earth is flowed into, voltage signal is formed, the signal is acquired, through delayer, locking phase
Amplifier and backend amplifier, are connected with computer, and the electric signal image of the position sample is obtained after analyzing processing；
(3) piezoelectric actuator driving probe is back to the initial position described in step (2)；
(4) second conductive layer 10 on 2 surface of needle point is made to be in contact with sample surfaces；Current source, the first conductive layer 9 and heat
Resistance elements 8 form the electrothermal circuit being closed；Electric signal applying unit heats thermal resistance material layer 8, and then to visiting
Needle needle point is heated so that the temperature of probe tip is higher than the temperature of sample；Probe actuation unit drives probe tip and sample
Condition contacts, and heat exchange occurs for sample and probe tip, and then influences the temperature of thermal resistance material layer 8, due to thermal resistance effect,
So that the resistance value of thermal resistance material layer 8 changes, the signal is acquired, through delayer, lock-in amplifier and backend amplifier,
It is connected with computer, the thermal signal image of the position sample is obtained after analyzing processing；
(5) according to the horizontal direction described in step (2), piezoelectric actuator drives probe to the next position；
(6) every bit repeats step (4) and (5), until point-by-point to sample surfaces according to the horizontal direction described in step (2)
It is scanned.
Embodiment 4：
In the present embodiment, the nanometer thermoelectric in-situ detector based on scanning probe microscopy and basic phase in embodiment 3
Together, except that the second conductive layer 10 is integrated in thermal resistance material layer 8.
Technical scheme of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (11)
1. a kind of micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy, for detect sample surface topography,
Thermal property and electric conductivity, it is characterized in that：Including as follows：
(1) scanning probe microscopy platform, probe, probe control unit
Probe control unit：Displacement and/or vibration are carried out for driving or controlling probe；
Probe：Conductive and thermal conductivity；
The probe includes feeler arm and needle point；
(2) Shape measure platform
Including displacement or vibration signals collecting unit, displacement signal or vibration signal for receiving probe；
Probe carries out transversal orientation scanning from initial position to sample surfaces, and probe tip and sample surfaces are controlled in scanning process
Point contact, displacement or vibration signals collecting unit receive the length travel signal or vibration signal of probe tip, acquired analysis
Obtain the topography signal of sample；
(3) thermal signal detection platform
Including calorifics circuit and thermal signal collecting unit；
Electric signal, the electric signal is encouraged to flow into probe and add to probe by electric signal applying unit in the calorifics circuit
Heat, probe carry out heat exchange with sample, so that the voltage signal in calorifics circuit is changed, acquired voltage signal changes
To the thermal signal of sample；
(4) electrically conductive signal detection platform
Including electrical return and electrical signal collection unit；
The electrical return encourages electric signal by electric signal applying unit, which flows into probe, sample successively, through telecommunications
Number collecting unit obtains the electrically conductive signal of sample；
(5) centralized control unit
For initializing system each unit, control system each unit obtains after receiving the pattern of sample, heat, electrically conductive signal, analysis
Pattern, heat, the electrically conductive signal image of sample.
2. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as described in claim 1, it is characterized in that：
The probe control unit is the piezoelectric actuator being connected with feeler arm；
The displacement or vibration signals collecting unit includes light source, photoelectricity four-quadrant detector and signal processor；
When working condition, sample is placed in scanning probe microscopy platform, and probe carries out displacement or shaken under piezoelectric actuator effect
Dynamic, light source irradiates feeler arm, and reflection signal is collected by photoelectricity four-quadrant detector, then after signal processor processes with
Centralized control unit is connected.
3. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as claimed in claim 2, it is characterized in that：
The signal processor includes that front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier and rear end are amplified
Device；Photoelectricity four-quadrant detector is connected by front-end amplifier with integrator, and integrator is connected with high-voltage amplifier, high pressure
The signal all the way of amplifier feeds back to piezoelectric actuator, constitutes closed-loop control, and another way signal is connected with delayer, delayer
It is connected with a frequency multiplication chain of lock-in amplifier and frequency tripling channel channel, lock-in amplifier is connected with backend amplifier,
Backend amplifier is connected with centralized control unit.
4. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as described in claim 1, it is characterized in that：
The thermal signal collecting unit includes delayer, lock-in amplifier and backend amplifier.
5. the micro-/ nano thermoelectricity based on scanning probe microscopy as described in any claim in Claims 1-4 is visited in situ
Device is surveyed, it is characterized in that：The probe includes feeler arm and needle point, and needle point is made of needle point ontology with coating, coating
It is made of the film two of film one, one surface of film, the film three on two surface of film positioned at needle point body surface；Film one has
Conductive, film two has electrical insulating property, film three conductive, and film one is different from the material of film three；Also, it is thin
Film one, film two and film three constitute thermocouple structure.
6. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as claimed in claim 5, it is characterized in that：
The thermocouple structure that film one, film two and the film three is constituted uses to be obtained following preparation method：
Step 1 prepares film one using the method for plated film in needle point body surface；
Step 2 prepares film two using the method for plated film on one surface of film；
Step 3 removes the film two at needle point body tip using the method for etching, exposes film one；
Step 4 prepares film three using the method for plated film in one surface of film that step 3 is exposed, and film one is made to exist with film three
Needle point tip position connects, and forms thermocouple structure；
Alternatively, the thermocouple structure that the film one, film two and film three are constituted is used and is obtained following preparation method：
Step 1, the method using plated film prepare film one, film two and film three in needle point body surface successively；
Step 2 applies voltage between film three and electrode layer, using point discharge principle, by adjusting film three and electrode
Distance between layer, makes the film three of needle point point melt, and exposes film two, and other position films three do not melt；
Step 3：The film two that removal step is exposed exposes film one；
Step 4：Using the method for plated film, material identical with film three is plated in the extending part of film one, make film one with it is thin
Film three connects at needle point tip position, forms thermocouple structure.
7. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as claimed in claim 6, it is characterized in that：
Including the following two kinds detection mode：
(1) pattern one：Surface topography and electrically conductive signal for detecting sample
Probe actuation unit driving probe is moved to sample surfaces initial position, and probe is from the initial position transversely to sample
Surface is oriented scanning, control probe tip and sample surfaces point contact in scanning process, while electric signal applying unit, thin
Film one, film three and sample form the electrical return being closed；Displacement or vibration signals collecting unit receive the vertical of probe tip
To displacement signal or vibration signal, analyze to obtain the topography signal of sample through centralized control unit；Meanwhile electric signal applying unit
Electric signal is applied to needle point, which flows into film one, film three and sample, voltage signal is formed, through electrical signal collection
Unit obtains the electrically conductive signal of sample, analyzes to obtain the electrically conductive signal image of sample through centralized control unit；
(2) pattern two：Thermal signal for detecting sample
Electric signal applying unit, film one, film three form the calorifics circuit being closed；Probe actuation unit driving probe is moved to
Sample surfaces position, makes needle point be in contact with sample surfaces, and electric signal applying unit applies electric signal to needle point, and electric current flows into
Needle point simultaneously heats it, and needle point carries out heat exchange with sample, makes to generate voltage signal in calorifics circuit, be adopted through thermal signals
Collection unit obtains the thermal signal of sample, analyzes to obtain the thermal signal image of sample through centralized control unit.
8. utilizing the detection mould of the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy described in claim 7
Formula is in situ, synchronizes, the method for the electricity of real-time detection sample, hot property, it is characterized in that：Include the following steps：
Step 1：Sample is fixed on scanning probe microscopy platform, and using above-mentioned detection mode one, probe is moved to initial bit
It sets, scanning transversely is oriented to sample surfaces, obtain the feature image and electrically conductive signal image of sample；
Step 2：Probe is moved to the initial position in step 1, using above-mentioned detection mode two, along the transverse direction described in step 1
Scanning is oriented to sample surfaces, obtains the thermal signal image of sample.
9. the micro-/ nano thermoelectricity based on scanning probe microscopy as described in any claim in Claims 1-4 is visited in situ
Device is surveyed, it is characterized in that：The needle point includes needle point ontology, thermal resistance material layer, the first conductive layer and the second conductive layer；
Thermal resistance material layer is located at needle point body surface, and the second conductive layer is located at thermal resistance material surface；First conductive layer and thermoelectricity
Resistance material layer is connected.
10. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as claimed in claim 9, it is characterized in that：
Second conductive layer is integrated in thermal resistance material layer.
11. the micro-/ nano thermoelectricity in-situ detector based on scanning probe microscopy as claimed in claim 9, it is characterized in that：
Including the following two kinds detection mode：
(1) pattern one：Surface topography and electrically conductive signal for detecting sample
Probe actuation unit driving probe is moved to sample surfaces initial position, and probe is from the initial position transversely to sample
Surface is oriented scanning, control probe tip and sample surfaces point contact in scanning process, while electric signal applying unit, the
One conductive layer, thermal resistance material layer and the second conductive layer form the electrical return being closed；Displacement or vibration signals collecting unit
The length travel signal or vibration signal for receiving probe tip, analyze to obtain the topography signal of sample through centralized control unit；Together
When, electric signal applying unit applies electric signal to needle point, and the first conductive layer of electric signal inflow, thermal resistance material layer, second are led
Electric layer and sample form voltage signal, the electrically conductive signal of sample are obtained through electrical signal collection unit, through centralized control unit point
Analysis obtains the electrically conductive signal image of sample；
(2) pattern two：Thermal signal for detecting sample
Electric signal applying unit, the first conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit is to thermoelectricity
Resistance material layer is heated, and then is heated to probe tip so that the temperature of probe tip is different from the temperature of sample；It visits
Needle driving unit driving probe tip is in contact with sample, and with probe tip heat exchange occurs for sample, and then influences thermal resistance
The temperature of material layer, due to thermal resistance effect so that the resistance value of thermal resistance material layer changes, and is adopted through thermal signal collecting unit
It is analyzed through centralized control unit after collection, obtains the thermal signal image of sample.
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| CN109917407A (en) * | 2019-03-22 | 2019-06-21 | 中国科学院重庆绿色智能技术研究院 | A kind of near field probe distance measuring method and device based on laser reflection |
| CN110907489A (en) * | 2019-11-13 | 2020-03-24 | 中国科学院上海硅酸盐研究所 | Nanoscale thermal conductivity-electric domain in-situ characterization device based on atomic force microscope |
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