CN105510642B - Nano magnetic heating in-situ detector and detection method based on scanning probe microscopy - Google Patents
Nano magnetic heating in-situ detector and detection method based on scanning probe microscopy Download PDFInfo
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- CN105510642B CN105510642B CN201410494331.5A CN201410494331A CN105510642B CN 105510642 B CN105510642 B CN 105510642B CN 201410494331 A CN201410494331 A CN 201410494331A CN 105510642 B CN105510642 B CN 105510642B
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Abstract
The present invention provides a kind of nano magnetic heating in-situ detectors based on scanning probe microscopy.The apparatus system is used with magnetic, conductive, thermal conductivity probe, it is capable of providing the surface topography detection, magnetic 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 magnetic, hot property.Therefore, which overcomes the limitation that existing scanning probe microscopy only has the function of the single detective of magnetic or thermal signal；Simultaneously, can in situ, synchronous, detection material in real time temperature be distributed with thermal conductivity, domain structure and its Dynamic Evolution, so as 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 nano magnetic pyrogen based on scanning probe microscopy
Position detection device and detection method.
Background technology
The fever of micro-/nano parts is a current important bottle for restricting electronic device stability and integrated level with heat dissipation problem
Neck.It is micro-/receive the thermal property of research material under scale, understand that fever and the physical process of heat dissipation have caused people to pay close attention to,
And gradually develop into a new subject --- it is micro-/to receive scale science of heat.
Under the conditions of usage, the fever of material and radiation processes usually with the microstructure of material and domain structure (including
Domain structure, ferroelectricity/piezoelectricity domain structure, conductive domain structure etc.) it is closely related.By taking magnetic material as an example, magnetic under being driven in outfield
Farmland overturning can generate microcell fever, if it is possible to which the physics such as magnetism, temperature, thermal conductivity are in real time joined in synchronous in microcell, original position
Amount is imaged, it is possible to be observed heat generating spot, the sinking path of material in real time in microcosmic point, be obtained they and material structure
Association between magnetism, this microcell fever for helping to understand magnetic material and the physical mechanism to radiate, micro- to reduction magnetoelectricity/
Power consumption, raising stability and the integrated level of nano parts have very important significance.In addition, in magnetic refrigerating material and magnetic Nano
For composite thermoelectric material, Material texture is explored in the magnetic domain overturning generation fuel factor under outer field action, the research of the fuel factor
It is of great significance with new material exploitation.
Existing micro-/calorifics Detection Techniques for receiving under scale can realize the measurement of micro-area temperature and thermal conductivity distribution, but
Be cannot it is in situ in microcell, synchronous, detect the physical parameters such as magnetism, temperature/thermal conductivity in real time, so as to limit to fever with
The deep understanding research of radiation processes and its physical mechanism.
Invention content
The technical purpose of the present invention be for it is above-mentioned it is micro-/receive the deficiencies of calorifics Detection Techniques under scale, provide it is a kind of it is micro-/receive
Signal detecting device under metrical scale, which can be used for synchronizing, is in situ, in real time to it is micro-/receive magnetism, the temperature of material under scale
Degree/thermal conductivity physical parameter is detected.
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-/
Nano magnetic heating many reference amounts in-situ detector, for synchronizing, microcell in situ, detecting sample of magnetic material to be measured in real time it is magnetic
With the thermoelectricity Physical Parameters such as temperature, thermal conductivity coefficient, Seebeck coefficient, and synchronous imaging；The detection device includes as follows：
(1) scanning probe microscopy platform, probe, probe control unit
Probe control unit：For driving or controlling probe to carry out displacement and/or vibration；
Probe：With magnetic, electric conductivity and thermal conductivity；
The probe includes feeler arm and needle point；
(2) pattern and magnetic signal detection platform
Including displacement or vibration signals collecting unit, for receiving the displacement signal of probe or vibration signal；
Probe carries out sample surfaces transversal orientation scanning from initial position, 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；
Probe is back to initial position and raises upwards after certain distance according to the transversal orientation to sample surfaces
It is scanned, probe tip is controlled to carry out length travel or vibration along the topography profile in scanning process, displacement or shake
Dynamic signal gathering unit receives the length travel signal or vibration signal of probe tip, and acquired analyze obtains the magnetic letter of sample
Number；
(3) thermal signal detection platform
Including calorifics circuit and thermal signal collecting unit；
Electric signal is encouraged in the calorifics circuit by electric signal applying unit, which flows into probe and probe is carried out
Heating, probe carry out heat exchange with sample, the voltage signal in calorifics circuit are made to change, the variation of acquired voltage signal
Obtain the thermal signal of sample；
(4) centralized control unit
For initializing system each unit, control system each unit receives after the pattern of sample, magnetic, thermal signal, analysis
To the pattern of sample, magnetic, thermal signal image.
Preferably, the scanning probe microscopy platform setting resistance heating platform, for providing varying temperature environment.
Preferably, the scanning probe microscopy platform setting hot-wire coil, for providing magnetic field 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 being located at the film 1 on 3 surface of needle point ontology, one surface of film
Film 25, the composition of film 36 on two surface of film；Film 1 is conductive, film 25 has electrical insulating property, film 36
With magnetism, film 1 is different from the material of film 36；Also, film 1, film 25 and film 36 form thermocouple junction
Structure, i.e.,：At the tip position of needle point ontology, one 4 surface of film be film 36, remaining position in addition to body tip, film
25 between film 1 and film 36.
One 4 material of film is unlimited, including a kind of material in metal and semiconductor with excellent conductive performance
Or two or more combined materials, such as metals and its alloy 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, including having the semiconductor of certain insulation performance, inorganic material or organic material
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, including ferromagnetic metal iron (Fe), cobalt (Co), nickel (Ni) and magnetic alloy.
The thermocouple structure that film one, film two and the film three is formed may be used following preparation method and obtain
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 prepares film 36 using the method for plated film in one surface of film exposed described in step 3, makes film 1
It is connect with film 36 at needle point tip position, 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 include but not limited to dry etching, wet etching the methods of, it is such as 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 formed 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 melts the film 36 of needle point point, 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, the 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, the present invention is based on the nano magnetic pyrogens of scanning probe microscopy
The operating mode of position detection device includes the following two kinds, is respectively used to the pattern of detection sample and magnetic signal, thermal signal：
(1) pattern one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact or vibration point contact, displacement are controlled in scanning process
Or vibration signals collecting unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain through centralized control unit
The topography signal of sample；
Probe is back to the initial position and raises certain distance upwards, then according to the transversal orientation pair
Sample surfaces are scanned, and probe tip are controlled to carry out length travel or vibration along the feature image in scanning process,
Displacement or vibration signals collecting unit receive the length travel signal or vibration signal of probe tip, are analyzed through centralized control unit
Obtain the magnetic signal image of sample；
(2) pattern two：For detecting the thermal signal of sample
Electric signal applying unit, film one, film three form the electrothermal circuit being closed；Probe actuation unit driving 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 nano magnetic pyrogens of scanning probe microscopy
Position detection device carries out the magnetic 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 sample surfaces scanning, obtains the feature image of sample and magnetic signal image；
Step 2：Probe is moved to the initial position in step 1, and using above-mentioned detection mode two, sample surfaces are walked
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, conductive layer 9 and magnetosphere 10；Thermal resistance
Material layer 8 is located at 3 surface of needle point ontology, and magnetosphere 10 is located at thermal resistance material surface；Conductive layer 9 and thermal resistance material layer 8
It is connected；Thermal resistance material layer 8 is made of thermal resistance material, for detecting sample temperature variation and thermal conductivity；Conductive layer 9 is by conduction
Material is formed, and is connect with thermal resistance material, for detecting the variation of thermal resistance material resistance value；Magnetosphere 10 is by magnetic material structure
Into for detecting sample magnetic signal.
8 material of thermal resistance material layer is unlimited, including with low-doped silicon, semiconductor and metallic resistance material
Deng.
9 material of conductive layer is unlimited, including a kind of material in metal and semiconductor with excellent conductive performance
Or two or more combined materials, such as metals and its alloy such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), graphite, stone
At least one of semiconductors such as black alkene.
10 material of magnetosphere is unlimited, including ferromagnetic metal iron (Fe), cobalt (Co), nickel (Ni) and magnetic alloy.
Preferably, insulating layer is set between the thermal resistance material layer and magnetosphere.
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 conductive layer 9 using the method for plated film in needle point body surface；
Step 3 prepares magnetosphere 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 the conductive layer 9 is 0.1 μm~1 μm.
When using above-mentioned probe with thermal resistance structure, the present invention is based on the nano magnetic pyrogens of scanning probe microscopy
The operating mode of position detection device includes the following two kinds, is respectively used to the pattern of detection sample and magnetic signal, thermal signal：
(1) pattern one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact or vibration point contact, displacement are controlled in scanning process
Or vibration signals collecting unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain through centralized control unit
The topography signal of sample；
Probe is back to the initial position and raises certain distance upwards, then according to the transversal orientation pair
Sample surfaces are scanned, and probe tip are controlled to carry out length travel or vibration along the feature image in scanning process,
Displacement or vibration signals collecting unit receive the length travel signal or vibration signal of probe tip, are analyzed through centralized control unit
Obtain the magnetic signal image of sample；
(2) pattern two：For detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit is to thermoelectricity
Resistance material layer is heated, and then probe tip is heated so that the temperature of probe tip is different from the temperature (one of sample
As be selected above the temperature of sample)；Probe actuation unit driving probe tip is in contact with sample, and sample occurs with probe tip
Heat exchange, and then the temperature of thermal resistance material layer is influenced, due to thermal resistance effect so that the resistance value of thermal resistance material layer occurs
Variation 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 8 and magnetosphere 10 are in multilayer laminated row at the tip position of needle point ontology
Row, it is contemplated that in actual fabrication process, since the tip location cross section of needle point ontology is smaller, coating prepares difficulty,
It especially prepares more difficult during the multilayer laminate constructions；On the other hand, in this multilayer laminate constructions, the point of needle point ontology
End position has concentrated the detection of magnetic signal and thermal signal, and the damage of thin film can lead to entire probe destruction, and utilization rate is not
It is high.
For this purpose, the present invention improves the stepped construction, thermal resistance material layer and conductive layer are arranged on probe wall
Position, and magnetosphere is only arranged on probe tip position, i.e., magnetosphere and thermal resistance material layer, conductive layer " divide
From ", this structure is specially：Probe includes feeler arm and needle point；Needle point includes needle point ontology and the magnetosphere positioned at its surface,
Thermal resistance material layer is set apart from needle point certain intervals on feeler arm, that is, non-between thermal resistance material layer and magnetosphere to be electrically connected
It is logical, and conductive layer is electrically connected with 8 phase of thermal resistance material layer.Preferably, conductive layer is arranged on thermal resistance material surface.
When using above-mentioned probe with thermal resistance structure, the present invention is based on the nano magnetic pyrogens of scanning probe microscopy
The operating mode of position detection device includes the following two kinds, is respectively used to the pattern of detection sample and magnetic signal, thermal signal：
(1) pattern one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact or vibration point contact, displacement are controlled in scanning process
Or vibration signals collecting unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain through centralized control unit
The topography signal of sample；
Probe is back to the initial position and raises certain distance upwards, then according to the transversal orientation pair
Sample surfaces are scanned, and probe tip are controlled to carry out length travel or vibration along the feature image in scanning process,
Displacement or vibration signals collecting unit receive the length travel signal or vibration signal of probe tip, are analyzed through centralized control unit
Obtain the magnetic signal image of sample；
(2) pattern two：For detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit is to thermoelectricity
Resistance material layer is heated；Probe actuation unit driving probe tip is in contact with sample, and sample occurs heat with probe tip and hands over
It changes, heat influences the temperature of thermal resistance material layer through air and probe wall, due to thermal resistance effect so that thermal resistance material layer
Resistance value change, analyzed after the acquisition of thermal signal collecting unit through centralized control unit, obtain the thermal signal figure of sample
Picture；
When using the probe of above-mentioned thermal resistance structure, using the present invention is based on the nano magnetic pyrogens of scanning probe microscopy
Position detection device carries out the magnetic 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 sample surfaces scanning, obtains the feature image of sample and magnetic signal image；
Step 2：Probe is moved to the initial position in step 1, and using above-mentioned detection mode two, sample surfaces are walked
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；During working condition, sample is placed in scanning probe microscopy platform, and probe carries out under piezoelectric actuator effect
Vibration, light source irradiation feeler arm, 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, forms closed loop control
System, another way signal are connected with delayer, and (frequency tripling leads to 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 nano magnetic heating 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 magnetic or thermal signal detecting function, the present invention
The detecting function limitation is breached, provides the detecting function of magnetic and thermal signal；
(2) apply magnetic field, electric field and temperature field by situ, practical usage environment can be simulated, realized in multiple physical
Original position excitation magnetic/electricdomain overturns, introduces leakage current etc. under the excitation or effect of field, realizes original position, synchronizes, detects material in real time
The temperature of material and thermal conductivity distribution, domain structure and its Dynamic Evolution, thus can in situ, intuitively research material magnetic-
Coupling Rule and mechanism between heat.
Therefore, the present invention has expanded the function of scanning probe microscopy, the not only research of magneto-electric functional material and device
Advanced test platform is provided, so as to the power consumption to reduce micro-/nano parts, its stability is improved 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 nano magnetic heating in-situ detector the present invention is based on scanning probe microscopy
The overlooking the structure diagram of probe；
Fig. 2 is the enlarged drawing for having in Fig. 1 thermocouple structure probe tip；
Fig. 3 is that the schematic diagram in Fig. 1 with thermocouple structure probe tip is prepared using point discharge fusion method；
Fig. 4 is that have thermal resistance structure in the nano magnetic heating in-situ detector the present invention is based on scanning probe microscopy
Probe tip structure diagram；
Fig. 5 is a kind of preferred function knot of the nano magnetic heating in-situ detector the present invention is based on scanning probe microscopy
Structure schematic diagram.
Specific embodiment
The present invention is described in further detail below in conjunction with attached drawing, embodiment, it should be pointed out that implementation as described below
Example is intended to 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, 9- conductive layers, 10- magnetospheres.
In the present embodiment, the nano magnetic heating in-situ detector based on scanning probe microscopy includes scanning probe microscopy
Platform, probe, probe control unit, pattern and magnetic signal detection platform, thermal signal detection platform and center control are single
Member.
Probe control unit is used to drive or control probe to carry out displacement and/or vibration；
Pattern includes displacement or vibration signals collecting unit with magnetic signal detection platform, for receiving the displacement of probe letter
Number or vibration signal；
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 probe is heated, 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, receives the pattern, magnetic, heat of sample
The pattern, magnetic, thermal signal image of sample are obtained after 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 needle point ontology 3 with surface coating, surface coating by film 1,
One 4 surface of film covering film 25,25 surface of film covering film 36.Film 1 is conductive, film 25 has electricity
Insulating properties, film 36 have magnetism, and film 1 is different from the material of film 36；Also, film 1, film 25 and film
36 form thermocouple structure, i.e.,：In the tip location of needle point ontology 3, one 4 surface of film covering film 36, and needle point ontology 3
Remaining position 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, using dry etching, wet etching the methods of, such as gone 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 located between film one 4 and 36.
The material of film 1 is conductive metal Pt, and thickness 100nm, the material of film 25 is insulating layer Al2O3, thickness
For 200nm, the material of film 36 is magnetism 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
Into.During 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 by front-end amplifier with integrator,
Integrator is connected with high-voltage amplifier, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, forms 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 nano magnetic heating in-situ detector based on scanning probe microscopy, at room temperature to the magnetic 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, the film 36 on 2 surface of control probe tip and sample surfaces point contact or vibration point contact in scanning process,
Reflection signal is collected by photoelectricity four-quadrant detector, is then connected by front-end amplifier with integrator, integrator and height
Pressure amplifier is connected, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, forms closed-loop control, another way signal with
Delayer is connected, and delayer is connected with 1 ω (frequency multiplication chain) and 3 ω (frequency tripling channel) channel of lock-in amplifier,
Lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with computer, and sample is obtained after analyzing and processing
Topography signal image；
(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, Ran Houru
Step (1) is described, by front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier, backend amplifier, with
Computer is connected, and the magnetic signal image of sample is obtained after analyzing and 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 probe electric signal, and electric current flows into needle point 2 and it heated, needle point 2 and sample
Carry out heat exchange, the voltage signal in the calorifics circuit is made to change, acquires 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 and processing；
(6) according to step (2) described in horizontal direction, 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, nano magnetic heating in-situ detector and phase complete in embodiment 1 based on scanning probe microscopy
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 melts the film 36 of needle point point, 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, the 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 nano magnetic heating in-situ detector based on scanning probe microscopy at room temperature to the magnetic of sample, hot
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 of the nano magnetic heating in-situ detector based on scanning probe microscopy and embodiment 1
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, conductive layer 9 and magnetosphere 10；Thermal resistance material layer 8 is located at 3 surface of needle point ontology, and magnetosphere 10 is located at thermoelectricity
Hinder 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 magnetosphere is iron (Fe), cobalt (Co) or nickel
(Ni), thickness is 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 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 prepare magnetosphere 10 on 8 surface of thermal resistance material layer.
Using the above-mentioned nano magnetic heating in-situ detector based on scanning probe microscopy, at room temperature to the magnetic 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, the magnetosphere 10 on 2 surface of control probe tip and sample surfaces point contact or vibration point contact in scanning process,
Reflection signal is collected by photoelectricity four-quadrant detector, is then connected by front-end amplifier with integrator, integrator and height
Pressure amplifier is connected, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, forms closed-loop control, another way signal with
Delayer is connected, and delayer is connected with 1 ω (frequency multiplication chain) and 3 ω (frequency tripling channel) channel of lock-in amplifier,
Lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with computer, and sample is obtained after analyzing and processing
Topography signal image；
(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 magnetosphere 10 in face carries out length travel or vibration, displacement or vibration signals collecting list along the feature image that step (2) obtains
Member receives the length travel signal or vibration signal of probe tip, and reflection signal is collected by photoelectricity four-quadrant detector, then
As described in step (1), by front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier, backend amplifier,
It is connected with computer, the magnetic signal image of sample is obtained after analyzing and processing；
(4) piezoelectric actuator driving probe is back to the initial position described in step (2)；
(5) magnetosphere 10 on 2 surface of needle point is made to be in contact with sample surfaces；Current source, conductive layer 9, thermal resistance material layer 8
Form the electrothermal circuit being closed；Electric signal applying unit heats thermal resistance material layer 8, and then probe tip is added
Heat so that the temperature of probe tip is higher than the temperature of sample；Probe actuation unit driving probe tip is in contact with sample, sample
Heat exchange occurs, and then influence the temperature of thermal resistance material layer 8 with probe tip, due to thermal resistance effect so that thermal resistance material
The resistance value of the bed of material 8 changes, and acquires the signal, through delayer, lock-in amplifier and backend amplifier, is connected with computer
It connects, the thermal signal image of the position sample is obtained after analyzing and processing；
(6) according to step (2) described in horizontal direction, 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 4：
In the present embodiment, nano magnetic heating in-situ detector and phase basic in embodiment 1 based on scanning probe microscopy
Together, except that using the probe with thermal resistance structure.
In the structure, probe includes feeler arm and needle point.Needle point includes needle point ontology and the magnetosphere positioned at its surface,
Thermal resistance material layer is set apart from needle point certain intervals on feeler arm, that is, it is non-between thermal resistance material layer and magnetosphere to be electrically connected,
Conductive layer is arranged on thermal resistance material surface.
8 material of thermal resistance material layer is low-doped silicon, and thickness is 5 μm, and 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 magnetosphere is iron (Fe), cobalt (Co) or nickel
(Ni), thickness is 0.1 μm,.
Using the above-mentioned nano magnetic heating in-situ detector based on scanning probe microscopy, at room temperature to the magnetic 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, the magnetosphere on control probe tip surface and sample surfaces point contact or vibration point contact in scanning process, instead
It penetrates signal to collect by photoelectricity four-quadrant detector, be then connected by front-end amplifier with integrator, integrator and high pressure
Amplifier is connected, and the signal all the way of high-voltage amplifier feeds back to piezoelectric actuator, forms closed-loop control, another way signal is with prolonging
When device be connected, delayer is connected with 1 ω (frequency multiplication chain) and 3 ω (frequency tripling channel) channel of lock-in amplifier, lock
Phase amplifier is connected with backend amplifier, and backend amplifier is connected with computer, and the shape of sample is obtained after analyzing and processing
Looks signal pattern；
(3) piezoelectric actuator driving probe is back to the initial position described in step (2) and raises a spacing upwards
From being scanned again to sample surfaces according to the transversal orientation described in step (2), probe tip surface controlled in scanning process
The feature image that is obtained along step (2) of magnetosphere carry out length travel or vibration, displacement or vibration signals collecting unit connect
The length travel signal or vibration signal of probe tip are received, reflection signal is collected by photoelectricity four-quadrant detector, then as walked
Suddenly (1) is described, by front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier, backend amplifier, with meter
Calculation machine is connected, and the magnetic signal image of sample is obtained after analyzing and processing；
(4) piezoelectric actuator driving probe is back to the initial position described in step (2)；
(5) magnetosphere of needle surface is made to be in contact with sample surfaces；Current source, conductive layer, thermal resistance material layer are formed
The electrothermal circuit of closure；Electric signal applying unit heats thermal resistance material layer；Probe actuation unit drives probe displacement
To sample surfaces position, the magnetosphere of needle surface is made to be in contact with sample surfaces, with needle point heat exchange, heat occur for sample
Amount influences the temperature of thermal resistance material layer through air and magnetosphere, due to thermal resistance effect so that the resistance of thermal resistance material layer
Value changes, and acquires the signal, through delayer, lock-in amplifier and backend amplifier, is connected with computer, analyzing and processing
The thermal signal image of the position sample is obtained afterwards；
(6) according to step (2) described in horizontal direction, 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.
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 (13)
1. a kind of nano magnetic heating in-situ detector based on scanning probe microscopy, it is characterized in that：Including as follows：
(1) scanning probe microscopy platform, probe, probe control unit
Probe control unit：For driving or controlling probe to carry out displacement and/or vibration；
Probe：With magnetic, electric conductivity and thermal conductivity；
The probe includes feeler arm and needle point；
(2) pattern and magnetic signal detection platform
Including displacement or vibration signals collecting unit, for receiving the displacement signal of probe or vibration signal；
Probe carries out sample surfaces transversal orientation scanning from initial position, 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 to obtain
The topography signal of sample；
Then, probe is back to initial position and raises upwards after certain distance according to the transversal orientation to sample surfaces
It is scanned, probe tip is controlled to carry out length travel or vibration, displacement or vibration signal along topography profile in scanning process
Collecting unit receives the length travel signal or vibration signal of probe tip, and acquired analysis obtains the magnetic signal of sample；
(3) thermal signal detection platform
Including calorifics circuit and thermal signal collecting unit；
Electric signal is encouraged in the calorifics circuit by electric signal applying unit, which flows into probe and probe is added
Heat, probe carry out heat exchange with sample, the voltage signal in calorifics circuit are made to change, acquired analysis obtains the heat of sample
Signal；
(4) centralized control unit
For initializing system each unit, control system each unit receives the pattern, magnetic, thermal signal of sample, sample is obtained after analysis
Pattern, magnetic, the thermal signal image of product.
2. the nano magnetic heating in-situ detector based on scanning probe microscopy as described in claim 1, it is characterized in that：It is described
Probe control unit be the piezoelectric actuator being connected with feeler arm；
The displacement or vibration signals collecting unit include light source, photoelectricity four-quadrant detector and signal processor；
During working condition, sample is placed in scanning probe microscopy platform, and probe carries out displacement or shaken under piezoelectric actuator effect
Dynamic, light source irradiation feeler arm, reflection signal is collected by photoelectricity four-quadrant detector, then after signal processor processes with
Centralized control unit is connected.
3. the nano magnetic heating in-situ detector based on scanning probe microscopy as claimed in claim 2, it is characterized in that：It is described
Signal processor include front-end amplifier, integrator, high-voltage amplifier, delayer, lock-in amplifier and backend amplifier；Light
Electric four-quadrant detector is connected by front-end amplifier with integrator, and integrator is connected with high-voltage amplifier, high voltage amplifier
The signal all the way of device feeds back to piezoelectric actuator, forms closed-loop control, and another way signal is connected with delayer, delayer and lock
One frequency multiplication chain of phase amplifier is connected with frequency tripling channel channel, and lock-in amplifier is connected with backend amplifier, rear end
Amplifier is connected with control centre.
4. the nano magnetic heating in-situ detector based on scanning probe microscopy as described in claim 1, it is characterized in that：It is described
Thermal signal collecting unit include delayer, lock-in amplifier and backend amplifier.
5. the nano magnetic heating in-situ investigation based on scanning probe microscopy as described in any claim in Claims 1-4
Device, it is characterized in that：The needle point is made of needle point ontology with coating, and coating is by being covered in the thin of needle point body surface
The film three that film one, the film two of one surface of film covering, two surface of film cover forms；Film one is conductive, film
Two with electrical insulating property, film three with magnetism, film one is different from the material of film three；Also, film one, film two and thin
Film three forms thermocouple structure.
6. the nano magnetic heating in-situ detector based on scanning probe microscopy as claimed in claim 5, it is characterized in that：It is described
Film one, the thermocouple structure that forms of film two and film three obtained using 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 formed is obtained using 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, melts the film three of needle point point, exposes film two, and other position films three do not melt；
Step 3：The film two that removal step 2 is exposed exposes film one；
Step 4：Using the method for plated film, the material identical with film three is plated in step 2 extending part, makes film one and film three
It is connected at needle point tip position, forms thermocouple structure.
7. the nano magnetic heating 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) detection mode one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact, displacement or vibration signals collecting list are controlled in scanning process
Member receives the length travel signal or vibration signal of probe tip, analyzes to obtain the topography signal of sample through centralized control unit；
Then, probe is back to the initial position and raises certain distance upwards, according to the transversal orientation to sample
Product surface is scanned, and probe tip is controlled to carry out length travel or vibration along feature image in scanning process, displacement or is shaken
Dynamic signal gathering unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain sample through centralized control unit
Magnetic signal image；
(2) detection mode two：For detecting the thermal signal of 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 probe tip be in contact with sample surfaces, and electric signal applying unit applies electric signal, electric current to probe
It flows into probe tip and it is heated, probe tip carries out heat exchange with sample, sends out the voltage signal in calorifics circuit
Changing obtains the thermal signal of sample through thermal signal collecting unit, analyzes to obtain the thermal signal figure of sample through centralized control unit
Picture.
8. the nano magnetic heating in-situ investigation based on scanning probe microscopy as described in any claim in Claims 1-4
Device, it is characterized in that：The needle point includes needle point ontology, thermal resistance material layer, conductive layer and magnetosphere；Thermal resistance material
Layer is located at needle point body surface, and magnetosphere is located at thermal resistance material surface；Conductive layer is mutually electrically connected with thermal resistance material layer.
9. the nano magnetic heating in-situ detector based on scanning probe microscopy as claimed in claim 8, it is characterized in that：Including
The following two kinds detection mode：
(1) pattern one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact, displacement or vibration signals collecting list are controlled in scanning process
Member receives the length travel signal or vibration signal of probe tip, analyzes to obtain the topography signal of sample through centralized control unit；
Probe is back to the initial position and raises certain distance upwards, then according to the transversal orientation to sample
Surface is scanned, and probe tip is controlled to carry out length travel or vibration, displacement or vibration along feature image in scanning process
Signal gathering unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain sample through centralized control unit
Magnetic signal image；
(2) pattern two：For detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit is to thermal resistance material
The bed of material is heated, and then probe tip is heated so that the temperature of probe tip is different from the temperature of sample；Probe drives
Moving cell driving probe tip is in contact with sample, and with probe tip heat exchange occurs for sample, and then influences thermal resistance material
The temperature of layer, due to thermal resistance effect so that the resistance value of thermal resistance material layer changes, after the acquisition of thermal signal collecting unit
It is analyzed through centralized control unit, obtains the thermal signal image of sample.
10. the nano magnetic heating in-situ investigation based on scanning probe microscopy as described in any claim in Claims 1-4
Device, it is characterized in that：The needle point includes needle point ontology and the magnetosphere positioned at its surface, apart from needle point one on feeler arm
Surely thermal resistance material layer is arranged at intervals, conductive layer is mutually electrically connected with thermal resistance material layer.
11. the nano magnetic heating in-situ detector based on scanning probe microscopy as claimed in claim 10, it is characterized in that：Institute
5 μm~50 μm are divided between stating.
12. the nano magnetic heating in-situ detector based on scanning probe microscopy as claimed in claim 10, it is characterized in that：Packet
Include the following two kinds detection mode：
(1) pattern one：For detecting the surface topography of sample and magnetic signal
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, and probe tip and sample surfaces point contact, displacement or vibration signals collecting list are controlled in scanning process
Member receives the length travel signal or vibration signal of probe tip, analyzes to obtain the topography signal of sample through centralized control unit；
Probe is back to the initial position and raises certain distance upwards, then according to the transversal orientation to sample
Surface is scanned, and probe tip is controlled to carry out length travel or vibration, displacement or vibration along feature image in scanning process
Signal gathering unit receives the length travel signal or vibration signal of probe tip, analyzes to obtain sample through centralized control unit
Magnetic signal image；
(2) pattern two：For detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed circuit；Electric signal applying unit is to thermal resistance material
The bed of material is heated；Probe actuation unit driving probe tip is in contact with sample, and with probe tip heat exchange occurs for sample,
Heat influences the temperature of thermal resistance material layer through air or through probe wall, due to thermal resistance effect so that thermal resistance material layer
Resistance value change, analyzed after the acquisition of thermal signal collecting unit through centralized control unit, obtain the thermal signal figure of sample
Picture.
13. utilize the detection mode of the nano magnetic heating in-situ detector based on scanning probe microscopy described in claim 7
Original position, synchronization, the magnetic of real-time detection sample, hot property method, 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 puts, transversely sample surfaces is oriented with scanning, obtain the feature image of sample and magnetic signal image；
Step 2：Probe is moved to the initial position in step 1, and using above-mentioned detection mode two, step 1 is carried out to sample surfaces
Described in transversal orientation scanning, obtain 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 |
| CN110333372A (en) * | 2019-07-18 | 2019-10-15 | 中国科学院宁波材料技术与工程研究所 | A kind of magnetic scanning microscope probe and preparation method thereof |
| CN110646640B (en) * | 2019-10-09 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | Material micro/nano scale magnetocaloric signal detection method based on scanning probe microscope |
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