CN105510638A - Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe - Google Patents

Probe for scanning probe microscope, preparation method of the probe, and detection method of the probe Download PDF

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CN105510638A
CN105510638A CN201410493965.9A CN201410493965A CN105510638A CN 105510638 A CN105510638 A CN 105510638A CN 201410493965 A CN201410493965 A CN 201410493965A CN 105510638 A CN105510638 A CN 105510638A
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probe
sample
signal
conductive layer
electric signal
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CN105510638B (en
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李润伟
陈斌
刘宜伟
王保敏
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The invention provides a probe for a scanning probe microscope. The probe is formed by a probe arm and a probe point, wherein the probe point includes a probe point body, a thermal resistance material layer, a conducting layer or a magnetic conducting layer; and the conducting layer is connected with the thermal resistance material layer, and is used for detecting changes of the thermal resistance material resistance. The probe can be used for in-situ representation for magnetism-electricity-heat multi-parameter of multi-function materials so as to visually research the coupling rule and mechanism between electricity-heat, magnetism-heat and magnetism-electricity-heat of the materials in situ.

Description

Probe in a kind of scanning probe microscopy, its preparation method and detection method
Technical field
The present invention relates to a kind of probe of scanning probe microscopy, particularly relate to the coupling of a kind of many reference amounts microscope probe, its preparation method and detection method.
Background technology
Along with the develop rapidly of nanoscale science and technology, the measuring technique for nano material is arisen at the historic moment, wherein the most strikingly scanning probe microscopy (STM) technology.
Scanning probe microscopy (STM) technology is based on scanning tunnel microscope (SPM) base growth, there is spatial resolution high, can in the multiple environment such as vacuum, air, even solution the plurality of advantages such as alternating temperature work, be widely used in the research fields such as physics, chemistry, biology, electronics.Scanning probe microscopy studies corresponding properties of samples by the interaction force between detector probe to sample or physical quantity, comprise atomic force microscope, magnetic force microscopy, piezoelectric forces microscope, conduction force microscope etc. at present, in order to detect the physical parameter such as surface topography, domain structure (comprising domain structure, ferroelectric/piezoelectricity domain structure, conduction domain structure etc.), microcell conductance of sample.
Along with the miniaturization of electron device and integrated, device size and device pitch reached micro-/receive yardstick, its heating becomes restriction bottleneck highly integrated further with heat dissipation problem.Micro-/receive under yardstick and characterize the physical property relevant to heat, understanding the physical process of generating heat and dispel the heat has become the brand-new branch of in modern science of heat one-micro-/to receive yardstick science of heat.Micro-/receive under yardstick, the micromechanism of material and domain structure particularly important on the impact of thermal property, micro-crack, hole, crystal boundary and even domain wall all may have influence on the thermal property of material.For multi-iron material, the magnetic under outfield drives/electricdomain upset (or domain wall drift) and leakage current all can cause microcell to generate heat.
Up to now, although people have developed the microcell thermal imaging based on scanning probe microscopy, but utilize this technology to be merely able to obtain single calorifics information, still can not original position, obtain other physical property infomations synchronously, in real time, such as domain structure, ferroelectric/piezoelectricity domain structure, conduction domain structure etc., magnetic-Re, electricity-Re cannot being carried out, or magnetic-electricity-thermal coupling imaging, studying because which limit to understand the physical mechanism of heating in material and heat radiation deep.
Summary of the invention
The invention provides the probe in a kind of scanning probe microscopy, it has new structure, can original position, synchronous characterize micro-/ nano magnetic-Re, electricity-Re in real time, or magnetic-electricity-thermal behavior, realize many reference amounts scanning probe function.
In scanning probe microscopy provided by the invention, a kind of probe structure (is called the probe with thermocouple structure) as shown in Figure 1, 2, comprise feeler arm 1 and needle point 2, needle point 2 is made up of needle point body 3 and overlayer, overlayer by being positioned at the film 1 on needle point body 3 surface, the film 25 on film one surface, the film 36 on film two surface form; Film 1 has electric conductivity; Film 25 has electrical insulating property; Film 36 has magnetic and electric conductivity, or film 36 has electric conductivity; Film 1 is different from the material of film 36; Further, film 1, film 25 and film 36 form thermocouple structure, that is: at the most advanced and sophisticated position of needle point body, film 1 surface is film 36, and all the other positions except body tip, film 25 is between film 1 and film 36.
Described film 1 material is not limit, comprise a kind of material in the metal and semiconductor with excellent conductive performance or two or more combined materials, metal and its alloys such as such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), a kind of material in the semiconductor such as graphite, Graphene or two or more combined materials.
Described film 25 material is not limit, and comprises semiconductor, inorganic material or the organic material etc. with insulating property, such as zinc paste (ZnO), bismuth ferrite (BiFeO 3), cobalt acid lithium (LiCoO 2), nickel oxide (NiO), cobalt oxide (Co 2o 3), cupric oxide (Cu xo), silicon dioxide (SiO 2), silicon nitride (SiN x), titania (TiO 2), tantalum pentoxide (Ta 2o 5), niobium pentaoxide (Nb 2o 5), tungsten oxide (WO x), hafnium oxide (HfO 2), aluminium oxide (Al 2o 3), carbon nano-tube, Graphene, graphene oxide, amorphous carbon, copper sulfide (Cu xs), silver sulfide (Ag 2s), a kind of material not in alkali (PA), polysulfones (PS) etc. of amorphous silicon, titanium nitride (TiN), polyimide (PI), polyamide (PAI), poly-west or two or more combined materials.
When described film 36 has electric conductivity, its material is not limit, and comprises a kind of material in the metal and semiconductor with excellent conductive performance or two or more combined materials.The described metal with excellent conductive performance and semiconductor include but not limited to metal and its alloys such as bismuth, nickel, cobalt, potassium, a kind of material in the semiconductor such as graphite, Graphene or two or more combined materials.
When described film 36 has magnetic and electric conductivity, its material is not limit, comprise and there is ferromagnetic metal and alloy materials etc., such as, a kind of material in the materials such as metallic iron (Fe), cobalt (Co), nickel (Ni) and magnetic alloy or two or more combined materials.
The described probe with thermocouple structure can adopt following preparation method to obtain:
The method of step 1, employing plated film prepares film 1 at needle point body surface;
The method of step 2, employing plated film prepares film 25 on the surface of film 1;
Step 3, the film 25 adopting the method removing needle point body tip of etching to locate, expose film 1;
Step 4, film one surface adopting the method for plated film to expose described in step 3 prepare film 36, film 1 is connected at the most advanced and sophisticated position of needle point with film 36, forms thermocouple structure.
In above-mentioned preparation method, the method for the plated film in described step 1,2,4 includes but not limited to the one or more kinds of combinations in the method such as various solution spin coating method, inkjet printing, solid sputtering, thermal evaporation, electron beam evaporation; The method except the most advanced and sophisticated film two of needle point in described step 3 includes but not limited to the methods such as dry quarter, wet etching, such as ion etching, reactive ion etching, chemical etching etc.
As shown in Figure 3, the described probe with thermocouple structure can also adopt following another kind of preparation method to obtain:
The method of step 1, employing plated film, prepares film 1, film 25 and film 36 successively on needle point body 3 surface;
Step 2, between film 36 and electrode layer 7, apply voltage, utilize point discharge principle, by regulating film 36 and the spacing of electrode layer 7, making film 36 melting of needle point point, expose film 25, and other position films 36 not having melting;
Step 3: the film 25 exposed described in removal step 2, exposes film 1;
Step 4: the method adopting plated film, at the material that the plating of described extending part is identical with film 36, makes film 1 be connected at the most advanced and sophisticated position of needle point with film 36, forms thermocouple structure.
In above-mentioned preparation method, the method for the plated film in described step 1,4 includes but not limited to the one or more kinds of combinations in the methods such as the sputtering of various solution spin coating method, inkjet printing, solid, thermal evaporation or electron beam evaporation.
Scanning probe microscopy of the present invention comprise scanning probe microscopy platform, probe, for driving or controlling the probe control unit that probe carries out displacement and/or vibration, and signal (comprising displacement and/or vibration, thermal and magnetic, electric signal) collection analysis unit.
When adopting the present invention to have the probe of thermocouple structure, the mode of operation of scanning probe microscopy is as follows:
(1) film three described in has electric conductivity
Described scanning probe microscopy also comprises electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, probe actuation unit, and centralized control unit,
Described probe control unit is used for driving or control probe and carries out displacement and/or vibration;
Described centralized control unit is used for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, heat, electric signal image after analysis;
The mode of operation of described scanning probe microscopy comprises the following two kinds, is respectively used to the pattern of detection sample, electric signal and thermal signal:
(1) pattern one: for detecting surface topography and the electric signal of sample
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, electric signal applying unit, film one, film three and sample form closed electrical return simultaneously; Displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis; Meanwhile, electric signal applying unit applies electric signal to needle point, and this electric signal flows into film one, film three and sample, and coating-forming voltage signal, obtains the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
(2) pattern two: for detecting the thermal signal of sample
Electric signal applying unit, film one, film three form closed electrothermal circuit; Probe actuation unit drives probe displacement is to sample surfaces position, needle point is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, electric current flows into needle point and heats it, needle point and sample carry out heat interchange, make to produce voltage signal in calorifics loop, obtain the thermal signal of sample through thermal signals collecting unit, obtain the thermal signal image of sample through centralized control unit analysis.
When utilizing above-mentioned scanning probe microscopy can carry out heat-electric in-situ investigation to sample to sample, detection method is as follows:
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the electric signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample.
(2) film three described in has magnetic and electric conductivity
Described scanning probe microscopy also comprises electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collecting unit, probe actuation unit, and centralized control unit,
Described probe control unit is used for driving or control probe and carries out displacement and/or vibration;
Described centralized control unit is used for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, magnetic, heat, electric signal image after analysis;
The mode of operation of described scanning probe microscopy comprises following three kinds, is respectively used to detect the pattern of sample, magnetic number, electric signal and thermal signal:
(1) pattern one: for detecting surface topography and the magnetic signal of sample
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis;
Probe is back to described initial position and upwards raises certain distance, then according to described transversal orientation, sample surfaces is scanned, control probe tip in scanning process and carry out length travel or vibration along described feature image, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the magnetic signal image of sample through centralized control unit analysis;
(2) pattern two: for detecting the thermal signal of sample
Electric signal applying unit, film one, film three form closed electrothermal circuit; Probe actuation unit drives probe displacement is to sample surfaces position, needle point is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, electric current flows into needle point and heats it, needle point and sample carry out heat interchange, make to produce voltage signal in calorifics loop, obtain the thermal signal of sample through thermal signals collecting unit, obtain the thermal signal image of sample through centralized control unit analysis;
(3) pattern three: for detecting the electric signal of sample
Electric signal applying unit, film one, film three and sample form closed electrical return; Probe actuation unit drives probe displacement is to sample surfaces position, needle surface is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, this electric signal flows into film one, film three and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
When utilizing above-mentioned scanning probe microscopy can carry out magnetic-Re-electric in-situ investigation to sample to sample, detection method is as follows:
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the magnetic signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Step 3: the initial position in probe displacement to step 1, adopts above-mentioned detection mode three, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the electric signal image of sample.
The invention allows for another kind of preferred probe structure (being called the probe with thermal resistance structure).In this structure, as shown in Figure 1, probe comprises feeler arm 1 and needle point 2.Needle point 2 as shown in Figure 4, comprises needle point body 3, thermal resistance material layer 8, first conductive layer 9 and the second conductive layer 10; Thermal resistance material layer 8 is positioned at needle point body 3 surface, and the second conductive layer 10 is positioned at thermal resistance material surface; First conductive layer 9 is connected with thermal resistance material layer 8; Thermal resistance material layer 8 is made up of thermal resistance material, for detecting sample temperature change and thermal conductance; First conductive layer 9 is made up of conductive material, is connected with thermal resistance material, for detecting the change of thermal resistance material resistance; Second conductive layer 10 is made up of conductive material, or further, the second conductive layer 10 is made up of magnetic conductive material, namely defines magnetic conductive layer.
Described thermal resistance material layer 8 material is not limit, and comprises and has low-doped silicon, semiconductor or metallic resistance material etc.
The first described conductive layer 9 material is not limit, comprise a kind of material in the metal, semiconductor etc. with excellent conductive performance or two or more combined materials, such as, metal and its alloy, a kind of material in the semiconductor such as graphite, Graphene or the combinations of two or more material such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K).
When the second described conductive layer 10 is made up of conductive material, material is not limit, comprise a kind of material in the metal and semiconductor with excellent conductive performance or two or more combined materials, metal and its alloy, a kind of material in the semiconductor such as graphite, Graphene or the combinations of two or more material such as such as bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K).
When the second described conductive layer 10 is made up of magnetic conductive material, material is not limit, and comprises ferromagnetic metal or ferromagnetic alloy etc., and ferromagnetic metal comprises iron (Fe), cobalt (Co), nickel (Ni) etc.
The described probe with thermal resistance structure can adopt following preparation method to obtain:
The method of step 1, employing plated film prepares thermal resistance material layer 8 at needle point body surface;
The method of step 2, employing plated film prepares the first conductive layer 9 at needle point body surface;
The method of step 3, employing plated film is at thermal resistance material layer 8 surface preparation the second conductive layer 10.
In above-mentioned preparation method, the method for the plated film in described step 1,2,3 includes but not limited to the one or more kinds of combinations in the method such as various solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporation.
As preferably, the thickness of described thermal resistance material layer 8 is 0.1 μm ~ 10 μm.
As preferably, the thickness of the first described conductive layer 9 is 0.1 μm ~ 1 μm.
When adopting the present invention to have the probe of thermal resistance structure, the mode of operation of scanning probe microscopy is as follows:
(1) when the second described conductive layer is made up of conductive material, when having electric conductivity
Described scanning probe microscopy also comprises electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, probe actuation unit, and centralized control unit,
Described probe control unit is used for driving or control probe and carries out displacement and/or vibration;
Described centralized control unit is used for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, heat, electric signal image after analysis;
The mode of operation of described scanning probe microscopy comprises the following two kinds, is respectively used to the pattern of detection sample, electric signal and thermal signal:
(1) pattern one: for detecting surface topography and the electric signal of sample
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, electric signal applying unit, the first conductive layer, thermal resistance material layer and the second conductive layer form closed electrical return simultaneously; Displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis; Simultaneously, electric signal applying unit applies electric signal to needle point, and this electric signal flows into the first conductive layer, thermal resistance material layer, the second conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis;
(2) pattern two: for detecting the thermal signal of sample
Electric signal applying unit, the first conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer, and then heats probe tip, makes the temperature of probe tip be different from the temperature (the general temperature selected higher than sample) of sample; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample.
When utilizing above-mentioned scanning probe microscopy can carry out heat-electric in-situ investigation to sample to sample, detection method is as follows:
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the electric signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample.
In thermal resistance structure described in above-mentioned (one), thermal resistance material layer and the second conductive layer are stacked arrangement at the most advanced and sophisticated position of needle point body, consider in actual fabrication process, because the tip location xsect of needle point body is less, therefore overlayer preparation difficulty, more difficult when especially preparing this multilayer laminate constructions, therefore as preferably, the second described conductive layer is integrated in thermal resistance material layer.
As another kind of preferred structure, arrange insulation course between described resistance elements and the second conductive layer, make resistance elements and the second conductive layer phase electrical isolation, the first described conductive layer and the second conductive layer are electrically connected.In this structure, when adopting above-mentioned pattern one to detect the electric signal of sample, electric signal applying unit, the first conductive layer and the second conductive layer form closed electrical return, electric signal applying unit applies electric signal to needle point, this electric signal flows into the first conductive layer, the second conductive layer and sample, coating-forming voltage signal, obtains the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
(2) when the second described conductive layer is made up of magnetic conductive material, when having magnetic and electric conductivity
Described scanning probe microscopy also comprises electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collecting unit, probe actuation unit, and centralized control unit,
Described probe control unit is used for driving or control probe and carries out displacement and/or vibration;
Described centralized control unit is used for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, magnetic, heat, electric signal image after analysis;
The mode of operation of described scanning probe microscopy comprises following three kinds, is respectively used to detect the pattern of sample, magnetic number, electric signal and thermal signal:
(1) pattern one: for detecting surface topography and the magnetic signal of sample
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis;
Probe is back to described initial position and upwards raises certain distance, then according to described transversal orientation, sample surfaces is scanned, control probe tip in scanning process and carry out length travel or vibration along described feature image, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the magnetic signal image of sample through centralized control unit analysis;
(2) pattern two: for detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer, and then heats probe tip, makes the temperature of probe tip be different from the temperature (the general temperature selected higher than sample) of sample; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample;
(3) pattern three: for detecting the electric signal of sample
Electric signal applying unit, conductive layer, thermoelectricity resistance layer, magnetic conductive layer and sample form closed electrical return; Probe actuation unit drives probe displacement is to sample surfaces position, probe tip is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, this electric signal streams is through conductive layer, thermal resistance material layer, magnetic conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
When utilizing above-mentioned scanning probe microscopy can carry out magnetic-Re-electric in-situ investigation to sample to sample, detection method is as follows:
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the magnetic signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Step 3: the initial position in probe displacement to step 1, adopts above-mentioned detection mode three, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the electric signal image of sample.
In thermal resistance structure described in above-mentioned (two), thermal resistance material layer 8 and magnetic conductive layer 10 are multilayer laminated arrangement at the most advanced and sophisticated position of needle point body, consider in actual fabrication process, because the tip location xsect of needle point body is less, therefore overlayer preparation difficulty, more difficult when especially preparing this multilayer laminate constructions; On the other hand, in this multilayer laminate constructions, the tip location of needle point body has concentrated the detection of magnetic signal, thermal signal and electric signal, and the damage of thin film can cause whole probe destruction, and utilization factor is not high.
For this reason, the present invention improves this stepped construction, thermal resistance material layer and conductive layer are arranged on probe wall position, and only magnetic conductive layer is arranged on probe tip position, carry out " separation " with thermal resistance material layer, conductive layer by magnetic conductive, this structure is specially: probe comprises feeler arm and needle point; Needle point comprises needle point body and the magnetic conductive being positioned at its surface, and on feeler arm, distance needle point certain intervals arranges thermal resistance material layer, that is, non-electric connection between thermal resistance material layer and magnetic conductive; Described needle point also comprises conductive layer, conductive layer and thermal resistance material layer phase electric connection, and conductive layer and magnetic conductive layer phase electric connection.As preferably, conductive layer is arranged on thermal resistance material surface, its one end and magnetic conductive layer phase electric connection.
When adopting the thermal resistance structure probe of above-mentioned improvement, the mode of operation of described scanning probe microscopy comprises following three kinds, is respectively used to detect the pattern of sample, magnetic number, electric signal and thermal signal:
(1) pattern one: for detecting surface topography and the magnetic signal of sample
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis;
Probe is back to described initial position and upwards raises certain distance, then according to described transversal orientation, sample surfaces is scanned, control probe tip in scanning process and carry out length travel or vibration along described feature image, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the magnetic signal image of sample through centralized control unit analysis;
(2) pattern two: for detecting the thermal signal of sample
Electric signal applying unit, conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, its heat has influence on the temperature of thermal resistance material layer through air and probe wall, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample;
(3) pattern three: for detecting the electric signal of sample
Electric signal applying unit, conductive layer, magnetic conductive layer and sample form closed electrical return; Probe actuation unit drives probe displacement is to sample surfaces position, probe tip is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, this electric signal streams is through conductive layer, magnetic conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
When adopting the thermal resistance structure probe of above-mentioned improvement, when scanning probe microscopy can carry out magnetic-Re-electric in-situ investigation to sample to sample, detection method comprises the steps:
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the magnetic signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Step 3: the initial position in probe displacement to step 1, adopts above-mentioned detection mode three, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the electric signal image of sample.
Present invention also offers a kind of preferred probe control unit structure, as shown in Figure 5, this probe control unit is the piezoelectric actuator be connected with probe.Now, described displacement signal acquisition unit comprises light source, photoelectricity four-quadrant detector and signal processor; During duty, sample is placed in scanning probe microscopy platform, and probe vibrates under piezoelectric actuator effect, light source irradiation feeler arm, reflected signal is collected by photoelectricity four-quadrant detector, is then connected with centralized control unit after signal processor processes.
As a kind of implementation, as shown in Figure 5, described signal processor comprises front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier and backend amplifier.Photoelectricity four-quadrant detector is connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, and lock-in amplifier is connected with backend amplifier, and backend amplifier is connected with control center.
As a kind of implementation, as shown in Figure 5, described thermal signal collecting unit comprises chronotron, lock-in amplifier and backend amplifier.
In sum, the invention provides the probe of two kinds of new structures for scanning probe microscopy, one is thermal resistance structure, another kind is thermocouple structure, utilize this probe can to the pattern of multifunctional material, magnetic signal and thermal signal carry out original position, synchronously, real-time detection, or to the pattern of multifunctional material, electric signal and thermal signal carry out original position, synchronously, real-time detection, even to the pattern of multifunctional material, magnetic signal, thermal signal and electric signal carry out original position, synchronously, real-time detection, thus achieve magnetic-electricity-Re many reference amounts in-situ characterization, can original position, electricity-the Re of research material intuitively, magnetic-Re, and the Coupling Rule between magnetic-electricity-Re is with machine-processed.
Accompanying drawing explanation
Fig. 1 is the plan structure schematic diagram of the probe of scanning probe microscopy of the present invention;
Fig. 2 is the structural representation that the present invention has the probe tip of thermocouple structure;
Fig. 3 adopts point discharge fusion method to prepare in Fig. 1 the schematic diagram with thermocouple structure probe tip;
Fig. 4 is the structural representation that the present invention has the probe tip of thermocouple structure;
Fig. 5 is the preferred illustrative view of functional configuration of one of scanning probe microscopy of the present invention.
Embodiment
Below in conjunction with accompanying drawing, embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Wherein: 1-feeler arm, 2-needle point, 3-needle point body, 4-film one, 5-film two, 6-film three, 7-electrode layer, 8-thermal resistance material layer, 9-first conductive layer, 10-second conductive layer.
Embodiment 1:
In the present embodiment, scanning probe microscopy comprises scanning probe microscopy platform, probe, electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collection unit and centralized control unit.Probe control unit is used for driving or control probe and carries out displacement and/or vibration.Centralized control unit: for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, heat, electric signal image after analysis;
As shown in Figure 1, probe comprises feeler arm 1 and needle point 2.
As shown in Figure 2, be made up of needle point body 3 and surface coating, surface coating is by film 1, film 1 surface coverage film 25, film 25 surface coverage film 36 for the structure of needle point 2.Film 1 has electric conductivity, film 25 has electrical insulating property, film 36 has electric conductivity, and film 1 is different from the material of film 36; Further, film 1, film 25 and film 36 form thermocouple structure, that is: in the tip location of needle point body 3, film 1 surface coverage film 36, and needle point body 3 all the other positions except tip, film 25 is between film 1 and film 36.
This probe tip with thermocouple structure can be adopted and prepare with the following method, and the method comprises the steps:
The method of step 1, employing plated film, the methods such as such as solution spin coating method, inkjet printing, solid sputtering, thermal evaporation, person's electron beam evaporation prepare film 1 on needle point body 3 surface;
The method of step 2, employing plated film, the methods such as such as solution spin coating method, inkjet printing, solid sputtering, thermal evaporation, person's electron beam evaporation prepare film 25 on needle point body 3 surface;
The methods such as step 3, employing dry quarter, wet etching, the methods such as such as ion etching, reactive ion etching, chemical etching remove the film 25 at needle point body 3 tip place, expose film 1;
The method of step 4, employing plated film, the methods such as such as solution spin coating method, inkjet printing, solid sputtering, thermal evaporation, person's electron beam evaporation prepare film 36 on needle point body 3 surface, make the film 1 surface coverage film 36 at needle point body 3 tip place, all the other positions except tip, film 25 is between film one 4 and 36.
The material of film 1 is conducting metal Pt, and thickness is 100nm, and the material of film 25 is insulation course Al 2o 3, thickness is 200nm, and the material of film 36 is magnetic conductive W metal, and thickness is 100nm.
Probe control unit adopts the piezoelectric actuator be connected with probe.The MFP-3D-SA-SCANNER scanner that this piezoelectric actuator selects AsylumResearch company of the U.S. to produce, sweep limit X × Y=90 × 90 μm 2.
As shown in Figure 5, displacement or vibration signals collecting unit comprise light source, photoelectricity four-quadrant detector and signal processor.Signal processor is made up of front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier and backend amplifier.During duty, sample is placed in scanning probe microscopy platform, probe vibrates under piezoelectric actuator effect, light source irradiation feeler arm, reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with control center.
Control center is made up of computing machine, initialization module, control module.
Thermal signal collecting unit is made up of chronotron, lock-in amplifier and backend amplifier.Electrical signal collection unit is made up of chronotron, lock-in amplifier and backend amplifier.In the present embodiment, this thermal signal collecting unit, electrical signal collection unit and signal processor carry out integrated.
Electric signal applying unit in calorifics loop is current source.
Electrical return is voltage source by electric signal applying unit.
In the present embodiment, the Fe film selecting growth on ferroelectric substrate PMN-PT is study sample, and the thickness of this sample is 90nm.
Utilize above-mentioned scanning probe microscopy at room temperature to carry out original position, synchronous, real-time detection to the thermoelectricity capability of sample, detection method is as follows:
(1) sample is fixed on scanning probe microscopy platform, by each unit initial parameter of initialization module initialization system;
(2) under control module effect, piezoelectric actuator drives probe displacement to sample surfaces initial position, light source irradiation feeler arm, and reflected signal is collected by photoelectricity four-quadrant detector; Probe transversely carries out directional scanning to sample surfaces from this initial position, and the film 36 controlling probe tip 2 surface in scanning process contacts with sample surfaces point cantact or oscillation point; Meanwhile, current source, film 1, film 36 and sample form closed electrical return;
Reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with computing machine, obtains the topography signal image of sample by analysis after process; Simultaneously, current source applies electric signal to probe, after this electric signal flows into film 1, film 36 and sample, flow into the earth, coating-forming voltage signal, gathers this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the electric signal image of this position sample;
(3) piezoelectric actuator drives probe be back to the initial position described in step (2) and upwards raise certain distance, according to the transversal orientation described in step (2), sample surfaces is scanned again, the feature image that the film 36 controlling probe tip 2 surface in scanning process obtains along step (2) carries out length travel or vibration, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, reflected signal is collected by photoelectricity four-quadrant detector, then as described in step (1), pass through front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier, backend amplifier, be connected with computing machine, the electric signal image of sample is obtained by analysis after process,
(4) piezoelectric actuator drives probe to be back to the initial position described in step (2);
(5) film 36 on needle point 2 surface is made to contact with sample surfaces; Current source, film 1 and film 36 form closed electrothermal circuit; Current source applies electric signal to probe, electric current flows into needle point 2 and heats it, needle point 2 and sample carry out heat interchange, voltage signal in this calorifics loop is changed, gather this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the thermal signal image of this position sample;
(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 complete to sample surfaces point by point scanning according to the horizontal direction described in step (2).
Embodiment 2:
In the present embodiment, scanning probe microscopy structure is identical with embodiment 1.
Difference is that probe tip that this has thermocouple structure is adopted and alternatively prepared, and the method comprises the steps:
The method of step 1, employing plated film, prepares film 1, film 25 and film 36 successively on needle point body 3 surface;
Step 2, between film 36 and electrode layer 7, apply voltage, utilize point discharge principle, by regulating film 36 and the spacing of electrode layer 7, making film 36 melting of needle point point, expose film 25, and other position films 36 not having melting;
Step 3: the film 25 exposed described in removal step 2, exposes film 1;
Step 4: the method adopting plated film, at the material that the plating of described extending part is identical with film 36, makes film 1 be connected at the most advanced and sophisticated position of needle point with film 36, forms thermocouple structure.
Utilize this scanning probe microscopy at room temperature to the electricity of sample, thermal behavior carries out original position, method that is synchronous, real-time detection is identical with embodiment 1.
Embodiment 3:
In the present embodiment, scanning probe microscopy structure is substantially identical with embodiment 1, and difference adopts the probe with thermal resistance structure.
As shown in Figure 1, this probe comprises feeler arm 1 and needle point 2.Needle point 2 as shown in Figure 4, comprises needle point body 3, thermal resistance material layer 8, first conductive layer 9 and the second conductive layer 10; Thermal resistance material layer 8 is positioned at needle point body 3 surface, and the second conductive layer 10 is positioned at thermal resistance material surface; First conductive layer 9 and thermal resistance material layer 8 phase electric connection.
Thermal resistance material layer 8 material is low-doped silicon, thickness is 2m, conductive layer 9 material is the one in bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), graphite, Graphene, thickness is 1 μm, second conductive layer 10 material is the one in bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), graphite, Graphene, and thickness is 0.1 μm.
The preparation method of above-mentioned probe is as follows:
The method of the plated film such as step 1, employing solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporation prepares thermal resistance material layer 8 at needle point body surface;
The method of the plated film such as step 2, employing solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporation prepares the first conductive layer 9 at needle point body surface, and this conductive layer is connected with thermal resistance material layer 8;
The method of the plated film such as step 3, employing solution spin coating method, inkjet printing, etching, solid sputtering, thermal evaporation, electron beam evaporation is at thermal resistance material layer 8 surface preparation the second conductive layer 10.
Utilize above-mentioned scanning probe microscopy at room temperature to the electricity of sample, thermal behavior carries out original position, method that is synchronous, real-time detection is as follows:
(1) sample is fixed on scanning probe microscopy platform, by each unit initial parameter of initialization module initialization system;
(2) under control module effect, piezoelectric actuator drives probe displacement to sample surfaces initial position, light source irradiation feeler arm, and reflected signal is collected by photoelectricity four-quadrant detector; Probe transversely carries out directional scanning to sample surfaces from this initial position, and the second conductive layer 10 controlling probe tip 2 surface in scanning process contacts with sample surfaces point cantact or oscillation point; Meanwhile, current source, the first conductive layer 9, thermal resistance material layer 8, second conductive layer 10 and sample form closed electrical return;
Reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with computing machine, obtains the topography signal image of sample by analysis after process; Simultaneously, current source applies electric signal to probe, after this electric signal flows into the first conductive layer 9, thermal resistance material layer 8, second conductive layer 10 and sample, flow into the earth, coating-forming voltage signal, gathers this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the electric signal image of this position sample;
(3) piezoelectric actuator drives probe to be back to the initial position described in step (2);
(4) second conductive layer 10 on needle point 2 surface is made to contact with sample surfaces; Current source, the first conductive layer 9 and thermal resistance material layer 8 form closed electrothermal circuit; Electric signal applying unit heats thermal resistance material layer 8, and then heats probe tip, makes the temperature of temperature higher than sample of probe tip; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer 8, due to thermal resistance effect, the resistance value of thermal resistance material layer 8 is changed, gathers this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the thermal signal image of this position sample;
(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 complete to sample surfaces point by point scanning according to the horizontal direction described in step (2).
Embodiment 4:
In the present embodiment, scanning probe microscopy device is substantially identical with embodiment 3, and difference is that the second conductive layer 10 is integrated in thermal resistance material layer 8.
Embodiment 5:
In the present embodiment, scanning probe microscopy device is substantially the same manner as Example 1, and difference utilizes above-mentioned scanning probe microscopy device at room temperature to carry out original position, synchronous, real-time detection to the magnetic of sample, heat, electrical property, and detection method is as follows:
(1) sample is fixed on scanning probe microscopy platform, by each unit initial parameter of initialization module initialization system;
(2) under control module effect, piezoelectric actuator drives probe displacement to sample surfaces initial position, light source irradiation feeler arm, and reflected signal is collected by photoelectricity four-quadrant detector, probe transversely carries out directional scanning to sample surfaces from this initial position, the film 36 controlling probe tip 2 surface in scanning process contacts with sample surfaces point cantact or oscillation point, reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with computing machine, the topography signal image of sample is obtained by analysis after process,
(3) piezoelectric actuator drives probe be back to the initial position described in step (2) and upwards raise certain distance, according to the transversal orientation described in step (2), sample surfaces is scanned again, the feature image that the film 36 controlling probe tip 2 surface in scanning process obtains along step (2) carries out length travel or vibration, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, reflected signal is collected by photoelectricity four-quadrant detector, then as described in step (1), pass through front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier, backend amplifier, be connected with computing machine, the magnetic signal image of sample is obtained by analysis after process,
(4) piezoelectric actuator drives probe to be back to the initial position described in step (2);
(5) film 36 on needle point 2 surface is made to contact with sample surfaces; Current source, film 1 and film 36 form closed electrothermal circuit; Current source applies electric signal to probe, electric current flows into needle point 2 and heats it, needle point 2 and sample carry out heat interchange, voltage signal in this calorifics loop is changed, gather this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the thermal signal image of this position sample;
(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 complete to sample surfaces point by point scanning according to the horizontal direction described in step (2);
(8) piezoelectric actuator drives probe to be back to the initial position described in step (2), and the film 36 on needle point 2 surface is contacted with sample surfaces;
(9) current source, film 1, film 36 and sample form closed electrical return; Current source applies electric signal to probe, after this electric signal flows into film 1, film 36 and sample, flow into the earth, coating-forming voltage signal, gather this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the electric signal image of this position sample;
(10) according to the horizontal direction described in step (2), piezoelectric actuator drives probe to the next position;
(11) every bit repeats step (8) and (9), until complete to sample surfaces point by point scanning according to the horizontal direction described in step (2).
Embodiment 6:
In the present embodiment, scanning probe microscopy device is substantially the same manner as Example 3, and difference is the second conductive layer 10 material is iron (Fe), cobalt (Co) or nickel (Ni).
Utilize above-mentioned scanning probe microscopy device at room temperature to carry out original position, synchronous, real-time detection to the magnetic of sample, heat, electrical property, detection method is as follows:
(1) sample is fixed on scanning probe microscopy platform, by each unit initial parameter of initialization module initialization system;
(2) under control module effect, piezoelectric actuator drives probe displacement to sample surfaces initial position, light source irradiation feeler arm, and reflected signal is collected by photoelectricity four-quadrant detector, probe transversely carries out directional scanning to sample surfaces from this initial position, the second conductive layer 10 controlling probe tip 2 surface in scanning process contacts with sample surfaces point cantact or oscillation point, reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with computing machine, the topography signal image of sample is obtained by analysis after process,
(3) piezoelectric actuator drives probe be back to the initial position described in step (2) and upwards raise certain distance, according to the transversal orientation described in step (2), sample surfaces is scanned again, the feature image that the second conductive layer 10 controlling probe tip 2 surface in scanning process obtains along step (2) carries out length travel or vibration, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, reflected signal is collected by photoelectricity four-quadrant detector, then as described in step (1), pass through front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier, backend amplifier, be connected with computing machine, the magnetic signal image of sample is obtained by analysis after process,
(4) piezoelectric actuator drives probe to be back to the initial position described in step (2);
(5) second conductive layer 10 on needle point 2 surface is made to contact with sample surfaces; Current source, the first conductive layer 9, thermal resistance material layer 8 form closed electrothermal circuit; Electric signal applying unit heats thermal resistance material layer 8, and then heats probe tip, makes the temperature of temperature higher than sample of probe tip; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer 8, due to thermal resistance effect, the resistance value of thermal resistance material layer 8 is changed, gathers this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the thermal signal image of this position sample;
(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 complete to sample surfaces point by point scanning according to the horizontal direction described in step (2);
(8) piezoelectric actuator drives probe to be back to the initial position described in step (2), and second conductive layer 10 on needle point 2 surface is contacted with sample surfaces;
(9) current source, the second conductive layer 10, thermoelectricity resistance layer 8, first conductive layer 9 and sample form closed electrical return; Current source applies electric signal to probe, this electric signal flows into conductive layer 9, after the second conductive layer 10 and sample, flow into the earth, coating-forming voltage signal, gathers this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the electric signal image of this position sample;
(10) according to the horizontal direction described in step (2), piezoelectric actuator drives probe to the next position;
(11) every bit repeats step (8) and (9), until complete to sample surfaces point by point scanning according to the horizontal direction described in step (2).
Embodiment 7:
In the present embodiment, scanning probe microscopy structure is substantially identical with embodiment 1, and difference adopts the probe with thermal resistance structure.
In this structure, probe comprises feeler arm and needle point.Needle point comprises needle point body and the magnetic conductive layer being positioned at its surface, on feeler arm, distance needle point certain intervals arranges thermal resistance material layer, that is, non-electric connection between thermal resistance material layer and magnetic conductive, conductive layer is arranged on thermal resistance material surface, its one end and magnetic conductive phase electric connection.
Thermal resistance material layer 8 material is low-doped silicon, thickness is 5 μm, conductive layer 9 material is the one in bismuth (Bi), nickel (Ni), cobalt (Co), potassium (K), graphite, Graphene, thickness is 1 μm, magnetic conductive 10 material is iron (Fe), cobalt (Co) or nickel (Ni), thickness is 0.1 μm.
Utilize above-mentioned nano magnetic-electricity-Re many reference amounts coupling in-situ detecting system, at room temperature to magnetic, the heat of sample, electrical property carries out original position, method that is synchronous, real-time detection is as follows:
(1) sample is fixed on scanning probe microscopy platform, by each unit initial parameter of initialization module initialization system;
(2) under control module effect, piezoelectric actuator drives probe displacement to sample surfaces initial position, light source irradiation feeler arm, and reflected signal is collected by photoelectricity four-quadrant detector, probe transversely carries out directional scanning to sample surfaces from this initial position, the magnetic conductive layer controlling probe tip surface in scanning process contacts with sample surfaces point cantact or oscillation point, reflected signal is collected by photoelectricity four-quadrant detector, then be connected with integrator by front-end amplifier, integrator is connected with high-voltage amplifier, one tunnel signal feedback of high-voltage amplifier is to piezoelectric actuator, form closed-loop control, another road signal is connected with chronotron, chronotron is connected with 3 ω (frequency tripling passage) passage with 1 ω (frequency multiplication chain) of lock-in amplifier, lock-in amplifier is connected with backend amplifier, backend amplifier is connected with computing machine, the topography signal image of sample is obtained by analysis after process,
(3) piezoelectric actuator drives probe be back to the initial position described in step (2) and upwards raise certain distance, according to the transversal orientation described in step (2), sample surfaces is scanned again, the feature image that the magnetic conductive layer controlling probe tip surface in scanning process obtains along step (2) carries out length travel or vibration, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, reflected signal is collected by photoelectricity four-quadrant detector, then as described in step (1), pass through front-end amplifier, integrator, high-voltage amplifier, chronotron, lock-in amplifier, backend amplifier, be connected with computing machine, the magnetic signal image of sample is obtained by analysis after process,
(4) piezoelectric actuator drives probe to be back to the initial position described in step (2);
(5) magnetic conductive of needle surface is made to contact with sample surfaces; Current source, conductive layer, thermal resistance material layer form closed electrothermal circuit; Electric signal applying unit heats thermal resistance material layer; Probe actuation unit drives probe displacement is to sample surfaces position, the magnetic conductive of needle surface is contacted with sample surfaces, sample and needle point generation heat interchange, its heat has influence on the temperature of thermal resistance material layer through air and magnetic conductive, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, gather this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the thermal signal image of this position sample;
(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 complete to sample surfaces point by point scanning according to the horizontal direction described in step (2);
(8) piezoelectric actuator drives probe to be back to the initial position described in step (2), and the magnetic conductive layer of needle surface is contacted with sample surfaces;
(9) current source, conductive layer, magnetic conductive layer and sample form closed electrical return; Current source applies electric signal to probe, after this electric signal flows into conductive layer, magnetic conductive layer and sample, flow into the earth, coating-forming voltage signal, gather this signal, through chronotron, lock-in amplifier and backend amplifier, be connected with computing machine, after analyzing and processing, obtain the electric signal image of this position sample;
(10) according to the horizontal direction described in step (2), piezoelectric actuator drives probe to the next position;
(11) every bit repeats step (8) and (9), until complete to sample surfaces point by point scanning according to the horizontal direction described in step (2).
Embodiment 8:
In the present embodiment, scanning probe microscopy device is identical with embodiment 5.Difference utilizes that above-mentioned scanning probe microscopy device at room temperature enters heat to sample, electrical property carries out original position, synchronous, real-time detection, and the step (3) namely in detection method and (4) are omitted.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.

Claims (14)

1. the probe in scanning probe microscopy, is characterized in that: comprise feeler arm and needle point, and described needle point comprises needle point body, thermal resistance material layer, the first conductive layer and the second conductive layer; Thermal resistance material layer is positioned at needle point body surface, and the second conductive layer is positioned at thermal resistance material surface; First conductive layer is connected with thermal resistance material layer; Thermal resistance material layer is made up of thermal resistance material, for detecting sample temperature change and thermal conductance; First conductive layer is made up of conductive material, is connected with thermal resistance material, for detecting the change of thermal resistance material resistance; Second conductive layer is made up of conductive material, or the second conductive layer is made up of magnetic conductive material.
2. the probe in scanning probe microscopy as claimed in claim 1, is characterized in that: described thermal resistance material layer material has low-doped silicon, semiconductor, or metallic resistance material.
3. the probe in the scanning probe microscopy stated as claim 1, is characterized in that: the material of the first described conductive layer has a kind of material in the metal of excellent conductive performance and semiconductor or two or more combined materials.
4. the probe in scanning probe microscopy as claimed in claim 3, is characterized in that: the first described conductive layer is the combination of a kind of material in bismuth, nickel, cobalt, potassium, graphite, Graphene or two or more material.
5. the probe in scanning probe microscopy as claimed in claim 1, is characterized in that: the second described conductive has a kind of material in the metal of excellent conductive performance and semiconductor or two or more combined materials; Or the second described conductive is ferromagnetic metal or ferromagnetic alloy.
6. the probe in scanning probe microscopy as claimed in claim 1, is characterized in that: the thickness of described thermal resistance material layer is 0.1 μm ~ 10 μm; The thickness of the first described conductive layer is 0.1 μm ~ 1 μm.
7. the probe in scanning probe microscopy as claimed in claim 1, is characterized in that: the second described conductive layer is integrated in thermal resistance material layer.
8. the probe in scanning probe microscopy as claimed in claim 1, it is characterized in that: arrange insulation course between described resistance elements and the second conductive layer, the first described conductive layer and the second conductive layer are electrically connected.
9. the method in the scanning probe microscopy of preparation as described in claim arbitrary in claim 1 to 6, is characterized in that: comprise the steps:
The method of step 1, employing plated film prepares thermal resistance material layer 8 at needle point body surface;
The method of step 2, employing plated film prepares the first conductive layer 9 at needle point body surface;
The method of step 3, employing plated film is at thermal resistance material layer 8 surface preparation the second conductive layer 10.
10. utilize the scanning probe microscopy of the probe had in claim 1 to 7 described in arbitrary claim sample to be carried out to the detection method of heat-electric in-situ investigation, it is characterized in that: described scanning probe microscopy also comprises probe actuation unit, electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collection unit and centralized control unit
Probe control unit: carry out displacement and/or vibration for driving or controlling probe;
Centralized control unit: for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, heat, electric signal image after analysis;
Detection method comprises the steps
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the electric signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Described pattern one is for detecting surface topography and the electric signal of sample, specific as follows:
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, electric signal applying unit, the first conductive layer, thermal resistance material layer and the second conductive layer form closed electrical return simultaneously; Displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis; Simultaneously, electric signal applying unit applies electric signal to needle point, and this electric signal flows into the first conductive layer, thermal resistance material layer, the second conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis;
Described pattern two is for detecting the thermal signal of sample, specific as follows:
Electric signal applying unit, the first conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer, and then heats probe tip, makes the temperature of probe tip be different from the temperature (the general temperature selected higher than sample) of sample; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample.
11. utilize the scanning probe microscopy of the probe had in claim 1 to 7 described in arbitrary claim sample to be carried out to the detection method of magnetic-Re-electric in-situ investigation, it is characterized in that: the second described conductive layer is made up of magnetic conductive material;
Described scanning probe microscopy also comprises probe actuation unit, electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collecting unit, and centralized control unit,
Probe control unit: carry out displacement and/or vibration for driving or controlling probe;
Centralized control unit: for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, magnetic, heat, electric signal image after analysis;
Detection method comprises the steps
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the magnetic signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Step 3: the initial position in probe displacement to step 1, adopts above-mentioned detection mode three, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the electric signal image of sample;
Described pattern one is for detecting surface topography and the magnetic signal of sample, specific as follows:
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis;
Probe is back to described initial position and upwards raises certain distance, then according to described transversal orientation, sample surfaces is scanned, control probe tip in scanning process and carry out length travel or vibration along described feature image, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the magnetic signal image of sample through centralized control unit analysis;
Described pattern two is for detecting the thermal signal of sample, specific as follows:
Electric signal applying unit, conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer, and then heats probe tip, makes the temperature of probe tip be different from the temperature (the general temperature selected higher than sample) of sample; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, and then have influence on the temperature of thermal resistance material layer, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample;
Described pattern three is for detecting the electric signal of sample, specific as follows:
Electric signal applying unit, conductive layer, thermoelectricity resistance layer, magnetic conductive layer and sample form closed electrical return; Probe actuation unit drives probe displacement is to sample surfaces position, probe tip is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, this electric signal streams is through conductive layer, thermal resistance material layer, magnetic conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
Probe in 12. 1 kinds of scanning probe microscopies, is characterized in that: comprise feeler arm and needle point, and described needle point comprises needle point body and the magnetic conductive layer being positioned at its surface, and on feeler arm, distance needle point certain intervals arranges thermal resistance material layer; Described needle point also comprises conductive layer, conductive layer and thermal resistance material layer phase electric connection, and conductive layer and magnetic conductive layer phase electric connection.
Probe in 13. scanning probe microscopies as claimed in claim 12, is characterized in that: described conductive layer is arranged on thermal resistance material surface.
14. utilize the scanning probe microscopy of the probe had described in claim 12 or 13 sample to be carried out to the detection method of magnetic-Re-electric in-situ investigation, it is characterized in that: described scanning probe microscopy also comprises probe actuation unit, electric signal applying unit, displacement or vibration signals collecting unit, thermal signals collecting unit, electrical signal collecting unit, and centralized control unit
Probe control unit: carry out displacement and/or vibration for driving or controlling probe;
Centralized control unit: for each unit of initialization system, each unit of control system, receives pattern, heat, the electric signal of sample, obtains the pattern of sample, magnetic, heat, electric signal image after analysis;
Detection method comprises the steps
Step 1: sample is fixed on scanning probe microscopy platform, adopts above-mentioned detection mode one, by probe displacement to initial position, transversely carries out directional scanning to sample surfaces, obtains feature image and the magnetic signal image of sample;
Step 2: the initial position in probe displacement to step 1, adopts above-mentioned detection mode two, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the thermal signal image of sample;
Step 3: the initial position in probe displacement to step 1, adopts above-mentioned detection mode three, and the transversal orientation scanning described in carry out step 1 to sample surfaces, obtains the electric signal image of sample;
Described pattern one is for detecting surface topography and the magnetic signal of sample, specific as follows:
Probe actuation unit drives probe displacement is to sample surfaces initial position, probe transversely carries out directional scanning to sample surfaces from this initial position, control probe tip in scanning process to contact with sample surfaces point cantact or oscillation point, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the topography signal of sample through centralized control unit analysis;
Probe is back to described initial position and upwards raises certain distance, then according to described transversal orientation, sample surfaces is scanned, control probe tip in scanning process and carry out length travel or vibration along described feature image, displacement or vibration signals collecting unit receive length travel signal or the vibration signal of probe tip, obtain the magnetic signal image of sample through centralized control unit analysis;
Described pattern two is for detecting the thermal signal of sample, specific as follows:
Electric signal applying unit, conductive layer and thermal resistance material layer form closed-loop path; Electric signal applying unit heats thermal resistance material layer; Probe actuation unit drives probe tip contacts with sample, sample and probe tip generation heat interchange, its heat has influence on the temperature of thermal resistance material layer through air and probe wall, due to thermal resistance effect, the resistance value of thermal resistance material layer is changed, through centralized control unit analysis after thermal signal collecting unit gathers, obtain the thermal signal image of sample;
Described pattern three is for detecting the electric signal of sample, specific as follows:
Electric signal applying unit, conductive layer, magnetic conductive layer and sample form closed electrical return; Probe actuation unit drives probe displacement is to sample surfaces position, probe tip is contacted with sample surfaces, electric signal applying unit applies electric signal to needle point, this electric signal streams is through conductive layer, magnetic conductive layer and sample, coating-forming voltage signal, obtain the electric signal of sample through electrical signal collection unit, obtain the electric signal image of sample through centralized control unit analysis.
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