CN107727886A - A kind of inversion type high speed Electrochemical Atomic Force Microscopy - Google Patents
A kind of inversion type high speed Electrochemical Atomic Force Microscopy Download PDFInfo
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- CN107727886A CN107727886A CN201711047170.5A CN201711047170A CN107727886A CN 107727886 A CN107727886 A CN 107727886A CN 201711047170 A CN201711047170 A CN 201711047170A CN 107727886 A CN107727886 A CN 107727886A
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- high speed
- afm
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
- G01Q60/00—Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
- G01Q60/24—AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
Abstract
The invention discloses a kind of inversion type high speed Electrochemical Atomic Force Microscopy, belong to scanning probe microscopy field.AFM probe is arranged in liquid cell by the present invention, needle point is upward, liquid cell bottom sets transparent glass window, laser, reflecting prism and position sensitive detector are arranged on to the lower section of liquid cell, sample stage is fixed on high speed scanner, described high speed scanner is fixed on auto-feeding device, and three is respectively positioned on the top of described liquid cell；Working electrode is arranged on sample stage, and reference electrode is fixed by screws in the side in electrochemical liquid pond, and annular is arranged on the bottom in electrochemical liquid pond to electrode.The present invention uses inversion type liquid cell not easy to leak, readily replaceable sample；Avoid simultaneously because liquid cell will be fixed on high speed scanner in structure is just put, the adverse effect to caused by high speed scanner dynamic property.
Description
Technical field
The invention belongs to scanning probe microscopy field, it is related to atomic force microscopy, particularly relates to a kind of inversion type
High speed Electrochemical Atomic Force Microscopy.
Background technology
Energy density is high, discharge voltage is high, cycle life is good, green turns into people always to energy storage device (such as：Electricity
Pond, electric capacity etc.) unremitting pursuit.Just because of there is these features, lithium ion battery since the advent of the world is widely used in rapidly hand
In the portable type electronic products such as machine, notebook computer.Lithium ion battery is also rapid at present to expand application to electric automobile, electronic work
The field such as tool, intelligent grid, distributed energy resource system and Aero-Space and national defence.With the extensive use of lithium ion battery,
How further to improve the performance of lithium ion battery and life-span turns into the current focus paid close attention to and studied.
In order to improve the performance of lithium ion battery and life-span, constantly seeking the same of new electrode material and battery system
When, the basic electrochemical issues for studying battery electrode material/solution interface are undoubtedly extremely important.When battery works, exist
Many important interfacial electrochemistry processes, including the decomposition of electrolyte, the growth of solid electrolyte interface film (SEI films) and
Insertion and abjection of lithium ion etc., it is exactly the performance that these interface processes determine lithium ion battery.Due to interfacial electrochemistry mistake
Journey has dynamic characteristic, therefore the research of interfacial electrochemistry is not only challenging, is also provided for development advanced characterization technology
Opportunity.
Currently advanced micro-imaging characterization technique mainly includes：Transmission electron microscopy (TEM), scanning electron microscopy
And Scanning Probe Microscopy (SPM) (SEM).Due to the resolution ratio with atom or nanometer level, TEM and SEM turn into already
The important means that nanometer characterizes, but high-power electron beam, to the demand of high vacuum condition, it is difficult to be surveyed with electrochemistry to make TEM and SEM
Amount method is combined, and realizes the in-situ observation of electrode material/solution interface.SPM has nanometer/atomic resolution, by wide
General applicability (vacuum, air, solution, high/low temperature etc.) and the compatibility easily combined with other characterizing methods, make SPM reach a conclusion after weighing a matter
The important characterizing method in material and biological field has been rapidly become since generation.
AFM (AFM) is that most commonly used important characterization method is applied to obtain in SPM.By under contact mode
The repulsive force between needle point and sample surfaces is detected, AFM can be provided with the nanometer even surface topography of atomic weight class resolution ratio
Picture, and have been used for the research of electrode material.Such as：Typical electrode materials LiFePO is observed using AFM4Surface before and after aging
Pattern, it is found that the electrode nanoparticle after aging is gathered into larger-sized particle.The coarsening of nano particle causes surface electric
Resistance increase or surface conductivity reduce, therefore cause the reduction of performance of lithium ion battery.Due in interface change procedure (such as electrode
Embedding and removing process, SEM growth etc.) in the microscopic appearance change of electrode surface be a universal phenomenon, therefore directly
It is extremely important for the interfacial reaction and ageing of electrode mechanism for studying and understanding electrode/solution to observe these changes.Electrochemistry
AFM (EC-AFM) is to be combined AFM high-resolution imaging functions with electrochemical measuring method, it has also become research fill/
The powerful of modification of surface morphology in discharge process.
However, the EC-AFM established on the basis of conventional AFM simply solves the problems, such as in situ imaging, and can not carry out in real time
Observation.The afm image that usual EC-AFM obtains the pixel of a frame 256 × 256 needs a few minutes clock time, if electrode material surface shape
Looks change procedure is faster than the time for obtaining a two field picture, and this change is difficult to be caught in and record.Therefore, slowly into
As speed turns into the main bottleneck of EC-AFM observation electrode material surface pattern complexity dynamic changes.Contemplate, if keeping EC-
While AFM nanometer scale space resolution ratio, temporal resolution, the characterizing method of development in real time, in situ, undoubtedly with important are improved
Scientific meaning and application value.
In recent ten years, high speed atomic force microscope (HS-AFM) turns into the focus that nanometer representational field is paid close attention to and studied.
In fact, development HS-AFM is not only and simply increases conventional AFM turntable driving speed and can be achieved with, but one has
The work of challenge, it is related to problems, including：High frequency micro-cantilever probe, probe deflection Precision measurement, high-velocity scanning controlling party
Formula processing etc. with scanning device, feedback control and data acquisition and in real time.Patent applicant this year it is newest deliver on
These aspects are systematically discussed and summarized in HS-AFM survey articles.Because AFM is widely applied field, various countries' research people
Member establishes respective " Laboratary type " HS-AFM mainly according to respective research direction and interest.The Ando of Kanazawa, Japan university
The seminar of leader is taught, has given priority to the HS-AFM for biological field research, and obtains important research progress.Such as：
Motion process of the myosin-V unimolecules along actin filament is observed with the video speed of 12.5 frames/second, this is also cell
The process of interior transmission vesica and organelle.With compared with the result that optical tweezer obtains, HS-AFM image shows go out molecular motion process
More details.In terms of material science research, Pyne et al. have studied the fluoride under sour environment using HS-AFM
Influence to hydroxyapatite crystals rate of dissolution, it was observed that the change of obvious rate of dissolution.Brausmann et al. the side of have studied
Solve the problems of dissolution of stone crystal.As a result show, HS-AFM image taking speeds are higher, and the details of dissolution of crystals dynamic process is more.
High speed atomic force microscope (HS-AFM) is incorporated into EC-AFM, Developing High-speed Electrochemical Atomic Force Microscopy
(HS-EC-AFM) image taking speed, is brought up into video magnitude (25 frames/second) from the frame of a few minutes 1, realizes electrode material/solution circle
The real-time in-situ observation in face, the more details information of electrode surface microscopic appearance and change of properties is obtained, no matter to nanometer electrification
Basic research is still all significant as the application study of representative using lithium ion battery.Examined in addition from technological layer
Consider, develop HS-EC-AFM value also reside in researcher can quick capture material surface region interested, and then locking is locally
Imaging, can not only observe transient phenomenon, but also drastically increase Efficiency.In addition, HS-EC-AFM is very
It is easily applied to other research fields, the burn into high speed nanometer etching and processing of such as metal material.
The content of the invention
The purpose of the present invention is a kind of inversion type high speed Electrochemical Atomic Force Microscopy (HS-EC-AFM) of development, be can be used for
In the solution real-time in-situ observation solid-state material surface topography dynamic change, be on micro-nano-scale carry out solid-state material/
The electrochemical process research of solution interface provides powerful measure.
Of the present invention is a kind of inversion type high speed Electrochemical Atomic Force Microscopy, is mainly included：AFM probe, laser
Device, reflecting prism, position sensitive detector, liquid cell, windowpane, working electrode, reference electrode, annular to electrode, sample stage,
High speed scanner and auto-feeding device.Wherein, described AFM probe is located in liquid cell, and upward, liquid cell bottom is set needle point
Transparent glass window is put, described laser, reflecting prism and position sensitive detector are arranged on the lower section of liquid cell, described sample
Sample platform is fixed on high speed scanner, and described high speed scanner is fixed on auto-feeding device, and three is respectively positioned on described
The top of liquid cell.The working electrode is arranged on sample stage, and the reference electrode is fixed by screws in electrochemical liquid
The side in pond, the annular are arranged on the bottom in electrochemical liquid pond to electrode.
Described high speed scanner uses combined three-dimensional high-speed scanning device, mainly by piezoelectric ceramic tube and bimorph
Composition, concrete structure can refer to patent of invention (patent name：A kind of combined three-dimensional high-speed scanning device, the patent No.：
ZL200910085101.2, authorization date：2011.1.12).
The advantage of the invention is that：
(1) inversion type structure make solution formd in liquid cell bottom with glass surface identical plane, avoid due to
Liquid level bending influence to caused by the laser beam direction of propagation, it is easier to adjust laser beam, make light beam focus on AFM micro-cantilevers.
(2) the upper part design open window in electrochemical liquid pond, makes sample be easily accessible in liquid cell, this is just
Avoid because liquid cell will be fixed on high speed scanner in structure is just put, to caused by high speed scanner dynamic property not
Profit influences.
(3) research shows, is an important factor for influenceing electrochemical measurement on the area ratio between electrode and working electrode.Should
Increase as far as possible to electrode size and reduce working electrode size.In the inversion type structure of this invention, the size of working electrode
Usually 5mmx5mm, i.e. area are about 25mm2；Can be of about 3000mm to the minimum area of electrode2, therefore area ratio is more than 100
Times, can solve this problem well.
(4) compared with positively fixed type, inversion type liquid cell not easy to leak.
(5) readily replaceable sample.
Brief description of the drawings
Fig. 1 is conventional EC-AFM operation principle schematic diagrams in the prior art.
A kind of inversion type high speed Electrochemical Atomic Force Microscopy structure chart of Fig. 2 present invention.
In figure：
101.AFM probe；102. laser；103. reflecting prism；104. position sensitive detector；
201. liquid cell；202. windowpane；203. working electrode；204. reference electrode；
205. annulars are to electrode；206. sample stage；301. high speed scanner；302. auto-feeding devices.
Embodiment
Below in conjunction with drawings and examples, the present invention is described in further detail：
Electrochemical solution pond and laser beam deflection detection means are to develop EC-HS-AFM key issue, because they are
The core of the imaging of Fast atom power and electrochemical measurement is contacted, for whether high-resolution and high stable imaging and simultaneously can be realized
It is most important to carry out electrochemical measurement.Conventional positively fixed type EC-AFM operation principle as shown in figure 1, atomic force micro-cantilever probe and
Sample is located in liquid cell, and the needle point of the atomic force micro-cantilever probe is down；Laser deflection detecting system (including：Swash
Light device and four-quadrant position sensitive detector) above liquid cell, for detecting micro-cantilever due to (described by sample surfaces
Sample is using silicon as substrate, and intermediate layer is golden conductive layer, and surface is film layer) active force and caused micro-strain signal, and give
Enter in electronic control system so as to obtain surface topography image.Liquid cell provides the environment of electrode surface reaction, and by electrification
Learn work stand control.There is working electrode in the liquid cell, to electrode and reference electrode, wherein reference electrode is calomel electrode,
It is platinum electrode to electrode.Wherein, sample is tested face-up, and the micro-strain of AFM micro-cantilevers, the laser of laser transmitting is in pin
The reflected light path at the sharp back side directly detects its detection by four-quadrant position sensitive and obtained, therefore described laser deflection detecting system
Positioned at the top of the liquid cell.
The present invention is to provide a kind of nanometer test platform suitable for real-time monitored electrochemical field in situ, one kind is inverted
Formula high speed Electrochemical Atomic Force Microscopy, as shown in Fig. 2 the inversion type high speed Electrochemical Atomic Force Microscopy includes：AFM is micro-
Cantilever probe (hereinafter referred to as AFM probe) 101, laser 102, reflecting prism 103, position sensitive detector 104, liquid cell
201st, windowpane 202, working electrode 203, reference electrode 204, annular are to electrode 205, sample stage 206, the and of high speed scanner 301
Auto-feeding device 302.Wherein, described AFM probe 101 is located in liquid cell 201, and the bottom of liquid cell 201 sets transparent glass
Glass window 202, described laser 102, reflecting prism 103 and position sensitive detector 104 are arranged on the lower section of liquid cell 201,
Described sample stage 206 is fixed on high speed scanner 301, and described high speed scanner 301 is fixed on auto-feeding device 302
On, three is respectively positioned on the top of described liquid cell 201.The working electrode 203 is arranged on sample stage 206, the reference
Electrode 204 is fixed by screws in the side in electrochemical liquid pond 201, and the annular is arranged on electrochemical liquid to electrode 205
The bottom in pond 201.
Described AFM probe 101, laser 102, reflecting prism 103, liquid cell 201, high speed scanner 301 and automatic
Approach device 302 to be installed in AFM main bodys, particular location relation is as follows：
Described AFM probe 101 is arranged in AFM main bodys by fixed mount.Described laser 102 and reflecting prism
103 are fixed in AFM main bodys by a two-dimensional adjustment platform, make the laser beam focus that laser 102 is launched in AFM probe 101
On.Described position sensitive detector 104 is fixed in AFM main bodys by a two-dimension translational platform, makes the anti-of AFM probe 101
Penetrate hot spot to fall on position sensitive detector 104, the photosignal of the position spirit detector 104 output is imaged for AFM.It is described
Electrochemical liquid pond 201 be arranged in AFM main bodys, the bottom in electrochemical liquid pond 201 sets transparent glass window 202, can be with
Realize the incidence and reflection of laser beam.
Described annular is more than the external diameter of windowpane 202 to the internal diameter of electrode 205, to avoid annular to electrode pair windowpane
The influence of thang-kng.The high speed scanner 301 and auto-feeding device 302 are arranged in AFM main bodys, and wherein auto-feeding fills
302 are put mainly to be made up of the common method such as micrometric screw and stepping electrode.
The operation principle of described inversion type high speed Electrochemical Atomic Force Microscopy provided by the invention is as follows：AFM is micro- outstanding
Arm probe is fixed in liquid cell by needle point frame, and needle point is upward.Sample stage is located at can be with auto-feeding above liquid cell
AFM micro-cantilever probes in liquid cell, laser deflection detecting system are located at below liquid cell.The light sent by semiconductor laser
Beam upwardly propagates by reflecting prism, is carried on the back by the needle point that AFM micro-cantilever probes are focused on after the windowpane 202 of liquid cell bottom surface
Face, it is then reflected by, is reached after again passing through the windowpane 202 of liquid cell bottom surface on four-quadrant position sensitive detector 104.When
When sample on the control high speed scanner 301 of auto-feeding device 302 contacts with the needle point of AFM micro-cantilever probes, AFM is micro-
Cantilever is because stress bending causes laser beam deflection, and micro-displacement is by four-quadrant position sensitive detector caused by light beam deflection
104 detections, the current signal of output are sent into electronic control system after being amplified by pre-current amplifier, and these are former at a high speed
The part and operation principle of sub- force microscope, the imaging of high speed pattern can be achieved.Three electrodes in liquid cell 201, including：
Working electrode 203, electrode 205 and reference electrode 204 are connected with the respective electrode of electrochemical workstation respectively, form three electrodes
System, for realizing electrochemical reaction.This inversion type Fast atom power mirror is combined with electro-chemical systems, for electrochemistry mistake
The Real Time Observation in situ that sample pattern changes in journey.
Embodiment
A kind of inversion type high speed Electrochemical Atomic Force Microscopy, AFM micro-cantilevers probe 101 are semiconductor laser 102, anti-
It is commercialized device to penetrate prism 103 and position sensitive detector 104, and electrochemical liquid pond 201 is by polytetrafluoroethylmaterial material system
Into being shaped as circular or square, external diameter 68mm, internal diameter 46mm, be highly 18mm, transparent glass window 202 is by quartz glass
It is made, a diameter of 38mm, thickness 5mm, liquid cell bottom can be fixed on by threaded ring or gluing method, when solution is deposited
When, because solution and the upper surface of windowpane 202 form plane, therefore the laser adjustment and detection to AFM have little to no effect.
Using calomel electrode as reference electrode 204, and the side of liquid cell 201 is fixed on, annular is made to electrode using metal platinized platinum
205, its external diameter is 46mm, internal diameter 39mm, thickness 1mm, and parallel with working electrode 203.Sample stage can use metal (copper,
Aluminium etc.) material is made.Visible patent (the patent name of combined three-dimensional high-speed scanning device：A kind of combined three-dimensional high-speed scanning
Device, the patent No.：ZL200910085101.2, authorization date：2011.1.12).
The high speed electrochemistry atomic force microscopy imaging resolution：10 nanometers, highest image taking speed：25 frames/second, maximum are swept
Retouch scope：10 microns.
Claims (4)
- A kind of 1. inversion type high speed Electrochemical Atomic Force Microscopy, it is characterised in that：Including AFM probe, laser, reflection rib Mirror, position sensitive detector, liquid cell, windowpane, working electrode, reference electrode, annular are to electrode, sample stage, high-velocity scanning Device and auto-feeding device；Wherein, described AFM probe is located in liquid cell, and upward, liquid cell bottom sets transparent glass to needle point Glass window, described laser, reflecting prism and position sensitive detector are arranged on the lower section of liquid cell, and described sample stage is fixed On high speed scanner, described high speed scanner is fixed on auto-feeding device, and three is respectively positioned on described liquid cell Top；The working electrode is arranged on sample stage, and the reference electrode is fixed by screws in the side in electrochemical liquid pond, The annular is arranged on the bottom in electrochemical liquid pond to electrode.
- A kind of 2. inversion type high speed Electrochemical Atomic Force Microscopy according to claim 1, it is characterised in that：Described height Fast scanner uses combined three-dimensional high-speed scanning device, and concrete structure uses the invention of Application No. 2009100851012 special A kind of combined three-dimensional high-speed scanning device disclosed in profit application.
- A kind of 3. inversion type high speed Electrochemical Atomic Force Microscopy according to claim 1, it is characterised in that：Described swashs Light device and reflecting prism are fixed in AFM main bodys by a two-dimensional adjustment platform, make the laser beam focus that laser is launched in AFM On probe；Described position sensitive detector is fixed in AFM main bodys by a two-dimension translational platform, makes the reflection of AFM probe Hot spot falls on position sensitive detector, and the photosignal of position spirit detector output is imaged for AFM；Described electrochemistry Liquid cell is arranged in AFM main bodys.
- A kind of 4. inversion type high speed Electrochemical Atomic Force Microscopy according to claim 1, it is characterised in that：Described ring Shape is more than the external diameter of windowpane to the internal diameter of electrode.
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Cited By (5)
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| WO2020000400A1 (en) * | 2018-06-29 | 2020-01-02 | Jiangsu Jitri Micro-Nano Automation Institute Co., Ltd. | A method for sem-guided afm scan with dynamically varied scan speed |
| CN111413388A (en) * | 2020-03-20 | 2020-07-14 | 中国科学院化学研究所 | Electrochemical testing device and method for observing columnar lithium electrode by atomic force microscope |
| CN112684212A (en) * | 2020-12-26 | 2021-04-20 | 温州大学 | Liquid phase imaging method of atomic force microscope |
| CN112924511A (en) * | 2019-12-05 | 2021-06-08 | 中国科学院大连化学物理研究所 | Photoelectrochemical pool based on atomic force microscope and scanning electrochemical microscope |
| WO2024016425A1 (en) * | 2022-07-19 | 2024-01-25 | 厦门大学 | Electrochemical nano infrared spectromicroscope and analysis method |
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| WO2024016425A1 (en) * | 2022-07-19 | 2024-01-25 | 厦门大学 | Electrochemical nano infrared spectromicroscope and analysis method |
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Granted publication date: 20200904 Termination date: 20211031 |