CN107727886B - Inverted high-speed electrochemical atomic force microscope - Google Patents
Inverted high-speed electrochemical atomic force microscope Download PDFInfo
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- CN107727886B CN107727886B CN201711047170.5A CN201711047170A CN107727886B CN 107727886 B CN107727886 B CN 107727886B CN 201711047170 A CN201711047170 A CN 201711047170A CN 107727886 B CN107727886 B CN 107727886B
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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 an inverted high-speed electrochemical atomic force microscope, and belongs to the technical field of scanning probe microscopy. The AFM probe is arranged in a liquid pool, the needle point is upward, a transparent glass window is arranged at the bottom of the liquid pool, a laser, a reflecting prism and a position sensitive detector are arranged below the liquid pool, a sample table is fixed on a high-speed scanner, the high-speed scanner is fixed on an automatic approximation device, and the laser, the reflecting prism and the position sensitive detector are all positioned above the liquid pool; the working electrode is arranged on the sample platform, the reference electrode is fixed on the side surface of the electrochemical liquid pool through a screw, and the annular counter electrode is arranged at the bottom of the electrochemical liquid pool. The inverted liquid pool adopted by the invention is not easy to leak and the sample is easy to replace; and meanwhile, the adverse effect on the dynamic performance of the high-speed scanner caused by the fact that the liquid pool needs to be fixed on the high-speed scanner in the upright structure is avoided.
Description
Technical Field
The invention belongs to the technical field of scanning probe microscopy, relates to an atomic force microscopy technology, and particularly relates to an inverted high-speed electrochemical atomic force microscope.
Background
The energy density is high, the discharge voltage is high, the cycle life is long, and the environment protection is always a continuous pursuit of people for energy storage devices (such as batteries, capacitors and the like). Due to these characteristics, lithium ion batteries have been widely and rapidly used in portable electronic products such as mobile phones and notebook computers since their appearance. Lithium ion batteries are also currently rapidly expanding in applications in the fields of electric automobiles, electric tools, smart grids, distributed energy systems, aerospace, national defense and the like. With the wide application of lithium ion batteries, how to further improve the performance and the service life of the lithium ion batteries becomes a hot spot of current attention and research.
In order to improve the performance and lifetime of lithium ion batteries, it is clearly important to study the underlying electrochemical problems at the battery electrode material/solution interface while continuously searching for new electrode materials and battery systems. When a battery is operated, there are many important interfacial electrochemical processes, including decomposition of an electrolyte, growth of a solid electrolyte interfacial film (SEI film), and intercalation and deintercalation of lithium ions, and it is these interfacial processes that determine the performance of a lithium ion battery. Because the interfacial electrochemical process has dynamic characteristics, the research of the interfacial electrochemistry is not only challenging, but also provides opportunities for developing advanced characterization technologies.
The current advanced microscopic imaging characterization technology mainly comprises: transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), and Scanning Probe Microscopy (SPM). Because of the resolution at atomic or nanometer level, TEM and SEM have long been important means for nanometer characterization, however, the requirement of high-energy electron beam for high vacuum condition makes it difficult to combine TEM and SEM with electrochemical measurement method to realize in-situ observation of electrode material/solution interface. SPM has nanometer/atomic resolution, and by virtue of its wide applicability (vacuum, atmosphere, solution, high and low temperatures, etc.) and its compatibility with other characterization methods, SPM has since its inception been rapidly becoming an important characterization method in the fields of materials and biology.
Atomic Force Microscopy (AFM) is the most widely used important characterization tool in SPM. By detecting the repulsive force between the tip and the sample surface in the contact mode, AFM can provide surface topography images with nanometer or even atomic scale resolution and has been used for the study of electrode materials. For example: LiFePO, a typical electrode material, was observed by AFM4The surface appearance before and after aging shows that the electrode nanoparticles after aging are aggregated into larger particles. Coarsening of the nanoparticles results in an increase in surface resistance or a decrease in surface conductivity, and thus, a decrease in performance of the lithium ion battery. Since changes in the micro-morphology of the electrode surface during interfacial changes (e.g., intercalation and deintercalation of the electrode, SEM growth, etc.) are a common phenomenon, direct observation of these changes is important for the study and understanding of the electrode/solution interfacial reactions and the electrode aging mechanism. An electrochemical atomic force microscope (EC-AFM) is a powerful tool for researching the surface morphology change in the charging/discharging process by combining an AFM high-resolution imaging function with an electrochemical measurement method.
However, EC-AFM based on conventional AFM only solves the in situ imaging problem and does not allow real-time observation. Typically, it takes several minutes for EC-AFM to obtain a frame of AFM image of 256 × 256 pixels, and if the electrode material surface topography changes faster than the time to obtain a frame of image, the changes are difficult to capture and record. Therefore, the slow imaging speed becomes the main bottleneck of observing the complicated dynamic change of the surface topography of the electrode material by the EC-AFM. It is assumed that the method has important scientific significance and application value certainly if the time resolution can be improved and a real-time and in-situ characterization method can be developed while the EC-AFM nanometer-scale spatial resolution is kept.
In recent decades, high speed atomic force microscopy (HS-AFM) has become a focus of attention and research in the field of nanotechnology characterization. In fact, developing an HS-AFM is not simply achieved by increasing the scan drive speed of a conventional AFM, but rather a challenging task involving a number of problems, including: high-frequency micro-cantilever probe, probe deflection precision detection, high-speed scanning control mode and scanning device, feedback control, data acquisition, real-time processing and the like. The applicant has systematically discussed and summarized these aspects in the recent review article published this year on HS-AFMs. Due to the wide application field of AFM, researchers in various countries establish respective 'laboratory type' HS-AFM mainly according to respective research directions and interests. The HS-AFM used for the research in the biological field is developed with emphasis on the subject group led by professor Ando of the university of Kingze, Japan, and has made an important research progress. For example: the movement process of myosin-V single molecules along actin filaments was observed at a video rate of 12.5 frames/sec, which is also the process of intracellular transport vesicles and organelles. HS-AFM images show more detailed information of the molecular motion process than the results obtained with optical tweezers. In the aspect of material science research, Pyne et al studied the influence of fluoride on the dissolution rate of hydroxyapatite crystals in an acidic environment by using HS-AFM, and observed a significant change in the dissolution rate. Brausmann et al investigated the dissolution problem of calcite crystals. The results show that the higher the HS-AFM imaging speed, the more detailed the crystal dissolution dynamics.
A high-speed atomic force microscope (HS-AFM) is introduced into the EC-AFM, a high-speed electrochemical atomic force microscope (HS-EC-AFM) is developed, the imaging speed is improved to a video magnitude (25 frames/second) from 1 frame in a few minutes, real-time in-situ observation of an electrode material/solution interface is realized, more detailed information of electrode surface micro-morphology and property change is obtained, and the method has important significance for basic research of nano electrochemistry and application research represented by a lithium ion battery. In addition, from the technical aspect, the development of the HS-EC-AFM is valuable in that researchers can quickly capture the interested area on the surface of the material, and then local imaging is locked, so that not only the evanescent phenomenon can be observed, but also the research efficiency is greatly improved. In addition, the HS-EC-AFM can be easily applied to other research fields, such as corrosion of metal materials, high-speed nano etching processing and the like.
Disclosure of Invention
The invention aims to develop an inverted high-speed electrochemical atomic force microscope (HS-EC-AFM), which can be used for real-time in-situ observation of dynamic changes of the surface morphology of a solid material in a solution and provides a powerful means for developing electrochemical process research of a solid material/solution interface on a micro-nano scale.
The invention relates to an inverted high-speed electrochemical atomic force microscope, which mainly comprises: the device comprises an AFM probe, a laser, a reflecting prism, a position sensitive detector, a liquid pool, a glass window, a working electrode, a reference electrode, an annular counter electrode, a sample stage, a high-speed scanner and an automatic approximation device. The AFM probe is positioned in the liquid pool, the needle point of the AFM probe faces upwards, the bottom of the liquid pool is provided with the transparent glass window, the laser, the reflecting prism and the position sensitive detector are arranged below the liquid pool, the sample stage is fixed on the high-speed scanner, the high-speed scanner is fixed on the automatic approximation device, and the laser, the reflecting prism and the position sensitive detector are all positioned above the liquid pool. The working electrode is arranged on the sample platform, the reference electrode is fixed on the side surface of the electrochemical liquid pool through a screw, and the annular counter electrode is arranged at the bottom of the electrochemical liquid pool.
The high-speed scanner adopts a combined three-dimensional high-speed scanning device which mainly comprises a piezoelectric ceramic tube and double piezoelectric plates, and the specific structure can be seen in the invention patent (the patent name is a combined three-dimensional high-speed scanning device, the patent number is ZL200910085101.2, and the authorization date is 2011.1.12).
The invention has the advantages that:
(1) the inverted structure enables the solution to form a plane which is the same as the surface of the glass at the bottom of the liquid pool, avoids the influence on the propagation direction of the laser beam due to the bending of the liquid level, is easier to adjust the laser beam and enables the laser beam to be focused on the AFM micro-cantilever.
(2) The upper part of the electrochemical liquid pool is provided with an open window, so that a sample to be detected can easily enter the liquid pool, and the adverse effect on the dynamic performance of a high-speed scanner caused by the fact that the liquid pool is fixed on the high-speed scanner in an upright structure is avoided.
(3) Studies have shown that the area ratio between the counter electrode and the working electrode is an important factor affecting electrochemical measurements. The counter electrode size should be increased as much as possible while the working electrode size is decreased. In the inverted configuration of the present invention, the working electrode is typically 5mmx5mm in size, i.e., about 25mm in area2(ii) a The minimum area of the counter electrode can reach about 3000mm2Therefore, the area ratio is more than 100 times, and this problem can be solved well.
(4) Compared with the positive type, the inverted liquid pool is not easy to leak.
(5) The sample is easily replaced.
Drawings
FIG. 1 is a schematic diagram of the working principle of a conventional EC-AFM in the prior art.
FIG. 2 is a schematic diagram of an inverted high-speed electrochemical atomic force microscope of the present invention.
In the figure:
an AFM probe 101; 102, a laser; a reflective prism 103; a position sensitive detector;
201. a liquid pool; 202, glazing; a working electrode; 204. a reference electrode;
205. an annular counter electrode; 206. a sample stage; 301, a high speed scanner; automatic approximation means 302.
Detailed Description
The invention will be described in further detail with reference to the following figures and examples:
the electrochemical solution pool and the laser beam deflection detection device are key problems for developing the EC-HS-AFM, because the electrochemical solution pool and the laser beam deflection detection device are the core of the connection of high-speed atomic force imaging and electrochemical measurement and are crucial to whether high-resolution and high-stability imaging can be realized and the electrochemical measurement can be carried out simultaneously. The working principle of the conventional upright EC-AFM is shown in FIG. 1, wherein an atomic force micro-cantilever probe and a sample are positioned in a liquid pool, and the tip of the atomic force micro-cantilever probe faces downwards; the laser deflection detection system (comprising a laser and a four-quadrant position sensitive detector) is positioned above the liquid pool, and is used for detecting a micro-deformation signal generated by the micro-cantilever due to the acting force of the surface of a sample (the sample takes silicon as a substrate, the middle layer is a gold conducting layer, and the surface is a thin film layer), and sending the micro-deformation signal into an electronic control system so as to obtain a surface topography image. The liquid pool provides the environment for the electrode surface reaction and is controlled by the electrochemical workstation. The liquid pool is provided with a working electrode, a counter electrode and a reference electrode, wherein the reference electrode is a calomel electrode, and the counter electrode is a platinum electrode. Wherein, the tested surface of the sample is upward, the AFM micro-cantilever deforms slightly, the reflected light path of the laser emitted by the laser on the back of the needle point is directly detected by the four-quadrant position sensitive detection, and therefore, the laser deflection detection system is positioned above the liquid pool.
The invention provides a nano test platform suitable for in-situ real-time observation electrochemistry field, an inverted high-speed electrochemistry atomic force microscope, as shown in figure 2, the inverted high-speed electrochemistry atomic force microscope comprises: an AFM micro-cantilever probe (hereinafter referred to as AFM probe) 101, a laser 102, a reflecting prism 103, a position sensitive detector 104, a liquid pool 201, a glass window 202, a working electrode 203, a reference electrode 204, an annular counter electrode 205, a sample stage 206, a high-speed scanner 301 and an automatic approximation device 302. The AFM probe 101 is positioned in a liquid pool 201, a transparent glass window 202 is arranged at the bottom of the liquid pool 201, the laser 102, the reflecting prism 103 and the position sensitive detector 104 are arranged below the liquid pool 201, the sample stage 206 is fixed on a high-speed scanner 301, the high-speed scanner 301 is fixed on an automatic approximation device 302, and the three are positioned above the liquid pool 201. The working electrode 203 is arranged on a sample stage 206, the reference electrode 204 is fixed on the side surface of the electrochemical liquid cell 201 through a screw, and the annular counter electrode 205 is arranged at the bottom of the electrochemical liquid cell 201.
The AFM probe 101, the laser 102, the reflecting prism 103, the liquid pool 201, the high-speed scanner 301 and the automatic approximation device 302 are all arranged on an AFM main body, and the specific position relation is as follows:
the AFM probe 101 is mounted on the AFM body through a fixing frame. The laser 102 and the reflecting prism 103 are fixed on the AFM body through a two-dimensional adjusting table, so that the laser beam emitted by the laser 102 is focused on the AFM probe 101. The position sensitive detector 104 is fixed on the AFM main body through a two-dimensional translation stage, so that a reflection spot of the AFM probe 101 falls on the position sensitive detector 104, and a photoelectric signal output by the position sensitive detector 104 is used for AFM imaging. The electrochemical liquid cell 201 is arranged on an AFM main body, and the bottom of the electrochemical liquid cell 201 is provided with a transparent glass window 202, so that incidence and reflection of laser beams can be realized.
The inner diameter of the annular counter electrode 205 is larger than the outer diameter of the glass window 202 to avoid the influence of the annular counter electrode on the light transmittance of the glass window. The high-speed scanner 301 and the automatic approximation device 302 are mounted on an AFM main body, wherein the automatic approximation device 302 is mainly composed of a micrometer screw, a stepping electrode and other common methods.
The working principle of the inverted high-speed electrochemical atomic force microscope provided by the invention is as follows: the AFM microcantilever probe is fixed in the liquid pool by the tip rack, and the tip is upward. The sample stage is positioned above the liquid pool and can automatically approach an AFM micro-cantilever probe in the liquid pool, and the laser deflection detection system is positioned below the liquid pool. The light beam emitted by the semiconductor laser travels upward through the reflecting prism, passes through the glass window 202 on the bottom surface of the liquid pool, is focused on the back surface of the tip of the AFM micro-cantilever probe, is reflected, passes through the glass window 202 on the bottom surface of the liquid pool again, and then reaches the four-quadrant position sensitive detector 104. When the automatic approximation device 302 controls a sample to be detected on the high-speed scanner 301 to be in contact with the needle tip of the AFM micro-cantilever probe, the AFM micro-cantilever deflects a laser beam due to stress bending, a micro displacement generated by the deflection of the laser beam is detected by the four-quadrant position sensitive detector 104, an output current signal is amplified by a front current amplifier and then is sent into an electronic control system, and the components and the working principle of the high-speed atomic force microscope are adopted, so that high-speed morphology imaging can be realized. Three electrodes in the fluid cell 201, including: the working electrode 203, the counter electrode 205 and the reference electrode 204 are respectively connected with corresponding electrodes of an electrochemical workstation to form a three-electrode system for realizing electrochemical reaction. The inversion type high-speed atomic force mirror is combined with an electrochemical system and used for in-situ real-time observation of the shape change of a detected sample in the electrochemical process.
Examples
An inverted high-speed electrochemical Atomic Force Microscope (AFM) micro-cantilever probe 101, a semiconductor laser 102, a reflecting prism 103 and a position sensitive detector 104 are commercial devices, an electrochemical liquid pool 201 is made of polytetrafluoroethylene materials and is circular or square in shape, 68mm in outer diameter, 46mm in inner diameter and 18mm in height, a transparent glass window 202 is made of quartz glass, 38mm in diameter and 5mm in thickness and can be fixed at the bottom of the liquid pool through a threaded clamping ring or an adhesive method, and when a solution exists, the solution and the upper surface of the glass window 202 form a plane, so that laser adjustment and detection of the AFM are hardly influenced. A calomel electrode is used as a reference electrode 204 and fixed on one side of the liquid pool 201, and a metal platinum sheet is used for manufacturing an annular counter electrode 205, wherein the outer diameter of the annular counter electrode is 46mm, the inner diameter of the annular counter electrode is 39mm, the thickness of the annular counter electrode is 1mm, and the annular counter electrode is parallel to the working electrode 203. The sample stage can be made of metal (copper, aluminum, etc.). The combined three-dimensional high-speed scanning device can be seen in a patent (the patent name is a combined three-dimensional high-speed scanning device, the patent number is ZL200910085101.2, and the authorization date is 2011.1.12).
The resolution of the high-speed electrochemical atomic force microscopic imaging is as follows: 10 nm, highest imaging speed: 25 frames/sec, maximum scan range: 10 microns.
Claims (3)
1. An inverted high-speed electrochemical atomic force microscope, characterized in that: the device is used for real-time in-situ observation of the dynamic change of the surface topography of the solid material in a solution; the inverted high-speed electrochemical atomic force microscope comprises an AFM probe, a laser, a reflecting prism, a position sensitive detector, a liquid pool, a glass window, a working electrode, a reference electrode, an annular counter electrode, a sample stage, a high-speed scanner and an automatic approximation device; wherein, theThe AFM probe is positioned in a liquid pool, the needle point of the AFM probe faces upwards, a transparent glass window is arranged at the bottom of the liquid pool, the laser, the reflecting prism and the position sensitive detector are arranged below the liquid pool, the sample stage is fixed on a high-speed scanner, the high-speed scanner is fixed on an automatic approximation device, and the laser, the reflecting prism and the position sensitive detector are all positioned above the liquid pool; the working electrode is arranged on the sample platform, the reference electrode is fixed on the side surface of the electrochemical liquid pool through a screw, the annular counter electrode is arranged at the bottom of the electrochemical liquid pool, the annular counter electrode is made of a metal platinum sheet, the outer diameter of the annular counter electrode is 46mm, the inner diameter of the annular counter electrode is 39mm, the thickness of the annular counter electrode is 1mm, and the annular counter electrode is parallel to the working electrode; the size of the working electrode is 5mmx5mm, namely the area is 25mm2(ii) a The minimum area of the counter electrode reaches 3000mm2The area ratio of the counter electrode to the working electrode is greater than 100; the laser and the reflecting prism are fixed on the AFM main body through a two-dimensional adjusting table, so that laser beams emitted by the laser are focused on the AFM probe; the position sensitive detector is fixed on the AFM main body through a two-dimensional translation stage, so that a reflection light spot of the AFM probe falls on the position sensitive detector, and a photoelectric signal output by the position sensitive detector is used for AFM imaging; the electrochemical liquid pool is arranged on the AFM body.
2. The inverted high-speed electrochemical atomic force microscope of claim 1, wherein: the high-speed scanner adopts a combined three-dimensional high-speed scanning device.
3. The inverted high-speed electrochemical atomic force microscope of claim 1, wherein: the inner diameter of the annular counter electrode is larger than the outer diameter of the glass window.
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| US11158486B2 (en) | 2018-06-29 | 2021-10-26 | Jiangsu Jitri Micro-Nano Automation Institute Co., Ltd. | Method for SEM-guided AFM scan with dynamically varied scan speed |
| CN112924511B (en) * | 2019-12-05 | 2021-12-14 | 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 |
| CN111413388B (en) * | 2020-03-20 | 2021-01-26 | 中国科学院化学研究所 | Electrochemical testing device and method for observing columnar lithium electrode by atomic force microscope |
| CN112684212B (en) * | 2020-12-26 | 2022-08-30 | 温州大学 | Liquid phase imaging method of atomic force microscope |
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| US5319960A (en) * | 1992-03-06 | 1994-06-14 | Topometrix | Scanning force microscope |
| JP4361405B2 (en) * | 2003-03-18 | 2009-11-11 | エスアイアイ・ナノテクノロジー株式会社 | Mask black defect correction by applying electrochemical method to AFM |
| JP2005037205A (en) * | 2003-07-18 | 2005-02-10 | Hitachi Kenki Fine Tech Co Ltd | Scanning probe microscope and measuring method of the same |
| US8601608B2 (en) * | 2005-03-31 | 2013-12-03 | Japan Science And Technology Agency | Cantilever for scanning probe microscope and scanning probe microscope equipped with it |
| CN101576466B (en) * | 2009-05-31 | 2011-01-12 | 北京航空航天大学 | Combined three-dimensional high-speed scanning device |
| CN103235158B (en) * | 2013-01-10 | 2015-07-01 | 北京航空航天大学 | Electrochemical atomic force microscope probe carriage-electrolytic cell device |
| CN103852461B (en) * | 2014-03-28 | 2016-01-20 | 厦门大学 | A kind of galvanochemistry Tip-Enhanced Raman Spectroscopy instrument based on scanning probe microscopy |
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