CN113533787B - Atomic force microscope-based electrochemical reaction process in-situ monitoring device and monitoring method thereof - Google Patents
Atomic force microscope-based electrochemical reaction process in-situ monitoring device and monitoring method thereof Download PDFInfo
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Abstract
The invention discloses an atomic force microscope-based electrochemical reaction process in-situ monitoring device and a monitoring method thereof. The testing device is realized by taking a local gold-plated silicon wafer as a working electrode, and taking a silver wire and a platinum wire as a reference electrode and a counter electrode respectively; the method is suitable for various electrochemical processes, such as the fields of electrochemical deposition, electrochemical corrosion, electrochemical synthesis and the like, and can be used for carrying out in-situ detection on the change of an electrochemical interface according to time, applied potential, reaction species concentration and environmental conditions such as temperature, humidity, pH, atmosphere and the like. The invention can obtain the electrochemical evolution information on the micro interface which can not be obtained by the conventional method, which is helpful for the deep understanding of the electrochemical reaction mechanism.
Description
Technical Field
The invention belongs to the technical field of electrochemical testing, relates to an electrochemical atomic force microscope in-situ monitoring device and a monitoring method thereof, and particularly relates to an electrochemical deposition and corrosion in-situ imaging method and device based on an atomic force microscope.
Background
Electrochemical processes generally refer to electrochemical oxidation and reduction reactions that occur at the surface of a solid in a particular electrolyte solution, the reaction rate of which strongly depends on: (i) Mass transport of reactive species from bulk solution to solid-liquid interface; (ii) The rate of electron transfer between the electrolyte and the metal surface. Therefore, a thorough understanding of the relationship between surface reactivity and solid-liquid interface morphology is crucial for effective control of electrochemical processes.
In particular, the electrochemical deposition and corrosion process controlled by specific conditions has independent control on the engraving shape/sizeThe nano particles with special structures have unique application prospects. For example, the electrochemical design of micro/nano structure can be researched by controlling the electro-corrosion process in the electrodeposition growth process, so as to controllably prepare the cage-shaped silver oxide Ag 7 O 8 NO 3 The structure has application prospect in the fields of being used as a substrate of Surface Enhanced Raman Scattering (SERS) sensing, visible light sensitive photocatalysis and the like. However, the optimization of the control conditions involved in the electrochemical engraving process, especially the law of influence on the nanoparticle growth mechanism, remains extremely challenging.
The conventional characterization technique is usually tested under ex-situ conditions, which only can test the sample state before and after the electrochemical reaction starts, and the analysis result is unreliable due to local differences and randomness, so that the intervention of the in-situ characterization technique without space-time limitation is required for further study of the electrochemical mechanism, especially the nanoparticle growth mechanism in the electrochemical deposition and corrosion processes. However, conventional morphology observation such as in-situ transmission electron microscope and in-situ scanning electron microscope is very harsh to the reaction environment of the observed object, and especially for an electrochemical system in a solution system, the in-situ observation is very difficult due to the requirements of electrolyte, atmosphere and operation space.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention is directed to developing a widely applicable in-situ visual monitoring technique for electrochemical processes.
The electrochemical reaction process in-situ monitoring device based on the atomic force microscope is an in-situ testing device with controllable specific conditions, and the atomic force microscope and the electrochemical workstation are used for measuring the derivative of the microstructure of the electrochemical interface in a combined mode. The method takes a specific conductive gold substrate as a working electrode, a silver wire as a reference electrode and a platinum wire as a counter electrode, and is controlled by an electrochemical workstation in a designed in-situ electrochemical liquid pool to realize the proceeding of the electrochemical reaction process and monitor the change of the microstructure morphology on the surface of the working electrode in real time by an atomic force microscope.
An in-situ monitoring device for an electrochemical reaction process based on an atomic force microscope comprises a Faraday shielding box, a shock-proof device arranged in the Faraday shielding box, the atomic force microscope arranged in the shock-proof device, an electrochemical workstation, an in-situ electrochemical liquid pool, an environmental chamber and a heating sample stage. The device can realize the in-situ monitoring of the electrochemical process under various specified conditions: the conditions of the concentration of reaction species, the acidity and the alkalinity of the electrochemical reaction and the like can be controlled by the components of the electrolyte additive in the in-situ electrochemical liquid pool; the protective atmosphere of the electrochemical reaction can be controlled through the environmental chamber, and the temperature and other conditions of the electrochemical process can be changed through heating the sample table. The Faraday shielding box can prevent the reaction system from being interfered by electromagnetic signals; the shockproof device can ensure the stability of the atomic force microscope test; the atomic force microscope is used for monitoring the surface morphology and the electric property evolution of the electrode; the electrochemical workstation is used for controlling the electrochemical reaction voltage.
The invention also provides an in-situ monitoring method of the electrochemical reaction process based on the atomic force microscope, which is realized based on the device, and comprises the steps of preparing a working electrode by thermally evaporating a conductive chromium-gold plating layer with a specific shape (T shape) and thickness on a silicon wafer substrate, cleaning the surface of the working electrode by using deionized water and ethanol, and drying the working electrode by using nitrogen for later use; silver wires with AgCl coatings on the surfaces and platinum wires are respectively used as a quasi-reference electrode and a counter electrode and are fixed on an in-situ electrochemical liquid pool by thermosetting adhesive; fixing an in-situ electrochemical liquid pool on a heating sample table loaded with a working electrode through an O ring and a spring clamp, adding a proper amount of electrolyte, and integrally loading the in-situ electrochemical liquid pool on an atomic force microscope with an environmental cavity to be tested; selecting an atomic force microscope probe with proper parameters such as elastic coefficient, coating, resonance frequency and the like according to different electrochemical reaction systems, and pre-scanning the surface of the working electrode through the atomic force microscope; connecting an electrochemical workstation and setting a specific program to perform electrochemical tests, including a chronoamperometry, a cyclic voltammetry and an electrochemical alternating-current impedance test; suspending an electrochemical test program at a specified time according to the reaction process, and scanning the electrode morphology by using an atomic force microscope; after the scanning is finished, the electrochemical process is continued, and the in-situ electrochemical morphology monitoring can be carried out at any time until the electrochemical reaction process is finished.
The invention is based on atomic force microscopy and develops a widely applicable in-situ monitoring device for electrochemical processes, which allows real-time and in-situ detection of the evolution of the solid-liquid interface in electrochemical processes under specific environmental conditions (atmosphere, temperature, pH).
An Atomic Force Microscope (AFM) can characterize the surface morphology and other interface properties of a sample through weak interaction Force between a probe tip and the sample to be detected, has no harm to the surface of the sample in a detection process, does not interfere a reaction process, has no strict requirement on a reaction environment, and is an ideal in-situ electrochemical characterization selection. When the AFM controls the tip to scan, the attractive or repulsive interaction with the sample surface will change as the distance between the two changes, causing deformation of the microcantilever. The degree of deformation of the microcantilever, which is directly related to the magnitude of the tip-sample interaction force, can be determined by the coupling of the laser reflection at the back of the microcantilever of the probe and the photodetector. When the deformation of the micro-cantilever is 0.01nm, after the laser is reflected to the detector, the micro-cantilever becomes 3-10nm displacement and generates a voltage difference signal which can be detected, and the surface information of the sample can be obtained by recording the voltage signal of the detector which changes along with the scanning position.
In the invention, the electrochemical reaction process in-situ monitoring method based on the atomic force microscope has two typical modes: (i) In the non-conductive probe mode, a silicon nitride probe without a coating is used as an atomic force microscope probe to realize in-situ monitoring of the morphology of the electrochemical interface; (ii) The probe mode of the tip conduction uses an atomic force microscope probe only with a Pt-plated tip conduction and other parts insulation to realize the simultaneous characterization of the electrochemical interface morphology and the electric properties such as surface current and potential information derivation.
The invention has the beneficial effects that:
according to the invention, the atomic force microscope and the electrochemical workstation are used in a combined manner, so that the problems of test time limitation and inconsistent test areas in the traditional ex-situ morphology characterization are solved, and the in-situ analysis and monitoring can be carried out on the electrochemical reaction solid-liquid interface in the same area at any time.
Drawings
FIG. 1 is a schematic structural diagram of an in-situ electrochemical reaction monitoring device according to the present invention;
FIG. 2 is a flow chart of the loading preparation of the heated sample plate and the working electrode;
FIG. 3 shows Ag 7 O 8 NO 3 The in-situ electrochemical deposition and the morphology of the corrosion process are evolved;
the system comprises a gas steel cylinder 1, an atomic force microscope control system 2, a laser detector 3, a laser emitter 4, an environment cavity 5, an electrochemical testing system 6, an electrochemical workstation 7, a vibration-proof device 8, a Faraday shielding box 9, a heating sample table 10, a heating plate 11, an in-situ electrochemical liquid pool 12, an O ring 13, a working electrode 14, an electrolyte 15, a reference electrode 16 and a counter electrode 17.
Detailed Description
An in-situ monitoring device for an electrochemical reaction process based on an atomic force microscope comprises a Faraday shielding box 9, a shockproof device 8 arranged in the Faraday shielding box 9, the atomic force microscope arranged in the shockproof device 8, an electrochemical workstation, an in-situ electrochemical liquid pool 12, an environmental chamber 5 and a heating sample table 10. The device can realize the in-situ monitoring of the electrochemical process under various specified conditions: the conditions of the concentration of the reactive species, the acidity and alkalinity, etc. of the electrochemical reaction can be controlled by the components of the electrolyte additive in the in-situ electrochemical liquid cell 12; the protective atmosphere of the electrochemical reaction can be controlled by the environmental chamber 5, and the temperature of the electrochemical process can be changed by heating the sample stage 10. The heating plate 11 is arranged on the heating sample table 10 and used for changing the temperature in the reaction process. The Faraday shielding box 9 can prevent the reaction system from being interfered by electromagnetic signals; the shockproof device 8 can ensure the stability of the atomic force microscope test; the atomic force microscope is used for monitoring the surface appearance and the electric property variation of the electrode 17; the electrochemical workstation is used for controlling the electrochemical reaction voltage. As in figure 1 the atomic force microscope control system 2 comprises a laser detector 3 and a laser emitter 4.
The electrochemical reaction process in-situ monitoring device based on the atomic force microscope is provided with a three-electrode in-situ electrochemical liquid pool 12, as shown in figure 1, a working electrode 14 of the electrochemical reaction process in-situ electrochemical liquid pool is a gold-plated silicon wafer substrate for the electrochemical reaction process, and a reference electrode 16 and a counter electrode 17 respectively adopt a silver wire and a platinum wire. Both the AFM tip and the three-electrode system described above were immersed in an electrolytic solution to allow in situ imaging of the electrochemical reaction. Depending on the polarization of the tip, there can be two different modes: a non-conductive probe mode and a conductive probe mode. The former uses a non-conductive AFM probe, such as a silicon nitride probe without a coating, to monitor the evolution of the in-situ surface morphology; the latter, in turn, enables simultaneous measurement of surface morphology (i.e., height images) and its distribution of electrochemical reactivity (i.e., current images) by using tip-conducting, otherwise insulated nanoelectrodes as atomic force microscope probes.
The in-situ AFM monitoring device can be applied to a plurality of electrochemical scenes, including but not limited to actions such as electrochemical deposition, electrochemical corrosion, electrochemical synthesis and the like. Below with Ag 7 O 8 NO 3 The actual application of the in-situ AFM electrochemical reaction process monitoring device and the detection method disclosed by the invention is shown by the competitive process of in-situ electrochemical deposition and corrosion:
apparatus and materials
Atomic force microscope (Agilent 5500), electrochemical workstation (Woogton PGSTAT302N, switzerland), 0.06M AgNO 3 Electrolyte and 0.16M H 3 BO 3 And (3) an additive.
Preparation of in situ electrochemical reaction device
In order to ensure that the electrochemical reaction process aggregation occurs in the probe area, the working electrode 14 in the shape shown in fig. 2 is designed, and specifically, the working electrode 14 is obtained by firstly evaporating a chromium layer with a thickness of 10nm and then evaporating a gold layer with a thickness of 50nm in a specified area on a flat silicon wafer.
Silver wires and platinum wires with AgCl coatings are respectively used as a reference electrode 16 and a counter electrode 17 and are fixedly arranged on the in-situ electrochemical liquid pool 12 through glue.
An O-ring 13 is placed between the in situ electrochemical liquid cell 12 and the working electrode 14 on the silicon wafer and compressed using a spring, and about 800 μ L of electrolyte 15 is added, taking care to prevent leakage of the electrolyte 15.
Electrochemical reaction condition control
In the electrochemical process, two processes of electrochemical deposition and electrochemical corrosion exist at the same time, and in order to research the competitive mechanism of the two processes, each possible influence factor needs to be regulated and controlled: injecting a specified quantity of AgNO into the in situ electrochemical liquid cell 12 3 Electrolyte 15 and H 3 BO 3 The additive can control the concentration of the reactants and the pH environment of the electrolyte 15; the conditions such as electrochemical reaction voltage (1.5V, 3V, 6V), reaction time (0-300 s) and the like can be controlled through an electrochemical workstation; the temperature (-30 ℃ to 250 ℃), the gas atmosphere (oxygen, argon, air), the pressure range, etc. of the electrochemical reaction can be adjusted by heating the sample stage 10 and the environmental chamber 5 (the gas cylinder 1 stores the required gas).
Atomic force microscope testing
In order to monitor the electrochemical reaction process in real time, the electrochemical test process can be suspended at any time, and the atomic force microscope is used for controlling the probe to move so as to realize the test of the evolution of the appearance or the electrical property of the electrochemical solid-liquid interface, the atomic force microscope test adopts a tapping mode, the probe in the test selects a non-conductive probe without a metal coating layer with the resonance frequency of about 80kHz, the test of a appearance graph and the scanning region of an impedance spectrum are 10um by 10um, the scanning speed is 0.5lines/s, and the imaging resolution is 256 x 256 pixels.
FIG. 3 shows Ag 7 O 8 NO 3 Firstly, under the voltage of 3V, the continuous deposition is respectively carried out on the same particle under each time length as shown in figure 3. It can be seen that at 10ms deposition, a small particle appears on the electrode, with a pronounced peak shape with a longest dimension of about 1.25 μm, as can be seen from the height profile along the longest dimensionA maximum height of about 379nm; after 40ms of deposition, the longest length of the particle is reduced by about 20nm, the height is reduced by about 23nm, the profile at the longest length ratio is changed into a gentle hill shape from an obvious convex peak shape, when the deposition time is continuously prolonged to 1s, the profile at the longest length ratio is greatly different, the hill shape is changed into a sharp peak plane again, the height is increased to 401nm, then the deposition time is prolonged to longer 60s and 300s, the particle is not grown, and the height and the length at the longest length ratio are both obviously reduced and changed in hundreds of nanometers. Therefore, focusing on the evolution of single particle growth in the micro-region, it can be observed in situ that the particles increase and decrease during the deposition process, and in the process of continuous variation, the situation that partial extinction exists for the single particles during the electrodeposition process is illustrated.
Claims (2)
1. An in-situ monitoring method for an electrochemical reaction process based on an atomic force microscope is realized based on an in-situ monitoring device for the electrochemical reaction process based on the atomic force microscope, and is characterized in that the device comprises a Faraday shielding box, a shockproof device arranged in the Faraday shielding box, the atomic force microscope arranged in the shockproof device, an electrochemical workstation, an in-situ electrochemical liquid pool, an environmental chamber and a heating sample table; the atomic force microscope is used for monitoring the surface appearance and the derivative of the electrical property of the electrode; the electrochemical workstation is used for controlling the electrochemical reaction voltage; the heating sample stage is used for changing the temperature condition of the electrochemical process; the environment cavity is used for controlling the protective atmosphere of the electrochemical reaction; the in-situ electrochemical liquid pool is fixed on the heating sample table, and the heating sample table is placed in the environmental cavity, so that the regulation and control of the concentration, pH, temperature and humidity, atmosphere and pressure of reaction species involved in the electrochemical reaction process are realized;
the method specifically comprises the following steps: preparing a working electrode by thermally evaporating a T-shaped conductive chromium-gold coating on a silicon wafer substrate, cleaning the surface of the working electrode by using deionized water and ethanol, and drying the surface of the working electrode by using nitrogen for later use; silver wires and platinum wires with AgCl coatings on the surfaces are respectively used as a quasi-reference electrode and a counter electrode, and are fixed on an in-situ electrochemical liquid pool by thermosetting adhesive; fixing an in-situ electrochemical liquid pool on a heating sample table loaded with a working electrode through an O ring and a spring clamp, adding a proper amount of electrolyte, and integrally loading the in-situ electrochemical liquid pool on an atomic force microscope with an environmental cavity to be tested; selecting an atomic force microscope probe according to different electrochemical reaction systems, and prescanning the surface appearance of the working electrode by using the atomic force microscope; connecting an electrochemical workstation and setting a specific program to carry out electrochemical tests, including a chronoamperometry, a cyclic voltammetry and an electrochemical alternating-current impedance test; suspending an electrochemical test program at a specified time according to the reaction process, and scanning the electrode morphology by using an atomic force microscope; after the scanning is finished, continuing the electrochemical process and monitoring the in-situ electrochemical morphology at any time until the electrochemical reaction process is finished;
the scanning region of the test and impedance spectrum of the atomic force microscope topography is a region of 10 Mum by 10 Mum, the scanning speed is 0.5lines/s, and the imaging resolution is 256 pixels by 256;
the T-shaped conductive chromium-gold plating layer is thermally evaporated on the silicon wafer substrate, specifically, a chromium layer with the thickness of 10nm is evaporated, and then a gold layer with the thickness of 50nm is evaporated.
2. The atomic force microscope-based electrochemical reaction process in-situ monitoring method according to claim 1, characterized in that: there are two typical modes: (i) In the non-conductive probe mode, a silicon nitride probe without a coating is used as an atomic force microscope probe to realize in-situ monitoring of the morphology of the electrochemical interface; (ii) The tip conducting probe mode uses an atomic force microscope probe with only tip conducting and the rest parts insulated to realize the simultaneous characterization of the electrochemical interface morphology and the electrical properties.
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