46 results about "Scanning electrochemical microscopy" patented technology

Sensors and systems for electrical, electrochemical, or topographical analysis, as well as methods of fabricating these sensors are provided. The sensors include a cantilever and one or more probes, each of which has an electrode at its tip. The tips of the probes are sharp, with a radius of curvature of less than about 50 nm. In addition, the probes have a high aspect ratio of more than about 19:1. The sensors are suitable for both Atomic Force Microscopy and Scanning Electrochemical Microscopy.

The present invention discloses a method of manufacturing an ultra-microelectrode and is characterized by sealing the top end of a capillary tube by adopting a flame fusing method, plating a dielectric film by adopting a cyclic voltammetry method for the first time and obtaining the top end of an ultra-microelectrode by using an electric shock method. Comparing with the traditional technology, thepresent invention discloses an ultra-microelectrode having a top end with a minimum diameter of 300-1000nm, having a uniform compact uneasy-falling dielectric film, and the size is controllable, thesensitivity is high, the steady-state current is reduced from 10[-7]A to 10[-9]A, the ultra-microelectrode can be tested in an organic system, and thus, application fields of the ultra-microelectrodeis widened greatly. The method has characteristics of simple manufacturing and low cost, and the manufactured ultra-microelectrode has a perfect electrochemical performance and can be used for singlecell detecting and probes of scanning electrochemical microscopes.

The invention relates to a multifunctional electrolytic tank for a scanning electrochemical microscope, which comprises an upper cover, a lower cover and a double-layer cylinder, wherein the upper cover and the lower cover are concave, the inner side of the upper cover and the inner side of the lower cover are respectively provided with an internal thread I, two ends of the double-layer cylinder are respectively provided with an external thread II, the external threads II are matched with the internal threads I, the double-layer cylinder is internally provided with electrolyte solution. The upper cover, the lower cover and the double-layer cylinder are connected by the internal threads I and the external threads II; the upper cover is provided with a circular hole I, a circular hole II and a circular hole III; the circular hole I is internally provided with a working electrode; the circular hole II is inserted with a glass bent tube I; the circular hole III is inserted with a glass bent tube II, the upper part of the side wall of the double-layer cylinder is provided with a water outlet, the bottom of the side wall of the double-layer cylinder is respectively provided with a water inlet, a side branch tube I and a side branch tube II; and the side branch tube I and the side tube II are symmetrically arranged, and are respectively provided with a reference electrode and a counter electrode. The multifunctional electrolytic tank can complete the experiments of a three-electrode system, a four-electrode system and a complex electrode system through different structures of the lower cover, has a simple structure, is convenient to disassemble, and improves the research efficiency.

The invention discloses a method for manifesting latent fingerprints on the basis of an electrochemical luminescence marker. According to the method, an activated terpyridine ruthenium composite is used as the electrochemical luminescence marker; the activated terpyridine ruthenium composite can be subjected to covalent binding with an amino group in fingerprint amino acid through N-hydroxysuccinimide eater on a molecule, so that the terpyridine ruthenium composite is marked and fixed on the fingerprints; then the terpyridine ruthenium composite and a coreactant (namely dinormal-butyl ethanolamine) in a solution are subjected to electrochemical luminescence reaction under certain potential, so that lines of the fingerprints comprising the integral morphology (namely a primary structure) and detailed features (namely a secondary structure) are manifested; according to the adopted electrochemical luminescence technology, an excitation light source is not required to be added, back light is eliminated, a self-quenching phenomenon of a radiant agent is greatly avoided, and the method is obviously superior to the traditional fluorescence imaging method; and an image can be quickly acquired by an imaging technology, and the speed of acquiring the image by the imaging technology is far higher than the speed of acquiring the image by a scanning electrochemical microscopy; and the used electrochemical luminescence coreactant is dinormal-butyl ethanolamine, and has the characteristics of high luminous intensity and environment-friendliness.

The invention provides an SECM (scanning electrochemical microscope) experimental device for tests in various environments. The SECM experimental device comprises a square glass shield, a gas inlet tube, an exhaust tube, a carrying plate with an electrolytic tank, a glass shield cover plate, a probe, a reference electrode, a counter electrode, a plastic cone, a probe support and rubber sealing rings. The integral square glass shield is formed by means of pouring and comprises a front side plate, a rear side plate, a left side plate and a right side plate which are identical, the carrying plate with the electrolytic tank is mounted at the bottom of the square glass shield, and the glass shield cover plate is placed on the upper portion of the glass shield. The plastic cone with the probe support is fixed into a circular hole of the rear side plate of the square glass shield, the top of the plastic cone can move in front-rear, left-right and up-down directions, and the probe support on the plastic cone can drive the probe to perform scanning and testing in different regions of a working electrode; gas can be injected onto the device via the gas inlet tube, and scanning electrochemical tests can be performed in environments with gas, mixed gas, gas and liquid interfaces and the like. The SECM experimental device is suitable for scanning electrochemical test research on metal materials in the various environments.

The invention relates to an elimination method of the jump of a current fitting curve by a scanning electrochemical microscope on a liquid / liquid interface, comprising the steps as follows: (1) a liquid / liquid interface is established; (2) the probe of the scanning electrochemical microscope extends into an organic phase containing reduction-state species and is close to the liquid / liquid interface; the distance d from the probe to the interface and the current value of the probe are recorded; furthermore, the relationship curve between the distance d and the current value of the probe is established; (3) the distance d is standardized as L and the standardized probe current I<T><k> is fit; (4) the relationship curve of fit standardized distance and standardized current is established; (5) discrete wavelet transformation is carried out to the signals (L is more than 2) so as to extract the similar and detailed components; and (6) a minimum average detail discrete wavelet transformation method is used for eliminating the fitting current jump which is generated when L is more than 2. The invention provides the minimum average detailed discrete wavelet transformation method by the discrete wavelet transformation method, which solves the fitting current jump problem of the standard current theory fitting curve of the liquid / liquid interface at large standard distance value.

The invention discloses a photoelectrochemical kinetics test system and method based on a scanning electrochemical microscope. The system includes a scanning electrochemical microscope device, a Pt ultra microelectrode, a sample fixing device, a light source device and a rotary table control device. The scanning electrochemical microscope comprises a three-dimensional control device and an electrochemical workstation. The sample fixing device comprises a PTFE chemical tank and a fixed part. The light source device comprises a radiator, a DC power supply and red, yellow, blue and white LED light sources arranged on the edge of the radiator disc in order. The rotary table control device comprises a central processor, a disc with light through hole, a controller and a stepper motor. The invention can overcome the defect of insufficient information acquisition in the current solar cell and photoelectrocatalysis interfacial chemical reaction kinetics, quickly get accurate information of interfacial reaction kinetics, and provide strong experimental parameters for researching solar cells or photoelectrocatalysis water decomposition device.

The invention relates to a scanning electrochemical microscope electrolytic cell for plate-shaped load sample corrosion research. The electrolytic cell comprises an upper structure and a lower structure, which jointly form an electrolytic cell cavity; the center of the lower structure is provided with a groove; and the upper structure comprises a rectangular frame, the front side wall of the rectangular frame is made of transparent materials, and the left side wall and the right side wall of the rectangular frame are respectively provided with a groove which is communicated with the outside and the electrolytic cell cavity. The invention also relates to a method for corroding the plate-shaped samples by using the electrolytic cell. The structure of the plate-shaped sample transversely passing the electrolytic cell is particularly suitable for corrosion tests of metallic material samples which are stressed and loaded or have residual stress. Therefore, by the electrolytic cell and the application thereof, the plate-shaped sample is subjected to longitudinal mechanical loading by constant load loading or slow strain rate stretching, the real-time and in-situ research on the influence of metallic materials, corrosion medium and mechanical factors on corrosion characteristics and a corrosion rate of metallic materials under the synergistic action can be done, and the microcosmic mechanism on corrosion can be deeply analyzed.

The invention relates to a scanning electrochemical microscope sample stage for testing a multi-standard sample strip electrolytic cell. The sample stage is formed by a Teflon carrier plate (the electrolytic cell at the upper end) and a U-shaped support. The left end wall and the right end wall of the electrolytic cell are respectively provided with a round hole for placing a counter electrode anda reference electrode respectively. The U-shaped support is fixed by screws with the carrier plate. Cylindrical small rods are riveted into the carrier plate in the positive direction and the negative direction of the X-axis and the positive direction of the Y-axis. The bottom surface is provided with a circular groove, the carrier plate at the center of the electrolytic cell is provided with a circular hole and the circular groove, a rubber gasket is placed in the groove, a test sample is placed on the rubber gasket, and then a metal pressing piece is placed. Bolts on the U-shaped support are adopted for fixation, and a probe is used for scanning the sample at the circular hole. The sample stage is simple and quick in sample preparation, convenient to remove and capable of testing multi-standard samples under the premise that the sample integrity is maintained. The tested sample can be reused for other test analysis, the application field of the SECM is expanded, and the utilizationrate is improved.

A method for shape representation of hydrogel micro-pore arrays comprises the steps that firstly, a selected hydrogel material is polyethylene glycol dimethacrylate and an optical masking method and a template method are adopted for preparing the polyethylene glycol dimethacrylate hydrogel micro-pore arrays with different pore diameters and different pore depths; secondly, a scanning electrochemical microscope probe is prepared and a scanning electrochemical microscope detection system is established; finally, home position representation is conducted on the shape of the polyethylene glycol dimethacrylate hydrogel micro-pore arrays in an aqueous solution through a scanning electrochemical microscope. According to the method, natural oxygen couples in the aqueous solution serve as redox couples, home position representation is conducted on the shape of the polyethylene glycol dimethacrylate hydrogel micro-pore arrays in the aqueous solution through the scanning electrochemical microscope technology, two-dimensional pore diameter and three-dimensional shape information of the surfaces of the hydrogel micro-pore arrays is obtained, and the method has the advantages that home position representation, reversible representation and lossless representation can be conducted on a sample in the aqueous solution and the three-dimensional shape information of the hydrogel material can be obtained.

The invention discloses a method for detecting the photoelectric property of a microcell of a photoelectric material, and relates to the technical field of photoelectrochemistry. On the basis of a scanning electrochemical microscope device, an optical fiber microprobe and a microelectrode probe are adopted, and a sample microcell (including crystal grains, crystal boundaries and the like) is accurately scanned in a photoelectrochemical cell, so that the photoelectrochemical performance of the material microcell is obtained. According to the method for detecting the photoelectric property of microcell of a photoelectric material , the photoelectric property differences corresponding to different surface microstructures of the material microcell can be measured; and the photoelectric property distribution of grain boundaries and different grain orientations is detected, so that the limitation that only the overall macroscopic photoelectric property of the material can be measured in thetraditional method is eliminated. The method has important guiding significance for photoelectric conversion mechanism research and process performance improvement.

The invention relates to a method for using a scanning electrochemical microscope (SECM) in coordination with silver staining to collect latent blood fingerprint image in a high-resolution way and belongs to the technical field of fingerprint identification. The method includes: using the principle that Ag+ ions combines with protein components in the blood of the ridge line are of a fingerprint and is reduced to Ag nano particles with electrochemical activity instead of reacting with the substrate in the valley line area to allow the fingerprint ridge line area and the fingerprint valley line area to form electrochemical activity difference; adding redox medium K3IrCl6 to solution, using the principle that the K3IrCl6 reacts with the Ag metal particles in the ridge line area to generate positive feedback effect instead of reacting with the valley line area to perform blood finger print collection based on SECM. The method has the advantages that image resolution is high, third-level fingerprint information can be collected, and the ideal latent blood fingerprint high-resolution image collecting method is promising in application prospect in the field of fingerprint identification.

The invention relates to a simple and feasible scanning electrochemical microscope test method. The method comprises the following steps: processing a large-sized electrolytic tank made of a polytetrafluoroethylene material, and stably sealing a test sample by using thermosol. The test sample has the characteristics of fast curing, non-pollution, non-toxic and high viscous force, has certain hardness, flexibility and re-viscidity, can be heated and melted again for use. The electrolytic tank is stabilized on a sample stage loading plate, and the edge of the test sample placed at the bottom ofthe electrolytic tank is sealed by using the thermosol. By adoption of the simple and feasible scanning electrochemical microscope test method provided by the invention, large-sized samples with multiple specifications can be tested, the maximum test area is 50mm*50mm, and the test sample can be a metal substrate, a test sample with film layer and coating and other test samples subject to other experiments, and can be square, circle, block, plate and other shapes. After the test is completed, the sample can be taken out just by smelting the thermosol again, thereby ensuring the integrity and reusability of the sample, improving the utilization rate of SECM and expanding the application scope and field of the SECM. The test method is simple and feasible and is easy to operate.

The invention provides an electrochemical detection device for scanning the appearance of a local area. The electrochemical detection device comprises a bipotentiostat, a probe signal receiving device, a lock-in amplifier, a sample signal collector, an electrolyzer horizontal knob, a test probe, a sample fixing table, a reference electrode, a test electrolyzer, an electrolyzer upper cover, a counter electrode and a computer. The electrochemical detection device overcomes the defects of weak signals, difficulty in acquiring of feedback current density signals, and single detection signals of conventional scanning electrochemical microscopes, and can acquire local microcosmic impedance distribution characters of sample surfaces and abundant information, so that the device is beneficial for researching and analyzing the true character of s sample.

The invention provides a preparation method for an isolated needle point with housing layers wrapped in dual manner, which relates to a scanning probe. The method comprises the following steps: 1) using a chemical etching method to prepare a needle point; 2) wrapping the surface of the needle point with a housing layer; and 3) using high polymer materials to package the part of the needle point wrapped by the housing layer in step 2 excluding the needle point end for a second time to obtain an isolated needle point with the housing layers wrapped in a dual manner. According to the invention, an atomic layer deposition technique is adopted and different source precursors are used so that the needle point surface can be wrapped by different inert housings. Through the control over the number of circulation turns of different source precursors, the thickness of the housing layer can be accurately controlled. The wrapping in dual manner can prevent the non-analyte molecules in the solution from interfering with the signal generated at the needle point and can isolate the interference of the Faraday current. Therefore, the method can be applied to electrochemical needle-enhanced Raman spectroscopy, electrochemical scanning tunneling microscope and electrochemical scanning microscope. Capable of being universally applied, the method can also be used to the wrapping of other needle points, like silver needle points, AFM needle points, and platinum iridium needle points. The method is simple to perform and is suitable for large batch production.

The invention relates to an electrochemical micromachining method for a ZnO substrate with a high-frequency AC electric heating technology. The method is characterized in that the method comprises the following steps: 1, preparing a corrosion solution containing NaNO2; 2, providing a high-frequency AC electric heater and a scanning electrochemical microscope (SECM), and fixing the heating microelectrode of the high-frequency AC electric heater on the SECM; and 3, putting a nano-wire or a film for synthesizing ZnO in the corrosion solution as a micromachining substrate, allowing the heating microelectrode to approach the ZnO substrate through the approximation device of the SECM, and adjusting the temperature of the heating microelectrode to carry out micromachining on the ZnO substrate. The method of the invention, which has the advantages of electrochemical micromachining efficiency improvement, controllable machining resolution and simplicity, has a good practicable value.

The invention provides a method for preparing a working electrode of a scanning electrochemical microscope. The method for preparing the working electrode of the scanning electrochemical microscope is characterized in that by utilizing the characteristics of non-polarity and low melting point of paraffin, paraffin is used for manufacturing a paraffin mould with the inner diameter equal to the outer diameter of the working electrode in a pouring mode according to the size of standard the working electrode of the scanning electrochemical microscope provided by a manufacture factory; a sample to be tested is put in the center of the paraffin mould; a prepared liquid epoxy resin solution is poured into a gap between the paraffin mould and the sample to be tested; after an insulation layer material solution is solidified, namely insulation layer materials and the sample to be tested are melted into a whole, the sample to be tested with the insulation layer materials is pulled out, the operations of coarse grinding, fine grinding and fine polishing are carried out on the sample to be tested, the sample to be tested is cleaned with acetone and anhydrous ethanol and then is dried, and the working electrode of the scanning electrochemical microscope is obtained. Through the method for preparing the working electrode of the scanning electrochemical microscope, the working electrode which is the same as the standard electrode of the scanning electrochemical microscope in shape, size and dimension is prepared simply and rapidly.

The invention discloses a barrier probe provided with a solid dielectric film on a probe point, and belongs to the probe design field of scanning probe microscopes. According to the technical schemes, the barrier probe provided with the solid dielectric film on the probe point comprises a conductive probe used for a scanning probe microscope, the conductive probe is formed by a conductive probe body and a conductive probe point arranged on a free end of the conductive probe body, and the conductive probe point is covered by at least one layer of solid dielectric film. The requirements on the hardness and chemical activity of a probe conductive material are not high, the wear resistance is good, the resolution is high, and the barrier probe is especially applicable to a scanning electrochemical microscope, a conductive atomic force microscope and a contact-mode scanning tunnel microscope and is simultaneously applicable to other scanning probe microscopes of existing modes.

The invention discloses an SECM-based test system for corrosion of a buried metal pipeline and stripping of an anti-corrosion layer. The ECM-based test system comprises an AC stray current loading system, an electrolytic tank system and a scanning electrochemical microscope test system, wherein the AC stray current loading system is used for providing an interference source of an AC stray currentfor the buried metal pipeline, the electrolytic tank system is used for simulating actual engineering conditions of the buried metal pipeline under different soil environments, and the scanning electrochemical microscope test system is used for acquiring a local microregion image and charge transfer characterstic of a breakage point of the anti-corrosion layer during the metal corrosion process under an effect of the stray current and analyzing data. The test system can be used for simulating local pipeline corrosion and stripping of the anti-corrosion layer caused by the stray current flowinginto / out of the breakage point of the anti-corrosion layer of the buried metal pipeline under different soil environments, stray current intensity, anti-corrosion layer types and breakage area ratiosof the anti-corrosion layer.

The invention discloses a scanning electrochemical microscope, which comprises a three-dimensional ball screw scanner, a three-dimensional piezoelectric scanner, a conductive probe, a conductive substrate, a working platform and a micro-control unit, and is characterized in that the three-dimensional ball screw scanner comprises an X adjusting shaft, a Y adjusting shaft and a Z adjusting shaft; every two of the X adjusting shaft, the Y adjusting shaft and the Z adjusting shaft are perpendicular to each other; the X adjusting shaft is arranged on the working platform; the three-dimensional piezoelectric scanner is arranged on the Z adjusting shaft; according to the scheme, a ball screw scanner, a piezoelectric scanner, a conductive probe, a conductive substrate and a micro-control unit which are high in stability are integrated in the scanning electrochemical microscope; the scanning range and linearity of the piezoelectric scanner are corrected through the ball screw scanner, use of aprecise distance testing instrument or a standard sample is avoided, and the advantages of being easy and convenient to operate and low in cost are achieved.

A new scanning electrochemical microscopy tip positioning method that allows topography and surface activity to be resolved independently is presented. A SECM tip is oscillated relative to the surface of interest. Changes in the oscillation amplitude, caused by the intermittent contact of the SECM tip with the surface of interest, are used to detect the surface of interest, and as a feedback signal for various types of imaging.

A new scanning electrochemical microscopy tip positioning method that allows topography and surface activity to be resolved independently is presented. A SECM tip is oscillated relative to the surface of interest. Changes in the oscillation amplitude, caused by the intermittent contact of the SECM tip with the surface of interest, are used to detect the surface of interest, and as a feedback signal for various types of imaging.

The invention discloses an electrolytic cell with a four-electrode system and applied to scanning electrochemical microscopes. The electrolytic cell comprises a cell body and an upper cover, and the upper cover is provided with two through holes; the upper-half parts and the lower-half parts at two sides of the cell body are respectively connected with two groups of capillaries, and each group of capillaries comprises two oppositely-arranged half-U-shaped capillaries; and the upper openings of all half-U-shaped capillaries are at a same horizontal height, and the ends of two half-U-shaped capillaries at one side go deep to the cell body and are provided with two face-to-face end openings. The electrolytic cell is capable of overcoming influences caused by electrode polarization and environment fluctuation and effectively eliminating contact impedance and line impedance, avoiding the problem that a subsequently-injected liquid is polluted when liquid-liquid interface research is performed, and enabling the formed liquid-liquid interface to be relatively clear and flat. The electrolytic cell is applicable to research on a liquid-liquid interface with an aqueous solution at the upper layer and also is applicable to research on a liquid-liquid interface with an aqueous solution at the lower layer. An upper-layer liquid is not damaged when a reference electrode and a counter electrode are inserted, so that the electrolytic cell is relatively widely applicable to liquid-liquid interface research systems.

The invention provides a double-electrolytic-cell device for micro-area electrochemical test and a using method thereof. The device comprises a hydrogen charging mechanism, a micro-area electrochemical testing mechanism and a gas collecting mechanism, and the hydrogen charging mechanism comprises a hydrogen charging cell, an observation mirror, a liquid inlet, a top plate, a hydrogen charging hole, an auxiliary electrode, a reference electrode, a lower sealing ring and an upper sealing ring; a sample is arranged between the lower sealing ring and the upper sealing ring, a hydrogen filling solution is loaded in the hydrogen charging cell, and the hydrogen filling solution is in contact with the lower surface of the sample; the micro-area electrochemical testing mechanism comprises an electrochemical workstation, a detection pool, a detection hole, a micro reference electrode and a platinum electrode probe; the detection pool is fixed on the top plate, and a hydrogen charging hole of thedetection pool is opposite to a detection hole of the detection pool; and when the sample is filled with hydrogen, the gas collecting mechanism discharges bubbles on the lower surface of the sample.According to the invention, a double-electrolytic-cell structure is adopted, preparation and installation processes of an experimental sample are simplified, hydrogen charging and in-situ micro-area electrochemical testing of the sample are realized, and application of the scanning electrochemical microscope in the field of hydrogen permeation research is expanded.

The invention discloses a scanning electrochemical microscope system and a control method thereof, which are applied to a scanning electrochemical microscope technology. The system comprises a probe used for detecting an electric signal, a probe positioning system which is used for driving the probe to move, a double potentiostat which is used for applying a test signal to the probe and detectinga feedback signal of the probe, and a computer which is used for controlling the probe positioning system to drive the probe to move, controlling the double potentiostat to apply a long-time potentialor at least two test signals with different potential levels to the probe when the probe stays at a detection position, and recording feedback signals corresponding to each test signal, and obtaininga scanning image corresponding to each potential level according to the feedback signals of all the detection positions with the same potential level. Compared with the prior art, efficiency is higher, and more test data can be obtained by scanning each time.

A method for characterizing the morphology of hydrogel micropore arrays. The hydrogel material selected first is polyethylene glycol dimethacrylate, and photomask method and template method are used to prepare The polyethylene glycol dimethacrylate hydrogel microwell array; then prepare the scanning electrochemical microscope probe and build the scanning electrochemical microscope detection system; finally apply the scanning electrochemical microscope to detect the polyethylene glycol dimethacrylate in the aqueous solution In situ characterization process of ester hydrogel microporous array morphology. In the present invention, the natural electron pair oxygen in the aqueous solution is used as the reducing pair, and the morphology of the polyethylene glycol dimethacrylate hydrogel micropore array in the aqueous solution is characterized in situ by using scanning electrochemical microscopy technology, and the water The two-dimensional pore size and three-dimensional shape information on the surface of the gel micropore array has the advantages of in-situ, reversible and non-destructive characterization of the sample in aqueous solution and gives the three-dimensional shape information of the hydrogel material.

The invention provides a method for preparing a working electrode of a scanning electrochemical microscope. The method for preparing the working electrode of the scanning electrochemical microscope is characterized in that by utilizing the characteristics of non-polarity and low melting point of paraffin, paraffin is used for manufacturing a paraffin mould with the inner diameter equal to the outer diameter of the working electrode in a pouring mode according to the size of standard the working electrode of the scanning electrochemical microscope provided by a manufacture factory; a sample to be tested is put in the center of the paraffin mould; a prepared liquid epoxy resin solution is poured into a gap between the paraffin mould and the sample to be tested; after an insulation layer material solution is solidified, namely insulation layer materials and the sample to be tested are melted into a whole, the sample to be tested with the insulation layer materials is pulled out, the operations of coarse grinding, fine grinding and fine polishing are carried out on the sample to be tested, the sample to be tested is cleaned with acetone and anhydrous ethanol and then is dried, and the working electrode of the scanning electrochemical microscope is obtained. Through the method for preparing the working electrode of the scanning electrochemical microscope, the working electrode which is the same as the standard electrode of the scanning electrochemical microscope in shape, size and dimension is prepared simply and rapidly.