CN116514051B - Microelectrode preparation method and microelectrode - Google Patents

Microelectrode preparation method and microelectrode Download PDF

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CN116514051B
CN116514051B CN202310302879.4A CN202310302879A CN116514051B CN 116514051 B CN116514051 B CN 116514051B CN 202310302879 A CN202310302879 A CN 202310302879A CN 116514051 B CN116514051 B CN 116514051B
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insulating sleeve
metal probe
microelectrode
tip
sleeve
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CN116514051A (en
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李哲
左安昊
方儒卿
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Tsinghua University
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Tsinghua University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/06—Insulating conductors or cables
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B1/00—Devices without movable or flexible elements, e.g. microcapillary devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/307—Disposable laminated or multilayered electrodes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/0009—Details relating to the conductive cores
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/02—Disposition of insulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2203/00—Basic microelectromechanical structures
    • B81B2203/04—Electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a microelectrode preparation method and a microelectrode. The preparation method of the microelectrode comprises the following steps: placing a metal probe in an insulating sleeve; heating the insulating sleeve at the tip of the metal probe; pulling the insulating sleeve along the axial direction of the insulating sleeve to break the insulating sleeve at the needle point and expose the needle point; the rest of the insulating sleeve is melted and adhered to the outer wall of the metal probe to form an insulating layer. The microelectrode is prepared by adopting the metal probe, the metal probe is provided with the tip, the insulating sleeve is sleeved on the outer wall of the metal probe by adopting the heating stretching method, so that an insulating layer is formed on the outer wall of the metal probe, the tip of the metal probe is exposed, the metal probe can be used as the microelectrode without polishing, the preparation process is simplified, the problem of breakage caused by polishing is avoided, and the preparation difficulty is reduced. Meanwhile, the manufacturing cost can be reduced, and the preparation of the microelectrode is convenient.

Description

Microelectrode preparation method and microelectrode
Technical Field
The invention relates to the technical field of electrochemical microelectrodes, in particular to a microelectrode preparation method and a microelectrode.
Background
In electrochemical studies, microelectrodes are often required to measure the reactivity at the reaction interface sites. In addition, the microelectrode can be directly connected with an electrode material on the metal surface with extremely small size and used for measuring the reaction characteristics of the electrode material under microscopic conditions. Therefore, a metal having a small feature size is required as a probe to realize the function of the microelectrode. In general, only a part of the metal probe with a very small tip is exposed for electrochemical experiments, and the rest part of the metal probe is coated with an insulating layer to avoid contact with electrolyte and only serves as a current collector for providing electrons.
In the traditional scheme, a platinum wire (with the diameter of more than 10 micrometers) is generally adopted as a metal carrier, and polytetrafluoroethylene or glass is coated on the whole platinum wire. And (3) cutting off the whole platinum wire, and polishing and grinding the tip of the platinum wire to make the surface smooth, thereby obtaining the microelectrode. When the platinum wire is adopted to manufacture the microelectrode, the surface of the platinum wire is required to be polished, the operation process is complex, in addition, the platinum wire is extremely easy to break in the processing process, and the preparation process difficulty is high. In addition, some researchers have coated the surface with an amorphous fluororesin solution, but the coated probe needs to be cut by a FIB/SEM (focused ion beam scanning electron microscope) instrument, which is costly, and thus the processing cost of the solution is high.
That is, the existing microelectrode has the problems of complex preparation process, great difficulty and high cost, and is inconvenient for forming and manufacturing the microelectrode.
Disclosure of Invention
Based on the above, it is necessary to provide a microelectrode preparation method and a microelectrode which can simplify the preparation process and reduce the preparation difficulty and the production cost, aiming at the problems of complex preparation process, high difficulty and high cost of the conventional microelectrode.
A method of preparing a microelectrode comprising:
Placing a metal probe in an insulating sleeve;
Heating the insulating sleeve at the tip of the metal probe;
Pulling the insulating sleeve along the axial direction of the insulating sleeve to break the insulating sleeve at the needle point and expose the needle point;
The rest of the insulating sleeve is melted and adhered to the outer wall of the metal probe to form an insulating layer.
In one embodiment, the step of placing the metal probe in the insulating sleeve comprises:
Determining the length of the insulating sleeve which coats the metal probe;
A marking point is arranged at the position of the insulating sleeve corresponding to the tip of the metal probe;
and inserting the tip of the metal probe into the insulating sleeve from one end of the insulating sleeve, and aligning the tip with the marking point.
In one embodiment, the step of heating the insulating sleeve at the tip of the metal probe comprises:
Placing a heating device below the insulating sleeve and aligning the heating device to the marking point;
Controlling the heating device to heat the insulating sleeve at the marked point.
In one embodiment, pulling the insulating sleeve in an axial direction of the insulating sleeve includes the steps of:
holding an end of the insulating sleeve away from the metal probe;
pulling the insulating sleeve away from the metallic probe breaks the insulating sleeve at the marked point.
In one embodiment, the step of heating the insulating sleeve at the tip of the metal probe comprises:
Placing the insulating sleeve in a needle drawing instrument;
The heating point of the heater of the needle drawing instrument is aligned with the marking point;
The heater heats the insulating sleeve.
In one embodiment, pulling the insulating sleeve in an axial direction of the insulating sleeve includes the steps of:
the needle pulling instrument clamps one end of the insulating sleeve, which is far away from the metal probe;
And controlling the needle pulling instrument to pull the insulating sleeve in a direction away from the metal probe according to a preset speed, so that the insulating sleeve is broken at the marked point.
In one embodiment, the method for preparing a microelectrode further comprises the steps of:
And if the gap exists between the fracture part of the insulating sleeve and the tip of the metal probe, repeating the heating and stretching step until the tip of the metal probe is exposed out of the insulating sleeve.
In one embodiment, the length of the metal probe extending into the insulation sleeve is 1/4-4/5 of the length of the insulation sleeve.
In one embodiment, the insulating sleeve is a capillary glass tube, or the insulating sleeve is made of an inert material.
The microelectrode comprises a metal probe and an insulating sleeve, wherein the insulating sleeve is coated on the outer wall of the metal probe by adopting the microelectrode preparation method according to any technical characteristic, and an insulating layer is formed.
After the technical scheme is adopted, the invention has at least the following technical effects:
According to the microelectrode preparation method and the microelectrode, when the microelectrode is prepared by using the preparation method, the metal probe is placed into the insulating sleeve. And heating the insulating sleeve at the tip of the metal probe, so that the insulating sleeve is softened after being heated, and pulling one end of the insulating sleeve away from the metal probe along the axial direction of the insulating sleeve, so that the insulating sleeve stretches towards the direction away from the metal probe. Under the action of the stretching force, the insulation sleeve can be locally broken at the needle point and is divided into two parts, and the part of the insulation sleeve sleeved on the metal probe is attached to the external force of the metal probe and is melted in a heating state and is adhered to the outer wall of the metal probe so as to form an insulation layer on the outer wall of the metal probe, so that the preparation of the microelectrode is completed.
According to the microelectrode preparation method, the microelectrode is prepared by adopting the metal probe, the metal probe is provided with the tip, the insulating sleeve is sleeved on the outer wall of the metal probe by adopting the heating stretching method, so that the insulating layer is formed on the outer wall of the metal probe, the tip of the metal probe is exposed, the microelectrode can be used as the microelectrode without polishing, the preparation process is simplified, the problem of breakage caused by polishing is avoided, and the preparation difficulty is reduced. Meanwhile, the metal probe is coated by adopting a heating and stretching method, cutting by using a focused ion beam scanning electron microscope is not needed, the manufacturing cost is reduced, and the microelectrode is convenient to prepare.
Drawings
FIG. 1 is a schematic view of a metal probe according to an embodiment of the present invention placed on an insulation sleeve;
FIG. 2 is a schematic illustration of the insulating sleeve of FIG. 1 after being stretched;
FIG. 3 is a flow chart of microelectrode preparation according to one embodiment of the present invention.
Wherein: 100. a metal probe; 110. a probe body; 120. a needle tip; 200. an insulating sleeve.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
Referring to fig. 1 to 3, the present invention provides a method for manufacturing a microelectrode. The preparation method of the microelectrode is used for preparing the microelectrode in the electrochemical field. The microelectrode is used for carrying out an electrochemical experiment so as to meet the requirements of the electrochemical experiment. It will be appreciated that in conventional solutions, a platinum wire (more than 10 microns in diameter) is typically used as the metal carrier, and polytetrafluoroethylene or glass is coated over the entire platinum wire. And (3) cutting off the whole platinum wire, and polishing and grinding the tip of the platinum wire to make the surface smooth, thereby obtaining the microelectrode. When the platinum wire is adopted to manufacture the microelectrode, the surface of the platinum wire is required to be polished, the operation process is complex, in addition, the platinum wire is extremely easy to break in the processing process, and the preparation process difficulty is high. In addition, some researchers have coated the surface with an amorphous fluororesin solution, but the coated probe needs to be cut by a FIB/SEM (focused ion beam scanning electron microscope) instrument, which is costly, and thus the processing cost of the solution is high.
Therefore, the present invention provides a novel microelectrode manufacturing method, which uses a metal probe 100 as a substrate, coats an insulating layer on the surface of the metal probe 100, and exposes the tip 120 of the metal probe 100, thereby forming a microelectrode. The microelectrode prepared by the preparation method can be directly used without polishing, reduces the processing difficulty, does not need to cut by using a FIB/SEM (focused ion beam scanning electron microscope), and reduces the cost. The following describes a specific method for preparing an embodiment of the microelectrode.
Referring to fig. 1 to 3, in an embodiment, a method of manufacturing a microelectrode includes:
S1: placing the metal probe 100 in the insulating sleeve 200;
s2: heating the insulation sleeve 200 at the tip 120 of the metal probe 100;
S3: pulling the insulating sleeve 200 in the axial direction of the insulating sleeve 200 breaks the insulating sleeve 200 at the needle tip 120 and exposes the needle tip 120;
s4: the remaining insulating sleeve 200 is melted and adhered to the outer wall of the metal probe 100 to form an insulating layer.
It can be appreciated that the metal probe 100 requires only a very small portion of the tip 120 to be exposed for electrochemical experiments, and the remaining portion to be coated with an insulating layer to avoid contact with the electrolyte, and only serves as a current collector for providing electrons. Therefore, the preparation method of the microelectrode of the invention realizes that the insulating layer is coated on the outer side of the metal probe 100, and exposes a small part of the needle tip 120 of the metal probe 100, thereby reducing the processing difficulty and the processing cost and facilitating the preparation of the microelectrode. In the preparation method of the microelectrode, a heating and stretching method is adopted to enable the insulation sleeve 200 to be coated on the outer wall of the metal probe 100 so as to form an insulation layer. Hereinafter, for simplicity of description, the needle tip 120 is directly said to expose the insulating layer.
Specifically, the insulating sleeve 200 is hollow, and the inner diameter of the insulating sleeve 200 is slightly larger than the outer diameter of the metal probe 100. In this way, the metal probe 100 can be placed into the insulating sleeve 200. The metal probe 100 is located at one end of the insulation sleeve 200, and the metal probe 100 is supported by the insulation sleeve 200. After the metal probe 100 is placed on the insulation sleeve 200, heating is performed at a position where the tip 120 of the metal probe 100 corresponds to the insulation sleeve 200, and the insulation sleeve 200 is stretched, so that the insulation sleeve 200 is broken at the tip 120 of the metal probe 100.
That is, the insulating sleeve 200 is heated and then subjected to a stretching process. When the insulating sleeve 200 is heated, it is necessary to heat the insulating sleeve 200 corresponding to the tip 120 of the metal probe 100. The insulating sleeve 200 softens when heated, and at this time, the end of the insulating sleeve 200 remote from the metal probe 100 is pulled so that the insulating sleeve 200 moves in a direction remote from the metal probe 100. Since the metal probe 100 is positioned inside the insulation sleeve 200, after the insulation sleeve 200 is softened by heating, a portion where the insulation sleeve 200 is sleeved is attached to the outer wall of the metal probe 100. At this time, when the insulating sleeve 200 is pulled, only the insulating sleeve 200 that does not cover the metal probe 100 is stretched, that is, the insulating sleeve 200 is separated into two parts during the stretching process, one part is attached to the metal probe 100 and remains stationary, and the other part moves in a direction away from the metal probe 100, so that the insulating sleeve 200 is broken.
To better describe the process of forming an insulating layer on the metal probe 100 by the insulating sleeve 200, it is noted that the insulating sleeve 200 includes a first insulating section and a second insulating section, which are integrally formed. The first insulation sleeve is sleeved on the metal probe 100, and the metal probe 100 does not exist in the second insulation section. And heating the joint of the first insulating section and the second insulating section. When heating, first insulating section and second insulating section are heated and soften, because first insulating section cover is established in the outside of metal probe 100, and the bonding is at the outer wall of metal probe 100 after first insulating section is heated and softened, at this moment, stretch the one end that first insulating section was kept away from to the second insulating section, and this tensile force can only drive the second insulating section and move towards the direction of keeping away from first insulating section to can not drive first insulating section and remove, after stretching to a certain extent, second insulating section and first insulating section can break in the junction of both for the tip 120 of metal probe 100 exposes.
It should be noted that, when the connection between the first insulation segment and the second insulation segment is heated at the connection between the first insulation segment and the second insulation segment corresponding to the tip 120 of the metal probe 100, that is, the position of the insulation sleeve 200 corresponding to the metal probe 100 is heated, after the insulation sleeve 200 is stretched, the insulation sleeve 200 is broken at the tip 120 of the metal probe 100, so that the tip 120 of the metal probe 100 is exposed. That is, after the partial tensile fracture of the insulating sleeve 200, a small portion of the metal/needle tip 120 of the metal probe 100 is exposed from the end of the insulating sleeve 200 at the needle tip 120, so that the electrochemical experiment can be performed later.
In addition, the microelectrode of the present invention is prepared by using the metal probe 100 as a needle body, and the end of the metal probe 100 is a needle tip 120. That is, the end of the metal probe 100 is a tip. When the metal probe 100 is used for preparing the microelectrode, the tip 120 of the metal probe 100 is directly the tip of the microelectrode, and the tip can be directly used for electrochemical experiments without polishing the end of the microelectrode, so that the preparation steps of the microelectrode are simplified, the preparation difficulty is reduced, and the breakage in the polishing process is avoided.
Referring to fig. 1 to 3, when a microelectrode is manufactured using the microelectrode manufacturing method of the above-described embodiment, the metal probe 100 is placed into the insulation sleeve 200, the insulation sleeve 200 is heated, and the heated position is ensured to correspond to the tip 120 of the metal probe 100, so that the insulation sleeve 200 is softened after being heated. Pulling the insulating sleeve 200 away from the end of the metal probe 100 and moving the insulating sleeve 200 in a direction away from the metal probe 100 causes the insulating sleeve 200 to break at the tip 120 of the metal probe 100, thereby exposing the tip 120 of the metal probe 100. At this time, the microelectrode is exposed at the tip 120 of the metal probe 100, the rest of the metal probe 100 is covered with the remaining insulation sleeve 200 to form an insulation layer, and then the insulation layer is adhered to the outer wall of the metal probe 100 to form the microelectrode, and the microelectrode can be subjected to an electrochemical experiment.
According to the microelectrode preparation method, the metal probe 100 is used for preparing the microelectrode, the metal probe 100 is provided with the needle tip 120, the insulating sleeve 200 is sleeved on the outer wall of the metal probe 100 by adopting a heating and stretching method, so that an insulating layer is formed on the outer wall of the metal probe 100, the needle tip 120 of the metal probe 100 is exposed, the microelectrode can be used as the microelectrode without polishing, the preparation process is simplified, the problem of breakage caused by polishing is avoided, and the preparation difficulty is reduced. Meanwhile, the metal probe 100 is coated by adopting a heating and stretching method, cutting by using a focused ion beam scanning electron microscope is not needed, the manufacturing cost is reduced, and the preparation of the microelectrode is facilitated.
To better illustrate the preparation of the microelectrode, the relationship between the insulating sleeve 200 and the insulating layer is described herein, the insulating sleeve 200 is an insulating tube in an initial state, the insulating sleeve 200 is not yet heated, and the length of the insulating sleeve 200 is greater than the length of the coated metal probe 100. The insulating sleeve 200 softens after heating and breaks the insulating sleeve 200 at the tip 120 of the metal probe 100, leaving the insulating sleeve 200 covering part of the metal probe 100 to form an insulating layer.
Referring to fig. 1 to 3, in an embodiment, a metal probe 100 includes a probe body 110 and a needle tip 120 as above, the needle tip 120 being disposed at one end of the probe body 110. The insulating layer covers one end of the probe body 110 near the needle tip 120 and partially covers the needle tip 120. The needle tip 120 is tapered, one end of the needle tip 120 away from the probe body 110 is a tip, and the probe body 110 is cylindrical. The insulating layer covers a portion of the tapered surface and a portion of the cylindrical surface.
It can be appreciated that after the insulating sleeve 200 is stretched by adopting the heating stretching method, the insulating sleeve 200 can be softened and attached to the tapered surface and the cylindrical surface of the part of the metal probe 100 after being heated, so as to ensure the coating effect on the metal probe 100, further ensure the quality of the formed insulating layer and avoid a gap between the insulating layer and the inner wall of the metal probe 100.
In one embodiment, the probe body 110 has a diameter dimension in the range of greater than 100 microns. Thus, the mechanical strength of the metal probe 100 can be improved, so that the mechanical strength of the metal probe 100 is far higher than that of a platinum wire, and the metal probe 100 is convenient to process.
In one embodiment, the tip 120 of the metallic probe 100 has a diameter dimension of less than 20 microns. In this way, the tip 120 of the metal probe 100 can meet the requirements of an electrochemical experiment.
Alternatively, the diameter of the needle tip 120 is gradually reduced in size from the end connected to the probe body 110 to the end distant from the probe body 110. This can prevent a step structure from being formed at the junction of the probe body 110 and the tip 120, and ensure structural strength of the metal probe 100.
Referring to fig. 1 to 3, in an embodiment, the step of placing the metal probe 100 in the insulation sleeve 200 includes:
Placing the metal probe 100 in the metal sleeve;
the position of the metal probe 100 in the insulating sleeve 200 is adjusted so that the metal probe 100 is in place.
It will be appreciated that the length of the insulating sleeve 200 is greater than the length of the sleeve that covers the metal probe 100, so that the insulating sleeve 200 can be pulled apart at the tip 120 of the metal probe 100, thereby forming an insulating layer on the outer wall of the metal probe 100 to cover the metal probe 100. The metal probe 100 is installed in the insulation sleeve 200, the inside diameter of the insulation sleeve 200 is slightly larger than the outside diameter of the metal probe 100, and the metal probe 100 is reciprocally moved/rotated in the insulation sleeve 200 to adjust the position of the metal probe 100 in the insulation sleeve 200 so that the metal probe 100 is in a proper position in the insulation sleeve 200, thereby facilitating the post-heating stretching of the insulation sleeve 200 to cover the metal probe 100.
In one embodiment, the step of placing the metal probe 100 in the insulating sleeve 200 further comprises:
determining the length of the insulating sleeve 200 covering the metal probe 100;
providing a marking point at a position of the insulating sleeve 200 corresponding to the needle tip 120 of the metal probe 100;
the tip 120 of the metal probe 100 is inserted into the insulation sleeve 200 from one end of the insulation sleeve 200 such that the tip 120 is aligned with the marking point.
To ensure that the metal probe 100 is placed in the proper position on the insulating sleeve 200, the insulating sleeve 200 may be marked in advance. Thus, after the metal probe 100 is placed in the insulating sleeve 200, the tip 120 of the metal probe 100 is positioned at a desired location, thereby ensuring that the metal probe 100 is in place in the insulating sleeve 200.
Specifically, after the insulating sleeve 200 is selected, determining the length of the insulating sleeve 200 covering the metal probe 100, and marking a point at the position of the outer wall of the insulating sleeve 200 corresponding to the needle point 120 of the metal probe 100 therein. The metal probe 100 is placed into the insulating sleeve 200 and the position of the metal probe 100 is adjusted so that the tip 120 of the metal probe 100 is aligned with the mark point, at which point the metal probe 100 is in place in the insulating sleeve 200. Indicating that the insulating sleeve 200 may be subjected to subsequent operations to encase the metal probe 100. Alternatively, a body view mirror may be used to determine and mark the location of the marker points.
Referring to fig. 1 to 3, in an embodiment, the step of heating the insulation sleeve 200 at the tip 120 of the metal probe 100 includes:
placing a heating device under the insulating sleeve 200 and aligning the heating device with the marking point;
the heating means is controlled to heat the insulating sleeve 200 at the marked point.
In one embodiment of the present invention, a separate heating device may be used to heat the insulating sleeve 200. The heating means is placed under the insulating sleeve 200 and is placed in correspondence with the marking points. When the metal probe 100 is in place in the insulation sleeve 200, the heating means is controlled to heat the insulation sleeve 200 at the marked point, so that the insulation sleeve 200 can be broken at the marked point to expose the tip 120 of the metal probe 100 when the insulation sleeve 200 is later stretched.
When the heating device is used for heating the insulating sleeve 200, as the outer diameter sizes of the metal probe 100 and the insulating sleeve 200 are smaller, the heating device can heat the insulating sleeve 200 in the lower part, so that the heating requirement of the insulating sleeve 200 can be met, and the condition of uneven heating can not occur. Like this, heating device heats back to insulating sleeve 200, after stretching insulating sleeve 200, insulating sleeve 200 fracture in mark point department, can guarantee the smoothness of fracture department, can not appear the problem such as burr, guarantees the quality of formation insulating layer.
Alternatively, the heating means may be an alcohol burner. Of course, in other embodiments of the present invention, the heating device may have other structures that can heat the insulating sleeve 200, and will not be described herein. Optionally, the heating temperature of the alcohol lamp ranges from 500 ℃ to 600 ℃. Illustratively, the heating temperature of the alcohol burner is about 600 ℃.
Referring to fig. 1 to 3, in an embodiment, pulling the insulation sleeve 200 in an axial direction of the insulation sleeve 200 includes the steps of:
holding an end of the insulating sleeve 200 remote from the metal probe 100;
Pulling the insulating sleeve 200 in a direction away from the metallic probe 100 breaks the insulating sleeve 200 at the marked point.
After the insulating sleeve 200 is heated, the insulating sleeve 200 is pulled at an end of the insulating sleeve 200 remote from the metal probe 100 such that the insulating sleeve 200 extends in a direction away from the metal probe 100. In this embodiment, pulling the insulating sleeve 200 may be such that an operator's hand directly holds the end of the insulating sleeve 200, directly dragging the insulating sleeve 200 to move away from the metal probe 100, causing the insulating sleeve 200 to break at the marked point, thereby exposing the tip of the metal probe 100. Of course, the end of the insulation sleeve 200 may be clamped by a clamp or the like, and the clamp may be automatically pulled by an instrument or manually pulled by an operator, so that the insulation sleeve 200 moves in a direction away from the metal probe 100.
Referring to fig. 1 to 3, in an embodiment, the step of heating the insulation sleeve 200 at the tip 120 of the metal probe 100 includes:
Placing the insulating sleeve 200 in a needle drawing instrument;
The heating point of the heater of the needle drawing instrument is aligned with the marking point;
the heater heats the insulation sleeve 200.
That is, in this embodiment, the stretching of the insulation sleeve 200 may be achieved by a drawing needle apparatus, and the drawing needle apparatus is provided with a heater, and after the insulation sleeve 200 is heated by the heater, the drawing needle apparatus is used to stretch the insulation sleeve 200, thereby forming an insulation layer on the surface of the metal probe 100.
Specifically, the insulating sleeve 200 is mounted in a needle drawing instrument, and the insulating sleeve 200 is clamped by the needle drawing instrument, so that the insulating sleeve 200 is supported. In addition, the heater is arranged in the drawing needle instrument, the heating point of the heater is aligned with the marking point of the insulating sleeve 200, and the heater is controlled to heat the insulating sleeve 200 at the marking point, so that the drawing treatment of the insulating sleeve 200 at the later stage is facilitated. Alternatively, the heater is a laser heater or a resistance wire heater.
Referring to fig. 1 to 3, in an embodiment, pulling the insulation sleeve 200 in an axial direction of the insulation sleeve 200 includes the steps of:
the needle pulling instrument clamps one end of the insulating sleeve 200 away from the metal probe 100;
and controlling the needle pulling instrument to pull the insulating sleeve 200 in a direction away from the metal probe 100 at a preset speed, so that the insulating sleeve 200 is broken at the marked point.
After the heater heats the insulating sleeve 200, the needle pulling instrument clamps one end of the insulating sleeve 200 far away from the metal probe 100 to start moving and moves towards the direction far away from the metal probe 100, so that the insulating sleeve 200 is in a stretched state, and the insulating sleeve 200 is ensured to be broken at the marked point, so that the needle tip 120 of the metal probe 100 is exposed. Moreover, the needle pulling instrument drives the insulating sleeve 200 to move at a preset speed, so that the stretching effect of the insulating sleeve 200 is ensured, and the stretching uniformity of the insulating sleeve 200 is ensured.
Optionally, the stretch rate of the needle puller is greater than 1mm/min. This can ensure the stretching effect of the insulating sleeve 200, thereby ensuring the quality of the insulating layer formed. It should be noted that, the drawing needle instrument and the drawing principle thereof are related to the prior art, and are not described herein.
In the present invention, the heated insulation sleeve 200 may be stretched manually, or the heated insulation sleeve 200 may be stretched automatically by a needle drawing machine, so that the heated insulation sleeve 200 is broken at the marking point, and the needle tip 120 of the metal probe 100 is exposed from the broken portion of the insulation sleeve 200. It should be noted that, the stretching direction of the insulating sleeve 200 during stretching is all along the length direction of the metal probe 100, that is, the stretching direction of the insulating sleeve 200 along the extension line direction of the tip 120 of the metal probe 100, so as to ensure the uniformity of the insulating sleeve 200 after stretching. As shown in fig. 1 and 2, the three arrows below the insulating sleeve 200 illustrate the heating position, and the arrow at the left end of the insulating sleeve 200 illustrates the stretching direction.
Referring to fig. 1 to 3, in an embodiment, the method for preparing a microelectrode further includes the steps of:
s5: if there is a gap between the broken portion of the insulating sleeve 200 and the tip 120 of the metal probe 100, the heating and stretching steps are repeatedly performed until the tip 120 is exposed out of the insulating sleeve 200.
That is, after the one-time heating and stretching process is adopted, the needle tip 120 of the metal probe 100 is still located in the insulation sleeve 200, and at this time, the heating and stretching process is repeated until the needle tip 120 is exposed from the breaking position of the insulation sleeve 200, so as to meet the requirement of the electrochemical experiment.
In one embodiment, the length of the metal probe 100 extending into the insulation sleeve 200 is 1/4 to 4/5 of the length of the insulation sleeve 200. This ensures the length of the insulating layer covered by the outer wall of the metal probe 100 while facilitating the stretching of the insulating sleeve 200 so that the tip 120 of the metal probe 100 is exposed.
In one embodiment, the insulating sleeve 200 is a capillary glass tube. That is, the insulating sleeve 200 is made of a glass material. After the capillary glass tube is heated, the physical state of the capillary glass tube is converted from a glassy state to a soft semi-glassy state, so that the surface of the metal probe 100 can be accurately attached, the effect of forming an insulating layer is ensured, and the condition of uneven deformation is avoided. Of course, in other embodiments of the invention, the insulating sleeve 200 is made of an inert material.
Referring to fig. 1 to 3, in the method for manufacturing a microelectrode according to the present invention, the insulation sleeve 200 is sleeved on the outer wall of the metal probe 100 by a heating and stretching method, so that an insulation layer is formed on the outer wall of the metal probe 100, and the method does not need to use amorphous fluoride for coating, thus being convenient to manufacture. Moreover, the insulating sleeve 200 is heated at the marked point of the insulating sleeve 200, so that the heating position is controllable, and compared with the current method for coating the platinum wire by the capillary, the heating and stretching method can accurately control the stretching site, so that a small part of the needle tip 120 of the metal probe 100 is exposed for electrochemical experiments. Meanwhile, as the melting point of the metal probe 100 is far higher than that of glass softening, the needle tip 120 of the metal probe 100 can be heated to dissolve the insulating sleeve 200, so that the needle tip 120 of the metal probe 100 is exposed, the surface is not required to be polished, the preparation process is simplified, the problem of breakage caused by polishing is avoided, and the preparation difficulty is reduced.
Meanwhile, the metal probe 100 is coated by adopting a heating and stretching method, cutting by using a focused ion beam scanning electron microscope is not needed, the manufacturing cost is reduced, and the preparation of the microelectrode is facilitated. The microelectrode adopts the metal probe 100 with high melting point and high mechanical strength, has better processing performance, and simultaneously adopts the capillary glass tube as a coating medium, thereby effectively reducing the preparation cost.
Referring to fig. 1 and fig. 2, the invention further provides a microelectrode, which comprises a metal probe 100 and an insulation sleeve 200, wherein the insulation sleeve 200 is coated on the outer wall of the metal probe 100 by adopting the microelectrode preparation method according to any embodiment, and an insulation layer is formed. According to the microelectrode, the insulating sleeve 200 is arranged on the outer side of the metal probe 100, and the insulating sleeve 200 is subjected to heating and stretching treatment, so that the insulating sleeve 200 forms an insulating layer on the outer side of the metal probe 100, meanwhile, the tip 120 of the metal probe 100 is exposed, the microelectrode can be used as the microelectrode without polishing, the preparation process is simplified, the problem of breakage caused by polishing is avoided, and the preparation difficulty is reduced. Meanwhile, the metal probe 100 is coated by adopting a heating and stretching method, cutting by using a focused ion beam scanning electron microscope is not needed, the manufacturing cost is reduced, and the preparation of the microelectrode is facilitated.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (9)

1. A method of preparing a microelectrode comprising:
Placing a metal probe in an insulating sleeve;
Heating the insulating sleeve at the tip of the metal probe;
Pulling the insulating sleeve along the axial direction of the insulating sleeve to break the insulating sleeve at the needle point and expose the needle point;
the rest of the insulating sleeve is melted and adhered to the outer wall of the metal probe to form an insulating layer;
If the gap exists between the broken part of the insulating sleeve and the tip of the metal probe, repeating the heating and stretching step until the tip of the metal probe is exposed out of the insulating sleeve;
The insulation sleeve comprises a first insulation section and a second insulation section which are integrated, the metal probe is located in the first insulation section, the connection part of the first insulation section and the second insulation section is heated, and the second insulation section is pulled, so that the first insulation section is coated on the metal probe.
2. The method of preparing a microelectrode according to claim 1, wherein the step of placing the metal probe in the insulating sleeve comprises:
Determining the length of the insulating sleeve which coats the metal probe;
A marking point is arranged at the position of the insulating sleeve corresponding to the tip of the metal probe;
and inserting the tip of the metal probe into the insulating sleeve from one end of the insulating sleeve, and aligning the tip with the marking point.
3. The method of preparing a microelectrode according to claim 2, wherein the step of heating the insulating sleeve at the tip of the metal probe comprises:
Placing a heating device below the insulating sleeve and aligning the heating device to the marking point;
Controlling the heating device to heat the insulating sleeve at the marked point.
4. The method of manufacturing a microelectrode according to claim 3, wherein pulling the insulating sleeve in the axial direction of the insulating sleeve comprises the steps of:
holding an end of the insulating sleeve away from the metal probe;
pulling the insulating sleeve away from the metallic probe breaks the insulating sleeve at the marked point.
5. The method of preparing a microelectrode according to claim 2, wherein the step of heating the insulating sleeve at the tip of the metal probe comprises:
Placing the insulating sleeve in a needle drawing instrument;
The heating point of the heater of the needle drawing instrument is aligned with the marking point;
The heater heats the insulating sleeve.
6. The method of manufacturing a microelectrode according to claim 5, wherein pulling the insulating sleeve in the axial direction of the insulating sleeve comprises the steps of:
the needle pulling instrument clamps one end of the insulating sleeve, which is far away from the metal probe;
And controlling the needle pulling instrument to pull the insulating sleeve in a direction away from the metal probe according to a preset speed, so that the insulating sleeve is broken at the marked point.
7. The method of manufacturing a microelectrode according to any one of claims 1 to 6, wherein the length of the metal probe extending into the insulating sleeve is 1/4 to 4/5 of the length of the insulating sleeve.
8. The method of any one of claims 1 to 6, wherein the insulating sleeve is a capillary glass tube or is made of an inert material.
9. A microelectrode comprising a metal probe and an insulating sleeve, wherein the insulating sleeve is coated on the outer wall of the metal probe by the microelectrode preparation method according to any one of claims 1 to 8, and an insulating layer is formed.
CN202310302879.4A 2023-03-23 2023-03-23 Microelectrode preparation method and microelectrode Active CN116514051B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013164375A (en) * 2012-02-13 2013-08-22 National Institute Of Advanced Industrial & Technology Heat-proof pressure-resistant corrosion resistance microelectrode
CN103713160A (en) * 2013-12-20 2014-04-09 华中科技大学 Noble metal ultramicro electrode and preparation method thereof
CN106248999A (en) * 2016-08-25 2016-12-21 浙江大学 The preparation method of the golden disk time micron electrode that a kind of geometry is controlled
CN106365111A (en) * 2016-08-25 2017-02-01 浙江大学 Preparation method for Pt disk sub-micron electrode with controllable geometrical shape

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013164375A (en) * 2012-02-13 2013-08-22 National Institute Of Advanced Industrial & Technology Heat-proof pressure-resistant corrosion resistance microelectrode
CN103713160A (en) * 2013-12-20 2014-04-09 华中科技大学 Noble metal ultramicro electrode and preparation method thereof
CN106248999A (en) * 2016-08-25 2016-12-21 浙江大学 The preparation method of the golden disk time micron electrode that a kind of geometry is controlled
CN106365111A (en) * 2016-08-25 2017-02-01 浙江大学 Preparation method for Pt disk sub-micron electrode with controllable geometrical shape

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