Micro-nano electrode preparation method and device based on liquid film form regulation and control technology

Abstract

The invention relates to a micro-nano electrode preparation method and device based on a liquid film form regulation and control technology. The method comprises the steps that an electrode to be machined penetrates through the space between a metal circular ring and a non-metal circular ring which are coaxially arranged in a nested mode; adding an electrolyte between the metal ring and the non-metal ring to form an electrolyte film; the to-be-machined electrode is connected with the positive electrode of a direct-current power source, and the metal ring is connected with the negative electrode of the direct-current power source; and / or the section diameter of the metal circular ring; according to the method, the size of a ring-solution interface and the trend of a liquid film are controlled according to the diameter of the cross section of a non-metal circular ring and / or the diameter of the cross section of the non-metal circular ring, the form of the electrolyte film is actively regulated and controlled, an electrode to be machined rotates, an electrochemical etching reaction is generated in the electrolyte film, and online preparation of a micro-nano electrode and an electrode in a complex shape is carried out. The method has the advantages of high machining precision, good surface quality, high micro degree, simple equipment, convenience in integration and the like.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of micro electrochemical machining, and particularly relates to a micro-nano electrode preparation method and device based on liquid film morphology control technology. BACKGROUND

[0002] Micro-nano electrodes have wide application prospects in the fields of electronic information, energy storage, biosensing, micro-nano machining, etc. due to their unique size effect and surface effect. In the field of micro-nano machining, the shape, size, precision and surface quality of the tool electrode will affect the machining quality. Therefore, it is necessary to develop a micro-nano electrode preparation method and device to meet the needs of high-precision and stable preparation of micro-nano electrodes and complex-shaped electrodes, and to provide a basis for opening up new research directions and application scenarios in the field of micro-nano machining.

[0003] At present, the processes for preparing micro-nano tool electrodes mainly include precision cutting machining technology, focused ion beam milling technology, wire electrode electric spark grinding technology, block electrode or blade electrode electric spark grinding machining technology, and electrochemical etching technology. Among them, the liquid film etching method, as one of the electrochemical etching technologies, can avoid the flexural deformation of the micro-nano tool electrode caused by cutting force, has lower cost and higher efficiency than the focused ion beam milling technology, has no thermal influence zone than the wire electrode electric spark grinding technology, has higher machining precision, surface quality and material utilization rate than the block electrode or blade electrode electric spark grinding machining technology, and has better controllability and on-line preparation than other electrochemical etching technologies such as immersion etching method. However, in the past research, the liquid film etching method generally adopts a natural form of liquid film, and the liquid film morphology is not effectively controlled.

[0004] For example, the patent CN105817723B discloses a method and device for preparing a nano tool electrode by double liquid film electrochemical etching, which can provide upward tension to the lower end electrode by using a viscous liquid film to reduce the tension on the lower end electrode, thereby realizing the preparation of a smaller diameter nano electrode. However, the natural form of liquid film is adopted, and the morphology of the liquid film will affect the movement and distribution of the product, the current density distribution on the anode surface, and further affect the morphology of the prepared electrode. The morphology of the liquid film, i.e. the thickness and curvature of the film surface, is mainly determined by factors such as surface tension of the electrolyte, diameter of the cathode ring and amount of injected electrolyte, and lacks effective control of the liquid film morphology. Therefore, the ability to adapt to complex etching paths is limited, which affects the accurate control of the shape and size of the electrode, and further affects the preparation precision and stability, which needs to be improved. SUMMARY

[0005] The present invention aims to at least partially solve one of the above-mentioned technical problems. The present invention provides a method and apparatus for preparing micro-nano electrodes based on liquid film morphology control technology, which can improve the accuracy of electrode preparation and the stability of the preparation process, and meet the preparation requirements of micro-nano electrodes and electrodes with complex shapes.

[0006] The technical solution adopted by this invention to solve its technical problem is:

[0007] The first aspect of this invention is to provide a method for preparing micro / nano electrodes based on liquid film morphology control technology, the method comprising:

[0008] The electrode to be processed is passed between metal rings and non-metal rings arranged in a coaxial nested configuration;

[0009] An electrolyte is added between the metal ring and the non-metal ring to form an electrolyte film;

[0010] The electrode to be processed is connected to the positive terminal of a DC power supply, and the metal ring is connected to the negative terminal of a DC power supply. By adjusting the relative axial positions of the metal ring and the non-metal ring, and / or adjusting the cross-sectional diameter of the metal ring, and / or adjusting the cross-sectional diameter of the non-metal ring, the morphology of the electrolyte film is controlled, causing the electrode to be processed to rotate and undergo an electrochemical etching reaction within the electrolyte film until the electrode to be processed breaks off to form a micro / nano electrode.

[0011] In order to further enhance the electrochemical etching reaction by controlling the liquid film morphology and to prepare micro / nano electrodes and electrodes with complex shapes, in a preferred technical solution, the non-metallic ring is adjusted to be flush with or higher than the metal ring in the axial direction, and / or the cross-sectional diameter of the metal ring is increased, so that the electrochemical etching reaction of the electrode to be processed on the side close to the metal ring is more intense.

[0012] In order to further improve the consistency of electrochemical etching reaction by controlling the liquid film morphology and to prepare micro- and nano-electrodes and electrodes with complex shapes, in the preferred technical solution, the electrochemical etching reaction on both sides of the electrode to be processed tends to be consistent by adjusting the non-metallic ring to be lower than the metal ring in the axial direction.

[0013] To further improve the uniformity of the reaction at the electrode to be processed, in a preferred embodiment, the metal ring is located inside the non-metal ring.

[0014] The second aspect of the present application provides a micro-nano electrode preparation device based on liquid film morphology regulation technology, comprising a driving mechanism, a direct current power supply, a metal ring and a non-metal ring arranged in a coaxial nested manner; the driving mechanism is operated based on any one of the micro-nano electrode preparation methods based on liquid film morphology regulation technology, and is used to drive the to-be-processed electrode to rotate between the metal ring and the non-metal ring and drive the metal ring and the non-metal ring to move relative to each other in the axial direction; the positive electrode of the direct current power supply is connected to the to-be-processed electrode, and the negative electrode of the direct current power supply is connected to the metal ring.

[0015] In order to facilitate the automatic threading of the to-be-processed electrode between the coaxially nested metal ring and non-metal ring and promote the uniform reaction of the to-be-processed electrode, in the preferred technical solution, the driving mechanism is used to drive the to-be-processed electrode, the metal ring and the non-metal ring to move relative to each other in three-dimensional directions.

[0016] In order to further simplify the structure of the driving mechanism and improve the operation stability, in the preferred technical solution, the driving mechanism comprises an X-axis moving assembly, a Y-axis moving assembly, a Z-axis moving assembly and a main shaft, the X-axis moving assembly is used to drive the Z-axis moving assembly to move left and right, the Y-axis moving assembly is used to drive the metal ring and the non-metal ring to move forward and backward, the Z-axis moving assembly is used to drive the main shaft to move up and down, and the main shaft is used to drive the to-be-processed electrode to rotate along the axial direction of the main shaft.

[0017] In order to further facilitate the collection of the processed micro-nano electrode, in the preferred technical solution, an electrode receiver is arranged on the Y-axis moving assembly.

[0018] In order to further facilitate the taking and placing of the to-be-processed electrode and improve the processing efficiency, in the preferred technical solution, a chuck is arranged on the main shaft, and a cross-shaped purple copper rod matched with the to-be-processed electrode is arranged on the chuck.

[0019] In order to further facilitate the control of the relative movement of the metal ring and the non-metal ring in the axial direction, in the preferred technical solution, the driving mechanism comprises a first support and a linear stepping device, the first support is used to support the metal ring, and the linear stepping device is used to drive the non-metal ring to move reciprocatingly in the axial direction; or, the first support is used to support the non-metal ring, and the linear stepping device is used to drive the metal ring to move reciprocatingly in the axial direction.

[0020] In order to further improve the support stability of the metal ring and the non-metal ring, in the preferred technical solution, the linear stepping device is provided with a second support, and the second support and the first support are both provided with grooves, and the metal ring and the non-metal ring are respectively supported and placed by the grooves of the first support and the second support.

[0021] In order to further improve the operation stability and operation precision, in the preferred technical solution, the isolation base provided with the driving mechanism is included.

[0022] In order to further improve the operation precision, in the preferred technical solution, the electron microscope towards the metal ring and the non-metal ring is included, and the electron microscope is used to observe the morphology of the electrolyte liquid film and the relative position of the metal ring and the non-metal ring.

[0023] In order to further improve the operation precision, in the preferred technical solution, the control device connected with the electron microscope is included, and the control device is used to control the operation of the driving mechanism.

[0024] Compared with the prior art, the present application has at least the following beneficial effects:

[0025] (1) The method of the present application passes the electrode to be processed between the coaxially nested metal ring and the non-metal ring, uses the metal ring and the non-metal ring to support the liquid film, adjusts the relative position of the metal ring and the non-metal ring in the axial direction, and / or adjusts the cross-sectional diameter of the metal ring, and / or adjusts the cross-sectional diameter of the non-metal ring, to adjust the size of the ring-solution interface and the direction of the liquid film, thereby actively controlling the morphology of the liquid film. The electrode to be processed is rotated and subjected to electrochemical etching reaction in the electrolyte liquid film, which solves the technical problem that the natural morphology of the liquid film affects the precision and stability of the prepared electrode and cannot meet the complex etching path. The method can realize the preparation of micro-nano scale electrodes and online preparation of complex shape electrodes, and has good market application prospect.

[0026] (2) The device of the present application can realize different liquid film morphologies by selecting metal rings / non-metal rings with different cross-sectional diameters, and can also realize different liquid film morphologies by driving the metal ring and the non-metal ring to move relatively in the axial direction. The required liquid film morphology can be further determined by the electron microscope. The electrode to be processed is driven to rotate between the metal ring and the non-metal ring, and the electrode to be processed, the metal ring and the non-metal ring are driven to move relatively in three-dimensional direction, which further solves the technical problem that the existing device cannot actively control the liquid film morphology flexibly, efficiently and accurately, and cannot perform online preparation of micro-nano electrodes and complex shape electrodes. The device has the advantages of high processing precision, good surface quality, high micro-fineness, simple equipment, easy integration, etc., and is conducive to promoting automatic large-scale production and stable processing, and has good industrial adaptability. BRIEF DESCRIPTION OF DRAWINGS

[0027] The above and / or additional aspects and advantages of the present application will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:

[0028] Figure 1 is a processing schematic diagram of embodiment 1 of the present application;

[0029] Figure 2 is a Ccd diagram of the liquid film morphology of the embodiment 1 of the present application;

[0030] Figure 3 is an electrochemical etching simulation diagram of different liquid film morphologies of the embodiment 1 of the present application;

[0031] Figure 4 is a structural schematic diagram of the embodiment 2 of the present application;

[0032] Figure 5 is an external device schematic diagram of the embodiment 2 of the present application;

[0033] Figure 6 is a metal circular ring support schematic diagram of the embodiment 2 of the present application;

[0034] Figure 7 is a non-metal circular ring support schematic diagram of the embodiment 2 of the present application;

[0035] In the figure, the marks are: seismic isolation base 1, movement support 2, Y-axis moving assembly 3, X-axis moving assembly 4, Z-axis moving assembly 5, main shaft 6, chuck 7, cross purple copper rod 8, electrode to be processed 9, electrode receiver 10, metal circular ring 11, non-metal circular ring 12, metal circular ring support 13, first bolt 14, first support 15, first screw 16, linear stepping device 17, second bolt 18, moving sliding table 19, connecting piece 20, second support 21, second screw 22, electrolyte liquid film 23, switch 24, direct current power supply 25, electron microscope 26, control device 27, groove 28, and the unmarked arrow indicates the moving direction. DETAILED DESCRIPTION

[0036] The embodiments of the present application are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference signs represent the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the accompanying drawings are exemplary and are intended to explain the present application, and cannot be understood as a limitation of the present application.

[0037] In the description of the present application, it should be understood that the terms "upper", "lower", "left", "right", "front", "back", "vertical", "horizontal", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application. In addition, the terms "first", "second" are only for the purpose of description, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features referred to. Therefore, the features defined as "first", "second" can be explicitly or implicitly included one or more of the features. In the description of the present application, the meaning of "a plurality of", "several" is two or more, unless otherwise explicitly specified and limited.

[0038] In the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection", "fixing" and the like should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0039] Embodiment 1:

[0040] In view of the fact that the existing liquid film etching method uses natural liquid film and has limited ability to adapt to complex etching paths, affecting the current situation of micro-nano electrodes and complex-shaped electrodes, the inventors found in research that in order to prepare electrodes with higher precision and complex-shaped electrodes, technical measures should be taken to effectively and accurately actively control the shape of the liquid film to improve the precision and stability of the prepared electrodes, such as Figure 1 As shown in the figure, it is a preferred embodiment of the micro-nano electrode preparation method based on the liquid film shape control technology according to the present application, which comprises the following steps:

[0041] Passing the electrode to be processed 9 through the coaxially nested metal ring 11 and non-metal ring 12;

[0042] Adding electrolyte between the metal ring 11 and the non-metal ring 12 to form an electrolyte liquid film 23;

[0043] The electrode to be processed 9 is connected to the positive terminal of the DC power supply 25, and the metal ring 11 is connected to the negative terminal of the DC power supply 25. By adjusting the relative position of the metal ring 11 and the non-metal ring 12 in the axial direction; and / or, adjusting the cross-sectional diameter of the metal ring 11; and / or, adjusting the cross-sectional diameter of the non-metal ring 12, the morphology of the electrolyte film 23 is controlled, so that the electrode to be processed 9 rotates and undergoes an electrochemical etching reaction in the electrolyte film 23 until the electrode to be processed 9 is disconnected to form a micro-nano electrode.

[0044] For example, such as Figure 1 As shown, taking the electrode to be processed 9 as a tungsten wire rod, the outer diameter of the metal ring 11 is smaller than the outer diameter of the non-metal ring 12, the metal ring 11 is fixed, and the non-metal ring 12 can move up and down as an example, the metal ring 11 is mounted on the metal ring support 13, and the non-metal ring 12 is mounted on the movable slide 19. The metal ring 11 and the non-metal ring 12 are coaxially arranged, which is equivalent to the non-metal ring 12 being coaxially nested outside the metal ring 11. The metal ring 11 and the non-metal ring 12 can be selected with different cross-sectional diameters. The tungsten wire rod is mounted on the chuck 7, and the tungsten wire rod is vertically arranged and passes between the metal ring 11 and the non-metal ring 12. The horizontal distance between the tungsten wire rod and the metal ring 11 is d. Electrolyte is added to the metal ring 11 and the non-metal ring 12. An electrolyte film 23 is formed between the rings 12. The relative axial positions of the metal ring 11 and the non-metal ring 12 can be adjusted by moving the non-metal ring 12 up and down, including when they are in a horizontal state or when one is at a higher position than the other. For example, the height difference between the metal ring 11 and the non-metal ring 12 is h, thereby controlling the shape of the liquid film. After connecting the negative terminal of the DC power supply 25 to the metal ring 11 and the positive terminal to the tungsten wire rod and turning on the circuit, the tungsten wire rod can be controlled to rotate and uniformly undergo an electrochemical etching reaction in the electrolyte film 23. As the electrochemical etching reaction occurs, the part of the tungsten wire rod in the electrolyte film 23 will become thinner and thinner, and eventually it will be pulled off and fall off under the gravity of the tungsten wire rod below, thus completing the fabrication of the micro-nano electrode.

[0045] The above method differs from existing liquid film etching methods, which form a circular liquid film on the surface of the metal ring 11, or dual-liquid film electrochemical etching, which forms circular liquid films on the surfaces of the metal ring 11 and the non-metal ring 12 respectively. An electrolyte is added between the coaxially nested metal rings 11 and 12 to form a horizontally annular electrolyte film 23. During the electrochemical etching reaction of the electrode 9 passing through the electrolyte film 23, the liquid film morphology can be actively controlled by changing the relative axial positions of the metal ring 11 and 12; and / or adjusting the cross-sectional diameter of the metal ring 11; and / or adjusting the cross-sectional diameter of the non-metal ring 12. To further verify the effect of actively controlling the liquid film morphology:

[0046] like Figure 2As shown, the experimental conditions: the cross-sectional diameter of the metal ring 11 is 100 μm, the inner diameter is 3-5 mm; the cross-sectional diameter of the non-metal ring 12 is 300 μm, the inner diameter is 300 μm, the electrolyte is KOH with a concentration of 0.5 mol / L, the thickness of the electrolyte liquid film 23 is 1-2 mm, the direct current power supply 25 is a pulse direct current power supply 25 with a voltage of 5 V, a pulse period of 1 μs, and a duty cycle of 20%, the relative position of the metal ring 11 and the non-metal ring 12 in the axial direction is changed, and the liquid film morphology is observed by Ccd, such as Figure 2 (a) shows the liquid film morphology photo when the metal ring 11 is 1 cm higher than the non-metal ring 12, such as Figure 2 (b) shows the liquid film morphology photo when the metal ring 11 is 2 cm higher than the non-metal ring 12, such as Figure 2 (c) shows the liquid film morphology photo when the metal ring 11 is 1 cm lower than the non-metal ring 12, such as Figure 2 (d) shows the liquid film morphology photo when the metal ring 11 is 2 cm lower than the non-metal ring 12, it can be seen that the above method can further regulate the liquid film morphology, such as the thickness of the liquid film, the curvature of the film surface, by moving the relative position of the metal ring 11 and the non-metal ring 12 in the axial direction on the basis of changing the diameter, thereby affecting the current density distribution on the anode surface to affect the electrochemical etching process, not only can change the etching level of the electrode, realize the online preparation of the micro-nano scale electrode, but also can realize the online preparation of the complex shape electrode, the online preparation of the complex shape electrode can prepare the electrode with ladder-shaped or variable-diameter structure under certain conditions, for example: by moving up and down to change the etching area of the electrode to be processed 9, cooperate with the liquid film morphology regulation to carry out the electrode with ladder-shaped or variable-diameter structure; in terms of precision and stability, the shape and size of the electrode can be more accurately controlled by precise regulation of the liquid film morphology, improve the preparation precision and stability, promote the large-scale production, and have good market application prospect.

[0047] Further, by adjusting the non-metal ring 12 to be flush with or higher than the metal ring 11 in the axial direction, and / or adjusting the cross-sectional diameter of the metal ring 11 to increase, the electrochemical etching reaction of the electrode to be processed 9 near the metal ring 11 side is more intense; for example, the micro-nano electrode finished product obtained by electron microscope shooting is drawn to prepare electrochemical etching simulation diagram under different liquid film morphologies, such as Figure 3 (a) shows that when the metal ring 11 and the non-metal ring 12 are in a horizontal state, the liquid film morphology is generally similar, but the electrochemical etching of the tungsten rod near the metal ring 11 side is more intense; such as Figure 3 (b) and Figure 3 (c) shows that when the metal ring 11 and the non-metal ring 12 are in a horizontal state, as the diameter of the metal ring 11 increases, the electrochemical etching reaction of the tungsten rod near the metal ring 11 side is more intense; such asFigure 3 (d) as shown, when the non-metallic annular ring 12 is higher than the metallic annular ring 11, the liquid film morphology changes, the curvature distribution of the liquid film changes, but the reaction is the same as that in the horizontal state, then the electrochemical etching reaction can be further enhanced by regulating the liquid film morphology, for example, the electrode size is reduced by the enhancement effect, the complex three-dimensional electrode structure is processed, the rotation can be axial rotation around the tungsten wire rod for uniform etching, or axial deflection around the tungsten wire rod for local etching, and then micro-nano electrodes and complex-shaped electrodes are prepared.

[0048] Further, by making the non-metallic annular ring 12 lower than the metallic annular ring 11, the electrochemical etching reactions on both sides of the electrode to be processed 9 tend to be consistent; for example, the micro-nano electrode product obtained by electron microscopy observation is drawn to draw the electrochemical etching simulation diagram under the corresponding liquid film morphology, as shown in Figure 3 (e) as shown, when the non-metallic annular ring 12 is lower than the metallic annular ring 11, the liquid film morphology is different, and at this time the electrochemical etching of the tungsten wire rod close to the two sides of the metallic annular ring 11 and the non-metallic annular ring 12 is almost the same, then the consistency of the electrochemical etching reaction can be further improved by regulating the liquid film morphology, for example, the preparation of electrodes with stepped or variable diameter structure is prepared by alternating use of the enhanced electrochemical etching control, and then micro-nano electrodes and complex-shaped electrodes are prepared.

[0049] Preferably, the metallic annular ring 11 is located in the non-metallic annular ring 12; for example, as shown in Figure 1 As shown, the outer diameter of the metallic annular ring 11 is smaller than the outer diameter of the non-metallic annular ring 12, and the coaxial nesting arrangement can make the metallic annular ring 11 located in the non-metallic annular ring 12, and the tungsten wire rod located between the two, which can make the electric field lines point to the metal ring from the electrode to be processed 9, further improving the uniformity of the reaction of the electrode to be processed 9.

[0050] Example 2:

[0051] In order to further realize the micro-nano electrode preparation method based on the liquid film morphology regulation technology described above, and promote automatic large-scale production and stable processing, as shown in Figures 4-5 As shown in the figure, it is a preferred embodiment of the micro-nano electrode preparation device based on the liquid film morphology regulation technology of the present application, which comprises a driving mechanism, a direct current power supply 25, a metallic annular ring 11 and a non-metallic annular ring 12 arranged in a coaxial nesting manner; the driving mechanism is based on the micro-nano electrode preparation method based on the liquid film morphology regulation technology described in embodiment 1, and is used to drive the electrode to be processed 9 to rotate between the metallic annular ring 11 and the non-metallic annular ring 12, and drive the metallic annular ring 11 and the non-metallic annular ring 12 to move along the axial direction, the positive electrode of the direct current power supply 25 is connected to the electrode to be processed 9, and the negative electrode of the direct current power supply 25 is connected to the metallic annular ring 11.

[0052] The device can realize different liquid film forms by selecting metal rings 11 and non-metal rings 12 with different cross-sectional diameters, or by adjusting the relative positions of the metal rings 11 and the non-metal rings 12 through the driving mechanism by driving the metal rings 11 and the non-metal rings 12 to move relatively along the axial direction. After starting the direct current power supply 25, the driving mechanism drives the electrode to be processed 9 to rotate between the metal rings 11 and the non-metal rings 12, so that the electrode to be processed 9 rotates and undergoes an electrochemical etching reaction in the electrolyte liquid film 23, until the electrode to be processed 9 is disconnected to form a micro-nano electrode, so as to prepare an electrode with higher precision and a complex-shaped electrode.

[0053] Further, the driving mechanism is used to drive the electrode to be processed 9, the metal rings 11 and the non-metal rings 12 to move relatively in three-dimensional directions, for example: Figure 4 As shown, the driving mechanism drives the tungsten rod to move left and right, up and down relative to the metal rings 11 and the non-metal rings 12, and drives the metal rings 11 and the non-metal rings 12 to move forward and backward relative to the tungsten rod, so as to adjust the relative positions of the tungsten rod and the metal rings 11 and the non-metal rings 12, automatically pass the electrode to be processed 9, i.e. the tungsten rod, between the coaxially nested metal rings 11 and the non-metal rings 12, and promote the electrode to be processed 9 to react uniformly.

[0054] Further, the driving mechanism includes an X-axis moving assembly 4, a Y-axis moving assembly 3, a Z-axis moving assembly 5 and a main shaft 6. The X-axis moving assembly 4 is used to drive the Z-axis moving assembly 5 to move left and right, the Y-axis moving assembly 3 is used to drive the metal rings 11 and the non-metal rings 12 to move forward and backward, the Z-axis moving assembly 5 is used to drive the main shaft 6 to move up and down, and the main shaft 6 is used to drive the electrode to be processed 9 to rotate along the axial direction of the main shaft 6, for example: Figure 4As shown, the tungsten wire rod is installed on the main shaft 6, the X-axis moving assembly 4 is arranged on the moving support 2, the Z-axis moving assembly 5 is driven by the lead screw of the X-axis moving assembly 4 to move left and right as the slider of the X-axis moving assembly 4, that is, to drive the tungsten wire rod to move left and right, adjust the lateral centering of the tungsten wire rod and the liquid film, the slider of the Y-axis moving assembly 3 supports the installation of the metal ring 11 and the non-metal ring 12, and the metal ring 11 and the non-metal ring 12 are driven by the lead screw of the Y-axis moving assembly 3 to move forward and backward, which cooperates with the X-axis moving assembly 4 to realize two-dimensional plane calibration of the liquid film and the tungsten wire rod, the main shaft 6 is installed on the slider of the Z-axis moving assembly 5, and the main shaft 6 is driven by the lead screw of the Z-axis moving assembly 5 to drive the tungsten wire rod to move up and down, control the height of the tungsten wire rod relative to the liquid film, realize the relative movement of the to-be-processed electrode 9, the metal ring 11 and the non-metal ring 12 in three-dimensional directions, and drive the to-be-processed tungsten wire rod to rotate along the main shaft 6 by the main shaft 6, so as to realize uniform circumferential etching, which can further simplify the structure of the driving mechanism and improve the operation stability.

[0055] Further, the Y-axis moving assembly 3 is provided with an electrode receiver 10, for example: Figure 4 As shown, the electrode receiver 10 is located below the metal ring 11 and the non-metal ring 12, and is moved to ensure that the tungsten wire rod is located above the electrode receiver 10, which can further facilitate the collection of the micro-nano electrode obtained by the electrode receiver 10.

[0056] Further, the main shaft 6 is provided with a chuck 7, and the chuck 7 is provided with a cross purple copper rod 8 matched with the to-be-processed electrode 9, for example: Figure 4 As shown, the cross purple copper rod 8 is locked by the chuck 7 below the main shaft 6, and the tungsten wire rod is placed in the cross purple copper rod 8, which can further facilitate the taking and placing of the to-be-processed electrode 9 and improve the processing efficiency.

[0057] Further, the driving mechanism comprises a first support 15 and a linear stepping device 17, the first support 15 is used for supporting the metal ring 11, and the linear stepping device 17 is used for driving the non-metal ring 12 to move back and forth along the axial direction; or, the first support 15 is used for supporting the non-metal ring 12, and the linear stepping device 17 is used for driving the metal ring 11 to move back and forth along the axial direction; for example: Figure 4 As shown, the metal ring 11 is placed in the first support 15 and fixed on the metal ring support 13 by the first screw 16, and the bottom of the metal ring support 13 is fixed on the Y-axis moving assembly 3 through the first bolt 14, as shown in Figure 4 and Figure 7As shown, the linear stepping device 17 is provided with a second support 21, the non-metallic ring 12 is placed in the second support 21 and is fixed on the connecting piece 20 through the second screw 22, the connecting piece 20 is connected with the moving slide 19 of the linear stepping device 17, the linear stepping device 17 is fixed on the Y-axis moving assembly 3 through the second bolt 18, the moving slide 19 is driven to move up and down by the lead screw of the linear stepping device 17, and in turn drives the non-metallic ring 12 to move up and down, that is, drives the non-metallic ring 12 to reciprocate along the axial direction, which can further facilitate the control of the relative position adjustment of the metal ring 11 and the non-metallic ring 12 along the axial direction.

[0058] Further, the linear stepping device 17 is provided with a second support 21, the second support 21 and the first support 15 are both provided with a groove 28, for example: Figure 1 As shown, the metal ring 11 and the non-metallic ring 12 have a rod part extending from the side, for example: Figure 4 and Figure 6 As shown, the rod part of the metal ring 11 is supported by the groove 28 of the first support 15 to realize the placement of the metal ring 11, for example: Figure 4 and Figure 7 As shown, the rod part of the non-metallic ring 12 is supported by the groove 28 of the second support 21 to realize the placement of the non-metallic ring 12, which can further improve the support stability of the metal ring 11 and the non-metallic ring 12.

[0059] Further, the isolation base 1 including a driving mechanism, for example: Figure 4 As shown, the movement support 2 and the Y-axis moving assembly 3 are installed on the isolation base 1, the slider of the Y-axis moving assembly 3 can move back and forth relative to the isolation base 1, the isolation base 1 can be used as a basic support component of the driving mechanism, further through the isolation of environmental vibration to ensure the relative position accuracy of the metal ring 11, the non-metallic ring 12 and the electrode to be processed 9, avoid the problems of liquid film rupture, etching position deviation caused by vibration, improve the operation stability and operation precision.

[0060] Further, an electron microscope 26 is included towards the metal ring 11 and the non-metallic ring 12, for example: Figure 5 As shown, the electron microscope 26 is used to watch the shape of the electrolyte liquid film 23, the relative position of the metal ring 11 and the non-metallic ring 12, and the required liquid film shape is determined through the electron microscope 26, which can further improve the operation precision.

[0061] Further, a control device 27 connected with the electron microscope 26 is included, the control device 27 is used to control the operation of the driving mechanism, for example: Figure 5As shown, the X-axis moving assembly 4, the Y-axis moving assembly 3, the Z-axis moving assembly 5, the main shaft 6, the linear stepping device 17, and the electron microscope 26 are electrically connected with the control device 27. The X-axis moving assembly 4, the Y-axis moving assembly 3, the Z-axis moving assembly 5, and the linear stepping device 17 are driven by stepping motors, so that the X-axis moving assembly 4, the Y-axis moving assembly 3, and the Z-axis moving assembly 5 can accept the position instructions of the control device 27 and feed back the actual displacement. The control device 27 controls the rotation speed and start-stop of the main shaft 6. The linear stepping device 17 is executed by the control device 27 to perform micro-feeding or positioning. The real-time image is obtained by the electron microscope 26 and transmitted to the control device 27 for visual feedback. The device operation can be further coordinated by the control device 27 to improve the operation precision and processing efficiency.

[0062] For example, the electrode 9 to be processed is a tungsten wire rod, the outer diameter of the metal ring 11 is smaller than the outer diameter of the non-metal ring 12, and the metal ring 11 is located inside the non-metal ring 12. The assembly and preparation process of the above device can include the following steps:

[0063] (1) respectively install the metal ring support 13 and the linear stepping device 17 on the Y-axis moving assembly 3;

[0064] (2) the metal ring 11 and the non-metal ring 12 can have different diameters. The metal ring 11 is installed horizontally on the metal ring support 13 through the first support 15, and the non-metal ring 12 is installed horizontally on the linear stepping device 17 through the second support 21 and the connecting piece 20. The positions of the two are adjusted so that the metal ring 11 and the non-metal ring 12 are coaxially nested;

[0065] (3) place the electrode receiver 10 on the Y-axis moving assembly 3 and below the metal ring 11 and the non-metal ring 12;

[0066] (4) clamp the tungsten wire rod in the cross-shaped copper rod 8 and install it on the main shaft 6 with the chuck 7;

[0067] (5) control the Y-axis moving assembly 3, the X-axis moving assembly 4, and the Z-axis moving assembly 5 by the control device 27 to adjust the position of the tungsten wire rod, so that the tungsten wire rod vertically passes through the metal ring 11 and the non-metal ring 12 and is located directly above the electrode receiver 10;

[0068] (6) add electrolyte between the metal ring 11 and the non-metal ring 12 to form an electrolyte liquid film 23, and use the metal ring 11 and the non-metal ring 12 to support the electrolyte liquid film 23;

[0069] (7) The morphology of the electrolyte liquid film 23 is observed by an electron microscope 26, and the moving slide 19 of the linear stepping device 17 is driven to move the non-metallic ring 12 up and down by the control device 27 to change the relative position of the metallic ring 11 and the non-metallic ring 12, including the two being in a horizontal state, the two being in a high-low state, etc., to control the ring-solution interface size and the liquid film direction, so as to realize the regulation of the morphology of the electrolyte liquid film 23;

[0070] (8) The negative electrode of the direct current power supply 25 is connected to the metallic ring 11, and the positive electrode is connected to the tungsten wire rod, and the switch 24 is turned on;

[0071] (9) The control device 27 controls the rotation of the main shaft 6, so that the tungsten wire rod uniformly undergoes an electrochemical etching reaction in the electrolyte liquid film 23;

[0072] (10) With the electrochemical etching reaction, part of the tungsten wire rod in the electrolyte liquid film 23 will become thinner and thinner, and finally will be pulled off under the gravity of the lower tungsten wire rod and fall into the electrode receiver 10, thereby completing the preparation of the micro-nano electrode.

[0073] In summary, the above device converts the liquid film morphology from a passive influencing factor in traditional technology into an active control variable, improves the precision and process stability of the prepared electrode, can realize the micro-nano scale preparation of the electrode and the online preparation of the complex shape electrode, has the advantages of high machining precision, good surface quality, high micro-fineness, simple equipment, easy integration, etc., is conducive to opening up a new research direction and providing a basis for application scenarios in the field of micro-nano machining, and has good industrial adaptability.

[0074] The above series of detailed descriptions are only specific descriptions of the feasible embodiments of the present application, and are not used to limit the protection scope of the present application. Any equivalent embodiments or changes made without departing from the spirit of the present application should be included in the protection scope of the present application.

Claims

1. A method for fabricating micro / nano electrodes based on liquid film morphology control technology, characterized in that, The methods include: The electrode to be processed (9) is passed between the metal ring (11) and the non-metal ring (12) arranged in a coaxial nested configuration; An electrolyte is added between a metal ring (11) and a non-metal ring (12) to form an electrolyte film (23); The electrode to be processed (9) is connected to the positive terminal of the DC power supply (25), and the metal ring (11) is connected to the negative terminal of the DC power supply (25). By adjusting the relative position of the metal ring (11) and the non-metal ring (12) in the axial direction; and / or, adjusting the cross-sectional diameter of the metal ring (11); and / or, adjusting the cross-sectional diameter of the non-metal ring (12), the shape of the electrolyte film (23) is controlled, so that the electrode to be processed (9) rotates and an electrochemical etching reaction occurs in the electrolyte film (23) until the electrode to be processed (9) is disconnected to form a micro-nano electrode.

2. The method for fabricating micro / nano electrodes based on liquid film morphology control technology according to claim 1, characterized in that, By adjusting the non-metallic ring (12) to be flush with or higher than the metal ring (11) in the axial direction, and / or by increasing the cross-sectional diameter of the metal ring (11), the electrochemical etching reaction of the electrode (9) to be processed on the side closer to the metal ring (11) becomes more intense; by adjusting the non-metallic ring (12) to be lower than the metal ring (11) in the axial direction, the electrochemical etching reactions on both sides of the electrode (9) to be processed tend to be consistent.

3. The method for fabricating micro / nano electrodes based on liquid film morphology control technology according to claim 1, characterized in that, The metal ring (11) is located inside the non-metal ring (12).

4. A micro / nano electrode fabrication device based on liquid film morphology control technology, characterized in that, The device includes a driving mechanism, a DC power supply (25), and a metal ring (11) and a non-metal ring (12) arranged in a coaxial nested configuration. The driving mechanism operates based on the micro / nano electrode preparation method based on liquid film morphology control technology as described in any one of claims 1 to 3. It is used to drive the electrode to be processed (9) to rotate between the metal ring (11) and the non-metal ring (12) and to drive the metal ring (11) and the non-metal ring (12) to move relative to each other along the axial direction. The positive terminal of the DC power supply (25) is connected to the electrode to be processed (9), and the negative terminal of the DC power supply (25) is connected to the metal ring (11).

5. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 4, characterized in that, The driving mechanism is used to drive the electrode to be processed (9), the metal ring (11) and the non-metal ring (12) to move relative to each other in three dimensions.

6. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 5, characterized in that, The driving mechanism includes an X-axis moving component (4), a Y-axis moving component (3), a Z-axis moving component (5), and a spindle (6). The X-axis moving component (4) is used to drive the Z-axis moving component (5) to move left and right. The Y-axis moving component (3) is used to drive the metal ring (11) and the non-metal ring (12) to move back and forth. The Z-axis moving component (5) is used to drive the spindle (6) to move up and down. The spindle (6) is used to drive the electrode to be processed (9) to rotate along the spindle (6) axis.

7. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 6, characterized in that, The Y-axis moving assembly (3) is provided with an electrode receiver (10), the spindle (6) is provided with a chuck (7), and the chuck (7) is provided with a cross copper rod (8) that cooperates with the electrode (9) to be processed.

8. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 4, characterized in that, The driving mechanism includes a first support member (15) and a linear stepping device (17). The first support member (15) is used to support the metal ring (11), and the linear stepping device (17) is used to drive the non-metallic ring (12) to reciprocate along the axial direction; or, the first support member (15) is used to support the non-metallic ring (12), and the linear stepping device (17) is used to drive the metal ring (11) to reciprocate along the axial direction.

9. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 4, characterized in that, This includes a vibration isolation base (1) for setting the drive mechanism.

10. The micro / nano electrode fabrication device based on liquid film morphology control technology according to claim 4, characterized in that, It includes an electron microscope (26) and a control device (27) connected together, the electron microscope (26) facing the metal ring (11) and the non-metal ring (12), and the control device (27) for controlling the operation of the drive mechanism.

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