CN114131125B - Tool electrode with surface hydrophobic structure and preparation method thereof - Google Patents
Tool electrode with surface hydrophobic structure and preparation method thereof Download PDFInfo
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- CN114131125B CN114131125B CN202111443964.XA CN202111443964A CN114131125B CN 114131125 B CN114131125 B CN 114131125B CN 202111443964 A CN202111443964 A CN 202111443964A CN 114131125 B CN114131125 B CN 114131125B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
- B23H1/00—Electrical discharge machining, i.e. removing metal with a series of rapidly recurring electrical discharges between an electrode and a workpiece in the presence of a fluid dielectric
- B23H1/04—Electrodes specially adapted therefor or their manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23H—WORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
- B23H3/00—Electrochemical machining, i.e. removing metal by passing current between an electrode and a workpiece in the presence of an electrolyte
- B23H3/04—Electrodes specially adapted therefor or their manufacture
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/022—Electroplating of selected surface areas using masking means
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/60—Electroplating characterised by the structure or texture of the layers
- C25D5/605—Surface topography of the layers, e.g. rough, dendritic or nodular layers
Abstract
The application relates to the technical field of special processing, in particular to a tool electrode with a surface hydrophobic structure and a preparation method thereof, wherein the tool electrode consists of an electrode substrate and an array ball pit microstructure arranged on the side wall surface of the electrode substrate, and the array ball pit microstructure is provided with a plurality of ball pits which are arranged in a hexagon shape. The array ball pit structure is used as a surface hydrophobic structure, a resident air film used as a side wall insulating layer is formed on the surface of the electrode, and the array ball pit structure can play a role in side wall insulation and stable processing in electrochemical machining or discharge-assisted chemical machining. The embodiment of the application can solve the problems of poor continuity and uneven distribution of the array microstructure caused by the curvature change of the surface of the micro-fine cylindrical electrode, and improves the service performance of the tool electrode with the surface hydrophobic structure.
Description
Technical Field
The application relates to the technical field of special processing, in particular to a tool electrode with a surface hydrophobic structure and a preparation method thereof.
Background
In recent years, advanced engineering materials have been rapidly developed, and various alloys, polymer materials, and the like having special physicochemical properties have been developed. Manufacturing techniques for these materials face significant challenges due to their extreme properties in terms of mechanical strength, brittleness, etc. Electrochemical Machining (ECM) is a material processing method based on electrochemical reaction, has the principle advantages of good integrity of a processed surface and online controllable size, is suitable for conductive alloy materials difficult to process, and has no influence on mechanical properties. A composite processing method developed based on electrolytic processing is represented by discharge Assisted Chemical engineering (SACE), and materials are removed based on a physical and Chemical combined action of electrolytic gas film breakdown discharge generated on a tool electrode, so that the ECM and SACE processes are receiving more and more attention because the materials are suitable for processing hard and brittle insulating materials such as silicon, quartz, and ceramics and organic polymer insulating materials without damage.
Stray corrosion due to the anodic dissolution principle is a bottleneck problem in the ECM process, and anodic dissolution occurs whenever there is an electric field in the electrolyte, thereby affecting process localisation. Stray corrosion is suppressed with a side-wall insulated tool electrode, but the side-wall insulation film on the electrode surface is difficult to prepare and has a limited lifetime. In the SACE process, the generation rate, the form and the stability of the air film (air bubble) wrapping the electrode have important influence on the discharge effect, and the processing quality and the processing efficiency are directly influenced, however, the air bubble transportation process and the air film form in the processing are difficult to control. Theoretical and experimental research results show that when the growth radius of bubbles on the surface of the metal electrode material is smaller, the bubbles tend to leave the surface, and a continuous resident gas film is difficult to form; on the contrary, on the surface of the hydrophobic material, the bubble growth radius can reach a larger value, a continuous resident gas film is prone to be formed, and the gas film can be stably maintained on the super-hydrophobic surface underwater for a long time through electrochemical gas generation. Therefore, the behavior of surface bubbles can be changed by changing the hydrophilic and hydrophobic properties of the surfaces of the ECM and SACE tool electrodes, the hydrophobic surface tool electrodes are expected to improve the gas film form, and a continuous and compact gas film is formed on the surfaces of the electrodes to serve as a side wall insulating layer in the ECM so as to inhibit the effect of stray corrosion; and the method can also be used for improving the distribution rule of bubbles or air films in the SACE and improving the processing quality and precision.
It is very challenging to produce a stable and corrosion resistant superhydrophobic surface on an intrinsically hydrophilic metal cylindrical electrode. The two common methods at present are surface roughening (such as chemical etching, laser ablation and the like) and modification method of low surface free energy substances (such as fluorosilane, mercaptan and the like). However, in the processing environment of ECM and SACE, the low-energy surface modifier is easily detached due to the generation of electrolytic bubbles, the scouring and corrosion of the electrolyte, and the harsh physicochemical environment such as high temperature and high pressure discharge, and the hydrophobic surface electrode manufactured by the method has poor durability. Secondly, a special micro-nano composite structure is manufactured on the metal surface, so that the stress balance condition of a gas-liquid interface is met, such as an array micro-groove, an array ball pit and other structures, and the method is a reference method for manufacturing a long-term reliable hydrophobic surface, but the method is only used for manufacturing a large-area large-scale plane at present. The curvature change of the surface of the micro-scale cylindrical tool electrode is large, and the array microstructures are distributed on the surface of the micro-scale cylindrical tool electrode continuously and uniformly, so that the manufacturing and application on the micro-scale cylindrical surface are not realized. The application of the tool electrode with the surface hydrophobic structure to ECM and SACE technological processes is also proposed for the first time, and how to evaluate the surface air film performance is still to be explored.
Disclosure of Invention
The application provides a tool electrode with a surface hydrophobic structure and a preparation method thereof, which can solve the difficult problems of poor continuity and uneven distribution of an array microstructure caused by the change of the surface curvature of a micro-fine cylindrical electrode, improve the service performance of the tool electrode with the surface hydrophobic structure, form a continuous and stable air film on the surface of the electrode, and respectively play roles in insulating the side wall and improving the processing stability in ECM and SACE.
The embodiment of the first aspect of the present application provides a tool electrode with a surface hydrophobic structure, where the tool electrode is composed of an electrode substrate and an array ball pit microstructure disposed on a side wall surface of the electrode substrate;
the electrode substrate is cylindrical and is made of copper or nickel;
the array ball pit microstructure is provided with a plurality of ball pits which are arranged in a hexagon shape, the material of the ball pits is copper or nickel, the array ball pit structure is used as a surface hydrophobic structure, and a resident air film which is used as a side wall insulating layer is formed on the surface of the electrode.
Optionally, according to an embodiment of the application, the radius of the ball pit is in the range of 0.5 μm-10 μm.
Optionally, according to an embodiment of the application, the angle between the tangent to the entrance of the ball pit and the horizontal is in the range of 60 ° -65 °.
In a second aspect, the present application provides a method for preparing a tool electrode with a surface hydrophobic structure, where the tool electrode is the tool electrode with a surface hydrophobic structure according to the above embodiment, and the method includes the following steps:
s1, dropping deionized water on a provided substrate to form a water film;
s2, sucking the microsphere-water-ethanol suspension, and injecting the suspension along the edge of the substrate to diffuse the suspension into the water film to form a self-assembled single-layer template;
s3, inserting a metal rod into the lower part of the single-layer template in an inclined mode, taking the single-layer template out of the water surface, rotating the single-layer template for 360 degrees, enabling the single-layer template to be uniformly attached to the surface of the metal rod, and drying the metal rod;
s4, performing electrochemical deposition on copper by taking the metal rod covered with the single-layer template as an anode, filling the deposited metal into the microsphere gaps of the single-layer template after the deposition time is preset, and drying after the preset height is formed;
s5, soaking the metal rod, chemically removing the microspheres, drying after washing, and polishing the end face of the metal rod by using abrasive paper to obtain the tool electrode.
Optionally, according to an embodiment of the present application, in S1, the substrate is a glass sheet, the substrate is treated by soaking with a surfactant, the surfactant is sodium dodecyl sulfate, the concentration is in a range of 5% to 20%, and the soaking time is in a range of 12h to 48 h.
Optionally, according to an embodiment of the present application, in S1, the volume of the deionized water added dropwise is L in μ L, and is in a range of 0.4S to 1.0S, where S is the area of the substrate in mm 2 。
Optionally, according to an embodiment of the present application, in S2, the microsphere-water-ethanol suspension is a mixture of monodisperse polystyrene microspheres, deionized water and ethanol, wherein the diameter of the polystyrene microspheres is in a range of 0.5 μm to 10 μm, the mass fraction of the polystyrene microspheres is in a range of 0.5wt% to 2wt%, and the ratio of the deionized water to the ethanol is in a range of 0.5 to 2.
Optionally, according to an embodiment of the present application, in S2, the volume of the microsphere-water-ethanol suspension injected into the water film is L in μ L, and is in a range of 0.04S to 0.1S, where S is the area of the substrate in mm 2 。
Alternatively, according to an embodiment of the present application, in S4, the metal bar covered with the single-layered template is used as an anode, and the electrochemical deposition is performed in an electrolytic cell using an electrolyte solution of copper sulfate or nickel sulfate having a concentration in a range of 0.05mol/L to 0.5mol/L, and a thickness of the deposition layer is controlled by a deposition time.
Optionally, according to an embodiment of the present application, in S5, a chemical reagent used for removing the polystyrene microspheres is tetrahydrofuran, and the soaking time is 1 to 4 hours.
According to the tool electrode with the surface hydrophobic structure and the preparation method thereof, the spherical pit microstructures arranged in an array mode are designed on the surface of the cylindrical electrode, the size and the arrangement mode of the spherical pits are designed according to the surface wetting behavior basic theory, a continuous template is formed by a self-assembly method in the microstructure preparation, and the pit structures are formed by utilizing an electrochemical deposition process. A gas film form observation mode is adopted to represent the continuous gas film formed on the surface of the tool electrode and the insulation characteristics of the side wall, the feasibility and the effectiveness of the application of the gas film form observation mode in the ECM and SACE processes are verified, and the difficulty in manufacturing the hydrophobic structure of the array on the surface of the cylindrical electrode can be solved.
Additional aspects and advantages of the present application will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the present application.
Drawings
The foregoing and/or additional aspects and advantages of the present application will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of a tool electrode with a surface hydrophobic structure provided in accordance with an embodiment of the present disclosure;
FIG. 2 is a schematic representation of a system according to the present applicationThe embodiment provides a schematic diagram of a spherical pit; wherein, D-the opening diameter of the ball pit; r cav -a ball pit radius; h-ball pit depth;
-the angle between the tangent to the entrance of the ball pit and the horizontal;
fig. 3 is a schematic diagram of application of a tool electrode having a surface hydrophobic structure in an ECM according to an embodiment of the present disclosure;
fig. 4 is a schematic diagram of an application of a tool electrode having a surface hydrophobic structure in a SACE according to an embodiment of the present application;
FIG. 5 is a schematic structural diagram of a performance testing apparatus for a tool electrode having a surface hydrophobic structure according to an embodiment of the present disclosure;
FIG. 6 is a schematic diagram illustrating a performance testing process of a tool electrode according to an embodiment of the present disclosure;
FIG. 7 is a flow chart of a method for preparing a tool electrode with a surface hydrophobic structure according to an embodiment of the present disclosure;
FIG. 8 is a flow chart of a process for preparing a tool electrode with a hydrophobic surface structure according to an embodiment of the present disclosure; wherein, A-substrate; b-a water film; c-microsphere-water-ethanol suspension; d-a single-layer template; e-a metal rod; f-a tool electrode;
fig. 9 is a schematic diagram illustrating a thickness variation law of a deposition layer according to an embodiment of the present disclosure.
Reference numerals: 1-a tool electrode with a surface hydrophobic structure; 101-an electrode substrate; 2-array ball pit microstructure; 201-ball pits; 3-an electrode holder; 4-a workpiece; 5-an electrolyte; 6-a power supply; 7-electrode holder; 8-workpiece; 9-an electrolyte; 10-a power supply; 11-an auxiliary electrode; 12-a triaxial motion platform, 13-a pulse power supply, 14-an electrode clamp, 15-a conductive anode strip, 16-an insulating anode strip, 17-electrolyte, 18-an electrolytic cell, 19-a high-speed camera, 20-a light source and 21-a computer.
Detailed Description
Reference will now be made in detail to the embodiments of the present application, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative and intended to explain the present application and should not be construed as limiting the present application.
Fig. 1 is a schematic view of a tool electrode having a surface hydrophobic structure according to an embodiment of the present disclosure.
As shown in fig. 1, the tool electrode with the surface hydrophobic structure is composed of an electrode substrate 101 and an array ball pit microstructure 2 arranged on a side wall surface of the electrode substrate.
Optionally, in an embodiment of the present application, the electrode base 101 has a cylindrical shape, and the material of the electrode base 101 is copper or nickel.
The array ball pit microstructure 2 is provided with a plurality of ball pits 201 which are arranged in a hexagon shape, the material of the ball pits is copper or nickel, the array ball pit structure is used as a surface hydrophobic structure, and a resident air film which is used as a side wall insulating layer is formed on the surface of an electrode.
Specifically, the array ball pit microstructures 2 are distributed on the side wall surface of the electrode substrate 101 and are composed of ball pits 201 which are closely arranged, the ball pits 201 are arranged in a planar hexagonal shape on the surface of the electrode substrate 101, and the array ball pit microstructures 2 are made of copper or nickel and the like.
Optionally, in one embodiment of the present application, the radius of the ball pit is in the range of 0.5 μm to 10 μm.
Optionally, in one embodiment of the present application, the angle between the tangent to the entrance of the ball pit and the horizontal is in the range of 60 ° -65 °.
Specifically, the radius R of the single ball pit 201 cav In the range of 0.5 to 10 μm, as shown in FIG. 2, the specific size thereof may be determined according to the designed electrode diameter d e Optimized selection of R cav At (0.001-0.1) d e Within the range. Included angle between tangent line of ball pit inlet and horizontal plane
In the range of 60-65 deg..
As a specific example, the tool electrode 1 is composed of an electrode base body 101 and an array ball pit microstructure 2, wherein the electrode substrate 101 is a cylinder with the diameter of 500 mu m and is made of copper; the array ball pit microstructure 2 is distributed on the side wall surface of the electrode base body 101 and is composed of ball pits 201 which are closely arranged, the ball pits 201 are arranged in a plane hexagon mode, and the material is copper. Radius R of a single ball pit 201 cav Within 500nm, the included angle between the tangent line of the entrance of the ball pit and the horizontal
Is 60 degrees.
The tool electrode having the surface hydrophobic structure described in the above embodiment may be applied to ECM processing, as shown in fig. 3, in which 3 is an electrode holder; 4 is a workpiece; 5 is an electrolyte; and 6 is a power supply. The growth radius of bubbles on the surface of the tool electrode with the surface hydrophobic structure can reach a larger value, a continuous resident air film is formed on the surface of the electrode, a stray current path between the tool electrode and a processing workpiece is blocked, a side wall insulating layer is used, stray corrosion is inhibited, and the processing precision of an ECM process is improved.
The tool electrode with surface hydrophobic structure described in the above embodiments can be applied in SACE process, as shown in fig. 4, where 7 is the electrode holder; 8 is a workpiece; 9 is an electrolyte; 10 is a power supply; and 11 is an auxiliary electrode. The continuous resident gas film is formed on the surface of the tool electrode with the surface hydrophobic structure, so that a stable discharge channel between the electrode and a workpiece is ensured, and the processing efficiency and the stability of the SACE technological process are improved.
In the embodiment of the present application, the performance of the tool electrode with a surface hydrophobic structure is tested by a performance testing device, as shown in fig. 5, the testing device includes a triaxial movement platform 12, a pulse power supply 13, an electrode holder 14, a conductive anode sheet 15, an insulating anode sheet 16, an electrolyte 17, an electrolytic cell 18, a high-speed camera 19, a light source 20, and a computer 21. The tool electrode 1 is installed on the triaxial moving platform 12 through an electrode clamp 14, part of the tool electrode is immersed in electrolyte 17 in an electrolytic cell 18, a conductive anode sheet 15 and an insulating anode sheet 16 are respectively installed and immersed in the electrolyte 17 in the electrolytic cell 18, the conductive anode sheet 15 and the tool electrode with a surface hydrophobic structure are respectively connected to the positive pole and the negative pole of a pulse power supply 13 through leads, the wall surface of the electrolytic cell 18 is made of a transparent material, and an electrochemical phenomenon, bubbles and a gas film form are observed from the side by a high-speed camera 19 and recorded in a computer 21.
As a specific example, the tool electrode was tested by the apparatus shown in FIG. 5, and a tool electrode 1 having a diameter of 500 μm was mounted on a triaxial moving platform 12 via an electrode holder 14, and immersed in an electrolyte 17 of 1mm in depth in an electrolytic bath 18, which was 1mol/L NaClO 3 The conductive anode sheet 15 and the insulating anode sheet 16 are respectively graphite and quartz glass, both are arranged and immersed in the electrolyte 17, the conductive anode sheet 15 and the tool electrode 1 are respectively connected to the positive pole and the negative pole of the pulse power supply 13 through leads, the wall surface of the electrolytic cell 18 is organic glass, and the electrochemical phenomenon and the forms of bubbles and air films are observed from the side surface by the high-speed camera 19 and recorded in the computer 21.
The performance flow of the tool electrode with the surface hydrophobic structure is shown in fig. 6, firstly, the high-speed camera 19 is turned on, the distance between the end surface of the tool electrode 1 and the conductive anode sheet 15 is adjusted to 50-1000 μm, and the end surface and the conductive anode sheet appear in the field of view of the high-speed camera 19, and video recording is started; then, the pulse power supply 13 is turned on, and the position where the bubbles are generated is observed and recorded; observing the motion track of the bubbles and recording; observing the form of the air film formed on the surface of the electrode, and recording; secondly, adjusting the distance between the end face of the tool electrode 1 and the insulating anode piece 16 to 50-1000 μm, enabling the end face and the insulating anode piece to appear in a visual field of a high-speed camera 19, starting to record video, adjusting to high voltage, observing the movement track of bubbles, and recording; observing the form of the air film formed on the surface of the electrode, and recording; observing and recording the discharge position; and finally, closing the statistical data of the testing equipment and evaluating the performance of the tool electrode.
As a specific example, the tool electrode performance was tested by the procedure shown in FIG. 6, first, the high-speed camera 19 was turned on, the distance between the end face of the tool electrode 1 and the conductive anode sheet 15 was adjusted to 50 μm and both appeared in the field of view of the high-speed camera 19, and video recording was started with fps set to 100; then, a pulse power supply 13 is turned on, voltage 10V is output, and the position of bubble generation, the track of bubble movement and the air film form formed on the surface of the electrode are observed and recorded; then, adjusting the distance between the end face of the tool electrode 1 and the insulating anode sheet 16 to 10 μm, enabling the end face and the insulating anode sheet to appear in the field of view of the high-speed camera 19, starting video recording, and setting fps to be 100; adjusting the output voltage of the pulse power supply 13 to 100V, observing the movement track of bubbles, the form of an air film and the discharge position, and recording; and finally, closing the statistical data of the test equipment.
From the characteristics of the bubble movement, the air film form and the like observed above, the insulating property of the air film is analyzed: the air bubble generating positions are all at the end parts and have excellent insulating property, and the air bubble generating positions are at the side walls and have poor insulating property; the track of the movement of the bubbles is good in insulating property towards the liquid level direction, and the track of the movement of the bubbles is radial away from the electrode and is poor in insulating property; the gas film has compact form and excellent insulating property, and the gas film has dispersed form and poor insulating property; similarly, the air film quality is excellent when the moving track of the air bubble is towards the liquid level direction, and the moving track of the air bubble is radial away from the electrode and is poor; the gas film is compact in shape, stable, and unstable when dispersed; the quality of the gas film is excellent when the discharging position is on the side wall with few end faces, and the quality of the gas film is poor when the discharging position is on the side wall with many end faces.
According to the tool electrode with the surface hydrophobic structure, the hydrophobic surface is formed by the array ball pit structure on the surface of the metal electrode; the continuous gas film formed on the side wall surface of the electrode can play a role in insulating the side wall and stabilizing the processing process; the adopted materials are all metals, no chemical modifier is used, and the prepared hydrophobic electrode has better durability; the size of the ball pit can be adjusted through the size of the microsphere template and the electrochemical deposition time, so that different application requirements are met; the process has application potential of mass production, and solves the problem that the array microstructures cannot be continuously and uniformly distributed on the surface of the micro-scale cylindrical tool electrode in the related technology due to large surface curvature change of the micro-scale cylindrical tool electrode.
Next, a method for manufacturing a tool electrode having a surface hydrophobic structure according to an embodiment of the present application will be described with reference to the accompanying drawings.
Fig. 7 is a flowchart of a method for manufacturing a tool electrode having a surface hydrophobic structure according to an embodiment of the present disclosure.
As shown in fig. 7, the tool electrode is the tool electrode with the surface hydrophobic structure of the above embodiment, and the preparation method includes the following steps:
step S1, deionized water is dripped on the provided substrate to form a water film.
First, a substrate a is provided, as shown in fig. 8 (a). Deionized water is dropped on the substrate a to form a water film B of a certain thickness, as shown in fig. 8 (B).
In one embodiment, a glass sheet having an area S in mm may be used as substrate A 2 The substrate A needs to be soaked by a surfactant, so that the hydrophilic capability of the substrate A is improved, and the gas-liquid interface of the formed water film B is flatter. The surfactant used is preferably Sodium Dodecyl Sulfate (SDS) with a concentration in the range of 5% to 20%, preferably 10%, and a soaking time of 12 to 48 hours, preferably 24 hours.
A water film B is fully paved on a substrate A (the area is S/mm) 2 ) In the case of the surface, the thickness of the water film B formed depends on the volume L (in. Mu.L) of the deionized water added dropwise, where L is in the range of (0.4-1.0) S, preferably 0.8S, and the thickness of the water film formed is about 1mm.
And S2, sucking the microsphere-water-ethanol suspension, injecting the suspension along the edge of the substrate, and diffusing the suspension into a water film to form a self-assembled single-layer template.
And (4) sucking the microsphere-water-ethanol suspension C, injecting the suspension C along the edge of the substrate A, and automatically diffusing the suspension C into the water film B as shown in (C) of figure 8 to form a self-assembled monolayer template D as shown in (D) of figure 8.
The volume L (in. Mu.L) of the microsphere-water-ethanol suspension C injected into the water film B determines the mass of the monolayer template D formed, and the volume thereof is in the range of (0.04-0.1) S, preferably 0.08S.
The microsphere-water-ethanol suspension C adopted is a mixture of monodisperse polystyrene microspheres, deionized water and ethanol. Wherein the diameter of the polystyrene microspheres determines the diameter of the formed ball pits 201, the diameter is in the range of 0.5-10 μm, the mass fraction of the polystyrene microspheres is in the range of 0.5-2wt%, preferably 1.25wt%, and the ratio of deionized water and ethanol is 0.5-2, preferably 1.
The monolayer template D formed spontaneously from the microsphere-water-ethanol suspension C must be made up of a monolayer of polystyrene microspheres.
And S3, obliquely inserting the metal rod below the single-layer template, taking the single-layer template out of the water surface, rotating the single-layer template for 360 degrees, uniformly attaching the single-layer template to the surface of the metal rod, and drying the metal rod.
And (E) obliquely inserting the metal rod E into the lower part of the single-layer template D, taking the single-layer template D out of the water surface, rotating the single-layer template D by 360 degrees to ensure that the template D is uniformly attached to the surface of the metal rod E, and then drying the metal rod E, as shown in fig. 8 (E).
The size of the metal rod E can be determined according to the design requirement, and the metal rod E is made of metal simple substances or alloys such as nickel, copper and the like within the range of 10-1000 mu m, and preferably made of copper simple substances.
The angle at which the metal rod E projects into the water film (from the horizontal) is in the range 10 ° to 60 °, preferably 40 °.
And S4, performing electrochemical deposition on copper by taking the metal rod covered with the single-layer template as an anode, filling the deposited metal into the microsphere gaps of the single-layer template after the deposition time is preset, and drying after the preset height is formed.
And (f) performing electrochemical deposition of copper by using the metal rod E covered with the single-layer template D as an anode, controlling the deposition time to enable the deposited metal to fill the microsphere gaps of the single-layer template D and form a certain height, and then drying, as shown in FIG. 8.
Taking the metal bar E covered with the single-layer template D as an anode, carrying out electrochemical deposition in an electrolytic cell, wherein the adopted electrolyte is copper sulfate or nickel sulfate, and the concentration of the electrolyte is in the range of 0.05-0.5mol/L, preferably 0.1mol/L; the thickness of the deposition layer is controlled by the deposition time, the thickness of the deposition layer increases along with the increase of the deposition time, and when copper sulfate with the potential of-0.6V and 0.1mol/L is used as the electrolyte, the thickness change rule is as shown in figure 9.
And S5, soaking the metal rod, chemically removing the microspheres, drying after washing, and polishing the end face of the metal rod by using abrasive paper to obtain the tool electrode.
The metal rod E was immersed, the microspheres were chemically removed, and the microspheres were rinsed and dried, as shown in fig. 8 (g). The end face of the metal rod E was sanded to obtain a tool electrode F having a surface hydrophobic structure, as shown in fig. 8 (h).
The chemical reagent for removing the polystyrene microspheres is tetrahydrofuran, and the soaking time is 1-4h, preferably 2h. After the microspheres are removed, the glass is sequentially washed for 15min by acetone, absolute ethyl alcohol and deionized water.
And (3) grinding the end face of the metal rod E by using No. 2000 abrasive paper, removing a deposition layer on the end face to obtain the tool electrode F with a surface hydrophobic structure, and ensuring that the tool electrode F is not deformed.
The following describes a method for preparing a tool electrode with a surface hydrophobic structure according to an embodiment of the present application, including the following steps:
1) Providing a substrate A (area 100 mm) 2 ) Before use, substrate a was soaked in 10% sodium lauryl sulfate for 24h.
2) 80 μ L of deionized water was dropped on the substrate A to form a water film B having a thickness of about 1mm.
3) Sucking 8 mu L of microsphere-water-ethanol suspension C, injecting the suspension C along the edge of the substrate A, and automatically diffusing the suspension C into a water film B to form a self-assembled single-layer template D; wherein the microsphere-water-ethanol suspension C is a mixture of monodisperse polystyrene microspheres, deionized water and ethanol. Wherein the diameter of the polystyrene microsphere is 500nm, the mass fraction of the polystyrene microsphere is 1.25wt%, and the proportion of deionized water and ethanol is 1.
4) And obliquely inserting a copper rod E with the diameter of 500 mu m below the single-layer template D, taking the single-layer template D out of the water surface, rotating the single-layer template D by 360 degrees to ensure that the template D is uniformly attached to the surface of the metal rod E, and then drying the metal rod E for 1h at 60 degrees.
5) And taking the copper bar E covered with the single-layer template D as an anode, performing electrochemical deposition on copper, wherein the electrolyte is 0.1mol/L copper sulfate, the deposition time is 25s, and then drying for 2h at 60 ℃.
6) The copper rod E is soaked in tetrahydrofuran for 2h. After removing the microspheres, cleaning the microspheres for 15min by using acetone, absolute ethyl alcohol and deionized water in sequence, and then drying the microspheres for 30min at 60 ℃.
7) The end face of the metal rod E was polished with # 2000 sandpaper to obtain a tool electrode F having a surface hydrophobic structure.
It should be noted that the foregoing explanation of the embodiment of the tool electrode with a surface hydrophobic structure also applies to the method for preparing the tool electrode with a surface hydrophobic structure of this embodiment, and is not repeated herein.
According to the preparation method of the tool electrode with the surface hydrophobic structure, the tool electrode with the surface hydrophobic structure is prepared, the spherical pit microstructures distributed in an array mode are designed on the surface of the cylindrical electrode, the size and the distribution mode of the spherical pits are designed according to the surface wetting behavior basic theory, in the preparation of the microstructures, a continuous template is formed by adopting a self-assembly method, and the pit structure is formed by utilizing an electrochemical deposition process. The continuous gas film and the side wall insulation characteristics formed on the surface of the tool electrode are represented by adopting a gas film form observation mode, the feasibility and the effectiveness of the gas film and the side wall insulation characteristics in application in ECM and SACE processes are verified, a continuous and stable gas film is formed on the surface of the electrode, and the effects of side wall insulation and processing stability improvement are respectively achieved in the ECM and the SACE.
In the description of the present specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or N embodiments or examples. Moreover, various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without being mutually inconsistent.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present application, "N" means at least two, e.g., two, three, etc., unless explicitly defined otherwise.
Any process or method descriptions in flow charts or otherwise described herein may be understood as representing modules, segments, or portions of code which include one or more N executable instructions for implementing steps of a custom logic function or process, and alternate implementations are included within the scope of the preferred embodiment of the present application in which functions may be executed out of order from that shown or discussed, including substantially concurrently or in reverse order, depending on the functionality involved, as would be understood by those reasonably skilled in the art of the embodiments of the present application.
Claims (10)
1. A tool electrode having a surface hydrophobic structure,
the tool electrode consists of an electrode base body and an array ball pit microstructure arranged on the side wall surface of the electrode base body;
the electrode substrate is cylindrical and is made of copper or nickel;
the array ball pit microstructure is provided with a plurality of ball pits which are arranged in a hexagon shape, the material of the ball pits is copper or nickel, the array ball pit microstructure is used as a surface hydrophobic structure, and a resident air film which is used as a side wall insulating layer is formed on the surface of the electrode.
2. The tool electrode with surface hydrophobic structure of claim 1,
the radius of the ball pits is in the range of 0.5 μm to 10 μm.
3. The tool electrode with surface hydrophobic structure of claim 1,
the included angle between the tangent line of the ball pit inlet and the horizontal is in the range of 60-65 degrees.
4. A method for preparing a tool electrode having a hydrophobic surface structure, wherein the tool electrode is the tool electrode having a hydrophobic surface structure according to any one of claims 1 to 3, and the method comprises the steps of:
s1, dripping deionized water on a provided substrate to form a water film;
s2, sucking the microsphere-water-ethanol suspension, and injecting the suspension along the edge of the substrate to diffuse the suspension into the water film to form a self-assembled single-layer template;
s3, inserting a metal rod into the lower part of the single-layer template in an inclined mode, taking the single-layer template out of the water surface, rotating the single-layer template for 360 degrees, enabling the single-layer template to be uniformly attached to the surface of the metal rod, and drying the metal rod;
s4, performing electrochemical deposition on copper by taking the metal rod covered with the single-layer template as an anode, filling the deposited metal into the microsphere gaps of the single-layer template after the deposition time is preset, and drying after the preset height is formed;
s5, soaking the metal rod, chemically removing the microspheres, drying after washing, and polishing the end face of the metal rod by using abrasive paper to obtain the tool electrode.
5. The method for preparing a tool electrode with a hydrophobic surface structure according to claim 4, wherein in S1, the substrate is a glass sheet, the substrate is treated by soaking with a surfactant, the surfactant is sodium dodecyl sulfate, the concentration of the surfactant is in the range of 5% -20%, and the soaking time is in the range of 12h-48 h.
6. The method for preparing a tool electrode with a surface hydrophobic structure according to claim 4, wherein the volume of the deionized water added dropwise in S1 is L in units of μ L and is (0.4 μ L/mm) 2 ～1.0μL/mm 2 ) S is in the range of S, wherein S is the area of the substrate and the unit is mm 2 。
7. The method for preparing a tool electrode with a hydrophobic surface structure according to claim 4, wherein in S2, the microsphere-water-ethanol suspension is a mixture of monodisperse polystyrene microspheres, deionized water and ethanol, wherein the diameter of the polystyrene microspheres is in the range of 0.5 μm to 10 μm, the mass fraction of the polystyrene microspheres is in the range of 0.5wt% to 2wt%, and the ratio of the deionized water to the ethanol is in the range of 0.5 to 2.
8. The method for preparing a tool electrode with a hydrophobic surface structure according to claim 4, wherein the volume of the microsphere-water-ethanol suspension injected into the water film in S2 is L, μ L, at (0.04 μ L/mm) 2 ～0.1μL/mm 2 ) S is in the range of S, wherein S is the area of the substrate and the unit is mm 2 。
9. The method for preparing a tool electrode with a surface hydrophobic structure as claimed in claim 4, wherein in the S4, electrochemical deposition is performed in an electrolytic cell using a metal rod covered with a single layer template as an anode, using an electrolyte of copper sulfate or nickel sulfate at a concentration ranging from 0.05mol/L to 0.5mol/L, and a thickness of the deposited layer is controlled by a deposition time.
10. The method for preparing a tool electrode with a hydrophobic surface structure according to claim 4, wherein in the step S5, the chemical reagent for removing the polystyrene microspheres is tetrahydrofuran, and the soaking time is 1-4h.
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