CN114178795B - Preparation method of anisotropic super-hydrophobic surface of metal material - Google Patents

Preparation method of anisotropic super-hydrophobic surface of metal material Download PDF

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CN114178795B
CN114178795B CN202111543614.0A CN202111543614A CN114178795B CN 114178795 B CN114178795 B CN 114178795B CN 202111543614 A CN202111543614 A CN 202111543614A CN 114178795 B CN114178795 B CN 114178795B
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CN114178795A (en
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胡静
杨晓红
叶霞
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Changzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • 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
    • B23H11/00—Auxiliary apparatus or details, not otherwise provided for
    • 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
    • B23H7/00—Processes or apparatus applicable to both electrical discharge machining and electrochemical machining
    • B23H7/02—Wire-cutting
    • 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
    • B23H7/00—Processes or apparatus applicable to both electrical discharge machining and electrochemical machining
    • B23H7/22—Electrodes specially adapted therefor or their manufacture
    • B23H7/24—Electrode material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/08—Devices involving relative movement between laser beam and workpiece
    • B23K26/082—Scanning systems, i.e. devices involving movement of the laser beam relative to the laser head
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/36—Removing material
    • B23K26/362—Laser etching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/70—Auxiliary operations or equipment
    • B23K26/702—Auxiliary equipment

Abstract

The invention belongs to the technical field of surface modification, and particularly relates to a preparation method of an anisotropic superhydrophobic surface of a metal material. The method comprises the steps of firstly pretreating a metal surface by adopting linear cutting equipment, then preparing a periodic array structure on the metal surface by adopting a laser marking machine, and then carrying out chemical modification in stearic acid solution to obtain an anisotropic superhydrophobic surface, wherein the contact angle is more than 150 degrees. The surface has wide application prospect in micro-fluid devices.

Description

Preparation method of anisotropic super-hydrophobic surface of metal material
Technical Field
The invention belongs to the technical field of surface modification, and particularly relates to a preparation method of an anisotropic superhydrophobic surface of a metal material.
Background
Under the inspired of nature, more and more bionic surfaces are prepared, and important applications are shown in the practical fields such as self-cleaning, micro-fluidic, oil-water separation and the like. The bionic surface with anisotropy becomes a research hot spot in the bionic field due to the advantages of the bionic surface in the aspects of water collection, medicine replenishment and the like. The biological surface has an anisotropic structure, so that special performance is given to the biological surface, and the biological surface is favorable for adapting to the environment. The biological surface generally has micro-nano structure and anisotropic structure, so that the fluid has special infiltration, movement and transmission performance on the biological surface. Many grass leaf surfaces have an anisotropic thorn-like structure. When the liquid drops are condensed on the blade, the liquid drops are not easy to separate from the blade due to the effect of the thorn structure. The anisotropic micro-nano structure and the characteristics thereof can be applied to practical production and life, such as self-cleaning coating, directional transportation of liquid drops, directional micro-fluid devices and the like.
At present, many scholars have proposed research for preparing anisotropic superhydrophobic surfaces. The Chinese patent 'an anisotropic superhydrophobic surface of aluminum material and a preparation method thereof' proposes to directionally rough grind and fine grind the aluminum material by using a hard rough material, then soak the aluminum material in weak alkaline boiling water, and finally modify the aluminum material by using a low surface energy substance to obtain the anisotropic superhydrophobic surface. The preparation method has the advantages that a plurality of procedures are needed before the modification of the low surface energy, the preparation method is complex, meanwhile, the directional coarse grinding or fine grinding cannot be set in a parameterization mode, and the obtained directional structure is not easy to control.
The anisotropic microstructure has special wettability. Therefore, development of a simple, efficient, controllable and low-cost preparation method for the super-hydrophobic surface of the metal material with infiltration anisotropy is imperative.
Disclosure of Invention
The invention provides an anisotropic superhydrophobic surface of a metal material and a preparation method thereof. The preparation method of the anisotropic superhydrophobic surface of the metal material comprises the following steps:
(1) Wire cutting pretreatment: carrying out surface cutting on the metal material on linear cutting equipment;
the processing parameters of the wire cutting pretreatment are as follows: the voltage is 1-2V, the current is 0-3A, the cutting frequency is 30-45 Hz, the pulse width of the pulse power supply is 32 mu S, and the pulse width is 8 mu S.
The wire cutting pretreatment adopts molybdenum wires with the diameter of 0.18mm, the discharge gap of 0.1mm and the compensation of 0.19mm.
(2) Ultrasonic cleaning;
the ultrasonic cleaning solution is an alcohol solution, and the ultrasonic time is 30 minutes.
(3) Preparing a rectangular groove periodic array structure by a laser marking machine;
and constructing a rectangular groove periodic structure on the surface of the metal material by using an infrared nanosecond laser. The partial periodic structure is divided into A and A ⊥ The rectangular groove structure A is a groove array structure obtained by a mode that a laser scans line by line under the control of CAD program; rectangular trench structure A ⊥ Is an array structure obtained by scanning a laser column by column, and is a rectangular groove structure and A in theory ⊥ The rectangular structures are perpendicular to each other.
Comparing blank sample with electrochemical workstation, and forming a groove array structure A, A ⊥ Of rectangular constructionCorrosion resistance and results show that the groove array structures A and A ⊥ The corrosion voltage of the rectangular structure moves leftwards, the corrosion performance is obviously increased, but the corrosion performance of the A-T rectangular structure is superior to that of the groove array structure A, and the A ⊥ The wettability of the rectangular structure is superior to that of the groove array structure A, the gradient change of the wettability is realized, and the application of the microfluidic device can be realized.
(4) The low surface energy modification is performed using a stearic acid solution.
The concentration of stearic acid is 2wt%, the temperature of the water bath is 70 ℃ during modification, and the soaking time is 2h.
The anisotropic superhydrophobic surface of the metal material prepared by the method has superhydrophobicity along the direction of the groove array structure A, and the contact angle is 148.2-150.1 degrees. Along trench array structure A ⊥ In the direction, the contact angle is 155.4-158.9 degrees.
Advantageous effects
(1) The invention pretreats the surface of metal material by regulating the pulse power supply parameter of the wire cutting equipment to obtain the surface microstructure, then obtains the submicron structure by infrared laser etching, and obtains the super-hydrophobic surface structure with anisotropy by low surface energy modification.
(2) The rough structure is obtained through linear cutting pretreatment, and the laser etching shape is controllable.
Drawings
FIG. 1 is a flow chart of an experiment;
FIG. 2 is a schematic diagram of water droplet flow;
FIG. 3 is a photograph of example 1 after wire cutting pretreatment;
fig. 4 is an SEM image and contact angle after laser etching in example 1;
FIG. 5 is a graph of corrosion resistance electric polarization curves for example 1 and the blank.
Detailed Description
The preparation method of the anisotropic superhydrophobic surface of the metal material comprises the following processing steps:
wire cutting pretreatment: cutting pretreatment is carried out on the metal surface by using linear cutting equipment, and a surface roughness structure is processed;
ultrasonic cleaning: immersing the sample in an alcohol solution for ultrasonic cleaning;
preparation of a periodic array structure: performing periodic array etching on the online cutting surface by using an infrared nanosecond laser etching method to process a surface microstructure;
low surface energy modification: and the free energy of the surface of the material is reduced by using stearic acid solution for modification.
Example 1
Taking TC4 as an example, the implementation process of the preparation method of the anisotropic superhydrophobic surface of the metal material is described, and the preparation method comprises the following steps:
wire cutting pretreatment: the TC4 material is fixed on a linear cutting device, a molybdenum wire with the diameter of 0.18mm is adopted to cut along the surface of the material, the cutting path is controlled by a pre-drawn CAD graph, the cutting path is a straight line, the discharge gap Z is 0.1mm, the compensation is 0.19mm, the pulse is a rectangular pulse, the voltage is 1V, the current is 3A, and the frequency is 30Hz. After the processing is finished, the ultrasonic cleaning is carried out for 30min.
Preparing a periodic array structure: and (3) preparing a rectangular groove array structure on the surface of TC4 by using an infrared laser etching method, and processing a surface microstructure, wherein the scanning power is 24W, the scanning interval is 100 mu m, and the scanning speed is 50mm/s.
Low surface energy modification: the processed sample was placed in a 2wt% stearic acid solution at 70℃in a water bath and immersed for 2 hours.
Example 2
Wire cutting pretreatment: the TC4 material is fixed on a linear cutting device, a molybdenum wire with the diameter of 0.18mm is adopted to cut along the surface of the material, the cutting path is controlled by a pre-drawn CAD graph, the cutting path is a straight line, the discharge gap Z is 0.1mm, the compensation is 0.19mm, the pulse is a rectangular pulse, the voltage is 2V, the current is 2A, and the frequency is 40Hz. After the processing is finished, the ultrasonic cleaning is carried out for 30min.
Preparing a periodic array structure: and (3) preparing a rectangular groove array structure on the surface of TC4 by using an infrared laser etching method, and processing a surface microstructure, wherein the scanning power is 24W, the scanning interval is 100 mu m, and the scanning speed is 50mm/s.
Low surface energy modification: the processed sample was placed in a 2wt% stearic acid solution at 70℃in a water bath and immersed for 2 hours.
Example 3
Wire cutting pretreatment: the TC4 material is fixed on a linear cutting device, a molybdenum wire with the diameter of 0.18mm is adopted to cut along the surface of the material, the cutting path is controlled by a pre-drawn CAD graph, the cutting path is a straight line, the discharge gap Z is 0.1mm, the compensation is 0.19mm, the pulse is a rectangular pulse, the voltage is 1V, the current is 3A, and the frequency is 45Hz. After the processing is finished, the ultrasonic cleaning is carried out for 30min.
Preparing a periodic array structure: and (3) preparing a rectangular groove array structure on the surface of TC4 by using an infrared laser etching method, and processing a surface microstructure, wherein the scanning power is 24W, the scanning interval is 100 mu m, and the scanning speed is 50mm/s.
Low surface energy modification: the processed sample was placed in a 2wt% stearic acid solution at 70℃in a water bath and immersed for 2 hours.
Comparative example
Taking the example of TC4 as an example,
ultrasonic cleaning: carrying out ultrasonic cleaning on the sample for 30min;
preparing a periodic array structure: and (3) preparing a rectangular groove array structure on the surface of TC4 by using an infrared laser etching method, and processing a surface microstructure, wherein the scanning power is 24W, the scanning interval is 100 mu m, and the scanning speed is 50mm/s.
Low surface energy modification: the processed sample was placed in a 2wt% stearic acid solution at 70℃in a water bath and immersed for 2 hours.
The superhydrophobic surfaces prepared in examples 1-3 and the superhydrophobic surface prepared in the comparative example were subjected to contact angle measurement to obtain blank samples without any treatment, and the results are shown in table 1.
Figure BDA0003415141780000051
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Claims (1)

1. The preparation method of the anisotropic superhydrophobic surface of the metal material is characterized by comprising the following steps of:
(1) Wire cutting pretreatment: fixing TC4 material on linear cutting equipment, cutting along the surface of the material by adopting molybdenum wire with phi of 0.18mm, roughening the surface of the metal, preparing a texture structure, controlling by a pre-drawn CAD graph, wherein the cutting path is a straight line, the discharge gap Z is 0.1mm, the compensation is 0.19mm, the pulse is rectangular pulse, the voltage is 1V, the current is 3A, and the frequency is 30Hz;
(2) Ultrasonic cleaning, namely after finishing processing, ultrasonic cleaning for 30min;
(3) Preparing a periodic array structure: preparing a rectangular groove periodic array structure on the surface of TC4 by utilizing an infrared laser etching method, firstly carrying out progressive scanning to obtain a parallel groove array structure A, and secondly carrying out progressive scanning by program control to obtain a groove array structure A which is mutually perpendicular to the groove array structure A ⊥ Obtaining A ⊥ A structure; processing a surface microstructure, wherein the scanning power is 24W, the scanning interval is 100 mu m, and the scanning speed is 50mm/s;
(4) Low surface energy modification: placing the processed sample in 2wt% stearic acid solution, and soaking for 2 hours at the water bath temperature of 70 ℃;
the anisotropic superhydrophobic surface has a contact angle of 150 ° in a direction along the trench array structure a, and has a contact angle of three dimensions along the trench array structure a ⊥ The contact angle was 158.9 ° in direction.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102586771A (en) * 2012-02-14 2012-07-18 中南林业科技大学 Metallic aluminum bionic super-hydrophobic surface preparation method
CN103590023A (en) * 2013-10-25 2014-02-19 湖南工业大学 Preparation method of lotus-leaf-like surface structure superhydrophobic copper sheet
CN106757224A (en) * 2016-12-01 2017-05-31 吉林大学 A kind of preparation method with the anisotropic fine copper super hydrophobic surface of wetting
CN106733555A (en) * 2017-01-06 2017-05-31 南京航空航天大学 A kind of controllable super hydrophobic surface and its construction method for clashing into drop bounce-back direction
CN110900687A (en) * 2019-12-20 2020-03-24 湖北理工学院 Preparation method of bionic rice leaf surface lattice anisotropic super-hydrophobic surface material

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