CN112176375A - Preparation method of wear-resistant corrosion-resistant super-hydrophobic surface - Google Patents
Preparation method of wear-resistant corrosion-resistant super-hydrophobic surface Download PDFInfo
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- CN112176375A CN112176375A CN201910605811.7A CN201910605811A CN112176375A CN 112176375 A CN112176375 A CN 112176375A CN 201910605811 A CN201910605811 A CN 201910605811A CN 112176375 A CN112176375 A CN 112176375A
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- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 27
- 238000005260 corrosion Methods 0.000 title claims abstract description 12
- 230000007797 corrosion Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 20
- 238000004070 electrodeposition Methods 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 10
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 10
- 238000005530 etching Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- MLXDKRSDUJLNAB-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MLXDKRSDUJLNAB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 230000002209 hydrophobic effect Effects 0.000 abstract description 4
- 230000003746 surface roughness Effects 0.000 abstract description 3
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract 2
- 230000004048 modification Effects 0.000 abstract 2
- 238000005536 corrosion prevention Methods 0.000 abstract 1
- 230000005661 hydrophobic surface Effects 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000005406 washing Methods 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 6
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- PKDCQJMRWCHQOH-UHFFFAOYSA-N triethoxysilicon Chemical compound CCO[Si](OCC)OCC PKDCQJMRWCHQOH-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000001453 impedance spectrum Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
- C25D5/44—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/02—Electrolytic coating other than with metals with organic materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
- Electroplating Methods And Accessories (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a preparation method of a wear-resistant corrosion-resistant super-hydrophobic surface. Texturing the surface of a 6061 aluminum alloy substrate by adopting a laser array etching mode, and carrying out surface modification by changing the radius of a micro spiral hole generated by laser to improve the surface roughness; preparing durable super-hydrophobic surface on the aluminum alloy substrate by adopting electrochemical deposition, wherein 1H,1H,2H, 2H-perfluorodecyl triethoxysilane is used for treating SiO2The particles are subjected to surface modification, the surface free energy is reduced, meanwhile, a honeycomb structure is formed on the surface of the aluminum alloy, the hydrophobic particles can be effectively stored, and the prepared hydrophobic surface has good mechanical stability and durability, and can be applied to the fields of marine materials, underwater corrosion prevention and the like.
Description
Technical Field
The invention belongs to the field of materials, and relates to a preparation method of a wear-resistant corrosion-resistant super-hydrophobic surface.
Background
Roughness affects the behavior of droplets in thermodynamics and hydrodynamics and plays an important role in determining surface wettability, in particular in achieving surface superhydrophobicity. Increasing the surface roughness may increase the static contact angle of the surface, rendering the surface hydrophobic. Laser surface texturing is considered one of the most promising ways to increase roughness under dry conditions. The most important advantages of laser surface engineering are its flexibility, accuracy, chemical-free production, and negligible impact on bulk material properties.
Because F atom core electron and bonding electron cloud have strong binding effect, the polarizability of C-F bond is low and the C-F bond has strong electronegativity, so that the fluorine-containing polymer has the characteristics of high chemical stability, low surface free energy, excellent stain resistance and difficult wetting to various liquids. And SiO2The particles have high chemical stability and low cost, and can be used as a functional component to be introduced into the fluorine-containing polymer, so that the durability, the hardness and the like of the composite material can be improved. For improving SiO2Agglomeration of particles and SiO enhancement2Interaction between particles and fluoropolymer, generally requires the presence of SiO2The particles are surface modified.
Direct Current (DC) electrodeposition is a significant advantage for cathodic electrodeposition in industrial applications, since it is simple, cost effective, and highly efficient, and moreover, large scale manufacturing is a significant advantage regardless of workpiece geometry. The structure and performance of the electrodeposited layer can be better controlled by adjusting the surface morphology of the electrodeposited layer by adjusting electrodeposition parameters such as composition and concentration of electrolyte, temperature, electrical parameters, and processing time.
Superhydrophobic surfaces are designed to prevent corrosion under water conditions, which is a serious problem in underwater operating systems in terms of loss of efficiency and performance. Therefore, superhydrophobic coatings with good resistance to mechanical loading have important implications for obtaining long-term performance in various industrial applications. Much research has been devoted to the development of durable superhydrophobic surfaces/coatings with mechanical and corrosion barrier properties. However, the synthesis of long-lived superhydrophobic coatings that retain their excellent performance remains one of the important scientific challenges.
Disclosure of Invention
The invention aims to provide a preparation method of a wear-resistant corrosion-resistant super-hydrophobic surface, and the prepared super-hydrophobic surface has better durability and excellent corrosion resistance.
The technical solution for realizing the purpose of the invention is as follows: the preparation method of the wear-resistant corrosion-resistant super-hydrophobic surface comprises the steps of texturing the surface of a 6061 aluminum alloy substrate in a laser array etching mode to improve the surface roughness; and depositing a hydrophobic substance on the aluminum alloy substrate subjected to texturing treatment by adopting an electrochemical deposition mode to prepare a super-hydrophobic surface, wherein the method comprises the following specific steps:
step 1, carrying out laser array etching texturing treatment on the surface of a clean aluminum alloy sheet base material to prepare a circular groove array, wherein the center-to-center distance of the circular grooves is 100 microns, and the laser array etching setting parameters are as follows: the diameter of a laser spot is 20 mm, the laser power is 100Hz, the processing times are 15-30 times, and the processing frequency is 20-30 Hz;
and 3, putting the two aluminum alloy sheets subjected to texturing treatment into deposition solution as a cathode and an anode respectively, and performing electrochemical deposition treatment.
Further, in step 1, the clean aluminum alloy sheet substrate passes through 180#, 400 # s#、600 #、800#And (4) polishing by using abrasive paper step by step to remove a surface rust layer and oxidation, ultrasonically cleaning, and drying.
Further, in step 1, the size of the aluminum alloy sheet base material was 1 cm x1 cm x2 mm.
Further, in step 2, SiO2The weight percentage of the nano-particle dispersion liquid is 2-5%, 1H,1H,2H, 2H-perfluorodecyl triethoxysilane (C)16H19F17O3Si) is 3 to 7 percent.
Further, in step 3, the distance between the electrodes is 4 cm, and a pulse direct current power supply is adopted.
Further, in step 3, electrochemical deposition treatment is performed by a constant current method.
Compared with the prior art, the invention has the following remarkable advantages: 1) the surface of the aluminum alloy substrate is textured in a laser array etching mode, and a groove texture is formed on the surface of the aluminum alloy, so that hydrophobic particles can be effectively stored, and the wear resistance and durability are remarkably improved; 2) The electrochemical deposition mode is adopted, so that the method is simple, controllable and high in efficiency.
Drawings
Fig. 1 is a graph of the three-dimensional topography and static water contact angle test results of the laser-textured substrate surface obtained by texturing in example 1 and the superhydrophobic surface prepared by electrochemical deposition at different times.
FIG. 2 is a zeta potential polarization curve of the superhydrophobic surface prepared under different deposition times, the textured substrate surface, and the aluminum alloy substrate surface of example 1.
FIG. 3 shows electrochemical impedance spectra of the superhydrophobic surface prepared in the aluminum alloy substrate surface, the textured substrate surface and different deposition times of example 2, and the electrochemical impedance spectra of the superhydrophobic surface prepared by soaking in 3.5% NaCl solution for 30min and 60 min.
FIG. 4 is a graph showing the wear test and the relationship between the static water contact angle and the wear length of the wear and corrosion resistant superhydrophobic surface of example 2.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Example 1
(1) Passing an aluminum alloy substrate through 400#、600#、800#And (3) polishing by using abrasive paper step by step to remove a surface rust layer and an oxide layer, placing the polished abrasive paper in a beaker, adding deionized water for ultrasonic washing, washing by using absolute ethyl alcohol, and drying.
(2) The clean substrate is placed on a laser instrument, the substrate is etched by changing the laser pulse width and the processing frequency, laser surface texture is carried out on the surface of the aluminum alloy by Nd: YAG pulse laser with the wavelength of 1064nm, the pulse energy of 30 mJ/pulse, the height of 180mm and the laser frequency of 100Hz, the center distance of a circular groove obtained after treatment is 100 mu m, the diameter of a laser spot is 20 mm, the laser power is 100Hz, the processing frequency is 20 times, and the processing frequency is 20 Hz.
(3) And (3) placing the textured substrate in a beaker, adding deionized water, ultrasonically washing with water, washing with absolute ethyl alcohol, and drying.
(4) The electrodeposition liquid is SiO2And 1H,1H,2H, 2H-perfluorodecyl triethoxy silicon (C)16H19F17O3Si) by first 0.3g of SiO in ethanol2 Dissolving the powder in 35 ml of absolute ethyl alcohol, placing the solution on a magnetic stirrer to be fully stirred uniformly, then dropwise adding 1.5 ml of 1H,1H,2H, 2H-perfluorodecyl triethoxy silicon, and continuously stirring for 2.5 hours until uniform mixed liquid is formed.
(5) Putting the two cleaned alloy sheets as a cathode and an anode into the deposition solution, wherein the distance between the two electrodes is 4 cm, a pulse direct current power supply and a constant current are adopted, the current is adjusted, and then the power supply is switched on. And fixing the current change time by adopting a controlled variable method, taking out the sample, and drying at normal temperature. As shown in FIG. 1, the deposition time of the laser-textured surface is 5min, 10min and 15min (abbreviated as SHS-5, SHS-10 and SHS-15) respectively.
(6) Samples SHS-5, SHS-10, SHS-15 were immersed in 3.5% NaCl solution and measured to obtain zeta potential polarization curves, as shown in FIG. 2, in which SHS-5 and SHS-10 (5.747X 10)-6 A cm-2、3.813 x10-6 A cm-2) Value ratio of (1.226X 10) to substrate surface-5 A cm-2) By 1 order of magnitude. It follows that the prepared superhydrophobic surface is effective and has a long-term potential to improve the corrosion resistance of aluminum substrates.
(7) The Electrochemical Impedance Spectroscopy (EIS) was measured by immersing the sample SHS-5 in 3.5% NaCl solution for the deposition time.
(8) Dragging the prepared superhydrophobic surface at 600 kPa#The SiC sandpaper moves in one direction. The superhydrophobic surface was evaluated for static water contact angle change.
Example 2
(1) Passing an aluminum alloy substrate through 400#、600#、800#Polishing with abrasive paper step by step to remove rust layer and oxide layer on the surface, placing in a beaker, adding deionized water, ultrasonically washing, and washing with anhydrous ethanolAnd (5) drying.
(2) The clean base material is placed on a laser instrument, the base material is etched by changing the laser pulse width and the processing frequency, laser surface texture is carried out on the surface of the aluminum alloy by Nd: YAG pulse laser with the wavelength of 1064nm, the pulse energy of 30 mJ/pulse, the height of 180mm and the laser frequency of 100Hz, the groove center distance is 100 mu m, the laser spot diameter is 20 mm, the laser power is 100Hz, the processing frequency is 20 times, and the processing frequency is 20 Hz. And (3) placing the textured substrate in a beaker, adding deionized water, ultrasonically washing with water, washing with absolute ethyl alcohol, and drying.
(3) The electrodeposition liquid is SiO2And 1H,1H,2H, 2H-perfluorodecyl triethoxy silicon (C)16H19F17O3Si) by first 0.4g of SiO in ethanol2 The powder is dissolved in 40 ml of absolute ethyl alcohol, placed on a magnetic stirrer and fully stirred for 30 minutes, then 1.5 ml of 1H,1H,2H, 2H-perfluorodecyl triethoxy silicon is added dropwise, and stirring is continued for 2.5 hours until uniform mixed liquid is formed.
(4) Putting the two cleaned alloy sheets as a cathode and an anode into the deposition solution, wherein the distance between the two electrodes is 4 cm, a pulse direct current power supply and a constant current are adopted, the current is adjusted, and then the power supply is switched on. And fixing the current change time by adopting a controlled variable method, taking out the sample, and drying at normal temperature.
(5) And (3) soaking the aluminum alloy sheet, the laser-textured substrate and the sample with the deposition time of 5min, 10min and 15min in 3.5% NaCl solution respectively to obtain the potentiodynamic polarization curve.
(6) The Electrochemical Impedance Spectroscopy (EIS) was measured by immersing the sample with a deposition time of 5min in a 3.5% NaCl solution, as shown in fig. 3, wherein the immersion times of 30min and 60min are respectively designated as SHS-5-30min and SHS-5-60min, and the EIS diagrams of the substrate surface and the superhydrophobic surface in a 3.5wt% NaCl solution and the fitting results thereof are shown. It is clear that the capacitive arc diameter of the superhydrophobic surface is much higher than the substrate surface.
(7) Dragging the prepared superhydrophobic surface at 600 kPa#The SiC sandpaper moves in one direction. The superhydrophobic surface was evaluated for static water contact angle change. As shown in fig. 4. MillAfter 600mm cutting, the CA of the resulting surface remains above 150 deg.. But after 700mm wear, surface CA drops to 142.6 ° ± 4.8 °. Indicating that the prepared superhydrophobic surface exhibits good mechanical durability to some extent.
Claims (6)
1. The preparation method of the wear-resistant corrosion-resistant super-hydrophobic surface is characterized by comprising the following specific steps of:
step 1, carrying out laser array etching texturing treatment on the surface of a clean aluminum alloy sheet base material to prepare a circular groove array, wherein the center-to-center distance of the circular grooves is 100 microns, and the laser array etching setting parameters are as follows: the diameter of a laser spot is 20 mm, the laser power is 100Hz, the processing times are 15-30 times, and the processing frequency is 20-30 Hz;
step 2, preparing electrochemical deposition liquid, and mixing SiO2Dispersing the particles in absolute ethyl alcohol, uniformly mixing the particles under magnetic stirring at normal temperature, dropwise adding 1H,1H,2H, 2H-perfluorodecyl triethoxysilane, and stirring for more than 2.5 hours;
and 3, putting the two aluminum alloy sheets subjected to texturing treatment into deposition solution as a cathode and an anode respectively, and performing electrochemical deposition treatment.
2. The method of claim 1, wherein in step 1, the clean aluminum alloy sheet substrate is passed through 180#, 400 # s#、600 #、800#And (4) polishing by using abrasive paper step by step to remove a surface rust layer and oxidation, ultrasonically cleaning, and drying.
3. The method of claim 1, wherein the aluminum alloy sheet substrate in step 1 has dimensions of 1 cm x1 cm x2 mm.
4. The method of claim 1, wherein in step 2, SiO2The mass fraction of the nano-particle dispersion liquid is 2-5%, and the mass fraction of 1H,1H,2H, 2H-perfluorodecyl triethoxysilane is 3-7%.
5. The method of claim 1, wherein in step 3, the electrode spacing is 4 cm and a pulsed dc power supply is used.
6. The method of claim 1, wherein in step 3, the electrochemical deposition process is performed using a constant current method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114737230A (en) * | 2022-05-09 | 2022-07-12 | 江苏大学 | Method and device for preparing functional film with cross-scale micro-nano structure by laser-enhanced electrochemical deposition |
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| CN114737230A (en) * | 2022-05-09 | 2022-07-12 | 江苏大学 | Method and device for preparing functional film with cross-scale micro-nano structure by laser-enhanced electrochemical deposition |
| CN114737230B (en) * | 2022-05-09 | 2024-03-19 | 江苏大学 | Method and device for preparing functional film with trans-scale micro-nano structure by laser enhanced electrochemical deposition |
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