CN109249137A - A kind of method of laser and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali - Google Patents
A kind of method of laser and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali Download PDFInfo
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- CN109249137A CN109249137A CN201811135348.6A CN201811135348A CN109249137A CN 109249137 A CN109249137 A CN 109249137A CN 201811135348 A CN201811135348 A CN 201811135348A CN 109249137 A CN109249137 A CN 109249137A
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- 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
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- 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
- B23K26/361—Removing material for deburring or mechanical trimming
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
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Abstract
Present invention relates particularly to a kind of methods on the compound etching super-hydrophobic aluminum alloy surface of laser and aqueous slkali, the described method comprises the following steps: (1) being cleaned and dried aluminum alloy surface, obtain clean aluminium alloy；(2) micro-structure is etched in clean aluminum alloy surface with infrared laser marking machine, obtains laser ablation aluminium alloy；(3) laser ablation aluminium alloy is subjected to cleaning, drying, obtains clean laser ablation aluminium alloy；(4) the laser ablation aluminum alloy surface for using etching alkaline solution cleaning, obtains composite construction aluminium alloy；(5) composite construction aluminium alloy is subjected to cleaning, drying, obtains clean composite construction aluminium alloy；(6) clean composite construction aluminium alloy is immersed constant temperature in stearic acid ethanol solution to modify, then cleaning, drying, obtains superhydrophobic surface of aluminum alloy.The present invention overcomes the uncontrollable defect with hydrophobic performance difference of existing chemical etching surface quality, the surface micro-structure quality and stability of preparation are good.
Description
Technical field
The invention belongs to Metal Substrate process for modifying surface fields, and in particular to a kind of laser and the compound etching of aqueous slkali are super thin
The method of water aluminum alloy surface.
Background technique
1060 aluminium alloys are widely used in daily life, have high plasticity, corrosion resistance, electric conductivity and thermal conductivity etc.
Advantage is widely used in the fields such as chemical industry instrument, kitchen tools, clock face and disk and facade decoration.Due to aluminium alloy
Itself has hydrophily, so that water stain be easily adhered to alloy product surface, clean surface and corrosion resistance with pollutant
It is lowered.Therefore, preparation super-hydrophobic aluminum alloy surface, which improves its automatically cleaning and corrosion resistance, is particularly important.
In nature, phenomena such as rolling the lotus leaf of water droplet, the ephydrid for swimming in the water surface, the cicada's wings for condensing out dewdrop etc.,
A kind of wellability that body surface is special is presented to us.Studies have shown that when the water contact angle of matrix surface is greater than 150 °, rolling
When dynamic angle is less than 10 °, which has ultra-hydrophobicity.Pass through structured surface micro-structure and modification low-surface energy substance, people
Can prepare the surface with ultra-hydrophobicity.Super hydrophobic surface has the advantages that many, in automatically cleaning, anticorrosion, resistance to
Friction, anti-frost, sliding drag reduction etc. have huge application value.For example, being prepared on kitchen, sanitary ware super-hydrophobic
Surface, it is possible to reduce the use of water resource and detergent, energy conservation and environmental protection；In chemical industry instrument surface structure micro-structure, it can be increased
Corrosion resistance effectively improves its service life；Super hydrophobic surface is prepared in architectural appearance combination with decorative surfaces, it can be made obtained from clear
Clean performance reduces cleaning cost and the pollution to environment.
Currently, the method for preparing super hydrophobic surface for being suitable for metal base is mainly chemical etching method, LBL self-assembly
Method, hydro-thermal method, laser ablation method etc..The disadvantages such as laser ablation method has production cost higher, and production efficiency is low；Chemical etching method
It is uncontrollable with surface quality, the disadvantages of production technology is complicated.Use the method for infrared laser and the compound etching of aqueous slkali can be with
Overcome laser ablation low efficiency and at high cost and chemical etching process complexity and the uncontrollable disadvantage of surface quality, obtains high contact
The super hydrophobic surface at angle.
Such as application No. is 201410667574.4 patents to disclose a kind of method for constructing high stable super hydrophobic surface,
Aluminium alloy is first put into alkaline etching in NaOH solution, places into phosphoric acid solution and is electrolysed, is then placed in ammonium hydroxide and corrodes, finally by
Dressing agent prepares super hydrophobic surface after surface modification.Disclosing one kind application No. is the patent of 201710311284.X need not repair
The preparation method on the anti-icing surface of bionic super-hydrophobic aluminium alloy of decorations is successively etched using laser and copper chloride solution, using true
The annealing of empty drying box prepares 150 ° of contact angle or so of super hydrophobic surface.Application No. is 201510281710.0
Patent discloses a kind of method for preparing aluminium alloy super-hydrophobic automatic cleaning surface using ultra-short pulse laser, is swashed using ultrashort pulse
Light device etches micro-structure in aluminum alloy surface, places into drying in thermostatic drying chamber, prepares super-hydrophobic automatic cleaning surface.It is above-mentioned
Several method can prepare super hydrophobic surface, but there is also some problems, such as complex process, severe reaction conditions, costs
It is too high, production efficiency is low etc..Therefore, simple process and low cost, the method for preparing super hydrophobic surface of high production efficiency are searched out
It is particularly important.
Summary of the invention
Invention broadly provides a kind of methods on the compound etching super-hydrophobic aluminum alloy surface of laser and aqueous slkali, overcome
The uncontrollable defect with hydrophobic performance difference of existing chemical etching surface quality.Its technical solution is as follows:
A kind of method of laser and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, comprising the following steps:
(1) aluminum alloy surface is cleaned and dried, obtains clean aluminium alloy；
(2) micro-structure is etched in clean aluminum alloy surface with infrared laser marking machine, obtains laser ablation aluminium alloy；
(3) laser ablation aluminium alloy is subjected to cleaning, drying, obtains clean laser ablation aluminium alloy；
(4) the laser ablation aluminum alloy surface for using etching alkaline solution cleaning, obtains composite construction aluminium alloy；
(5) composite construction aluminium alloy is subjected to cleaning, drying, obtains clean composite construction aluminium alloy；
(6) clean composite construction aluminium alloy is immersed constant temperature in stearic acid ethanol solution to modify, then cleaning is dried
It is dry, obtain superhydrophobic surface of aluminum alloy.
Preferably, aluminum alloy surface is cleaned by ultrasonic respectively using dehydrated alcohol and distilled water in step (1), supersonic frequency
For 36kHz, cleaning temperature is 45-70 DEG C, and single scavenging period is 4-10min, is dried using the constant temperature of 115-145 DEG C of operating condition
Case 8-30min dry to aluminum alloy surface.
Preferably, etching condition is laser frequency 20kHz in step (2), laser power 30W, and optical maser wavelength is
1064nm。
Preferably, etching technics scanning speed is 100mm s in step (2)-1, sweep span is 200 μm.
Preferably, aluminium alloy is cleaned by ultrasonic respectively using dehydrated alcohol and distilled water in step (3) and step (5).
Preferably, aqueous slkali is sodium hydroxide solution in step (4), and the concentration of aqueous slkali is 0.3-0.5mol/L, etching
Time is 2.5-6.5min.
Preferably, the concentration of stearic acid ethanol solution is 0.1-0.15mol/L in step (6), and the modification time is 2-
3h, the temperature of constant temperature modification are 55-65 DEG C.
A kind of super-hydrophobic aluminum alloy surface, is prepared by the above method.Aluminium alloy model used in the present invention
1060。
Using the above scheme, the invention has the following advantages that
(1) it is firmly combined, is modified with matrix in the micro-structure that aluminum alloy surface etches using infrared laser and aqueous slkali
Material is not easily to fall off with aluminum alloy surface ining conjunction with by hydroxyl, therefore the surface of preparation is with stablizing permanent ultra-hydrophobicity,
It is not easy to wear；
(2) the infrared laser equipment cost that this method uses is not high, and chemical reagent is not also expensive；Processing a collection of sample only needs
4-5h can be completed, and batch more mass production efficiency is higher；Laser can carry out at room temperature with etching alkaline solution, be not required to vacuum etc.
Harsh processing environment；
(3) by adjusting technological parameter, the micro-structure surface of the channel form of rule, and the average contact angle on surface can be obtained
Greater than 160 °, it can reach 172.18 °；
(4) water droplet is dropped in sample surfaces meeting fast scroll, can take away the pollutant on surface in the process of rolling, have
Very strong self-cleaning performance can operate with the automatically cleaning of kitchen tools and horological instruments.
Detailed description of the invention
Fig. 1 is the compound etching super-hydrophobic automatic cleaning aluminum alloy surface micro-structure diagram of embodiment 1；
Fig. 2 is the compound etching super-hydrophobic automatic cleaning aluminum alloy surface contact angle schematic diagram of embodiment 1；
Fig. 3 is the automatically cleaning lab diagram of the compound etching super-hydrophobic automatic cleaning aluminum alloy surface of embodiment 1；
Fig. 4 is the compound etching super-hydrophobic automatic cleaning aluminum alloy surface micro-structure diagram of embodiment 2；
Fig. 5 is the compound etching super-hydrophobic automatic cleaning aluminum alloy surface contact angle schematic diagram of embodiment 2；
Fig. 6 is 1 laser ablation super-hydrophobic aluminum alloy surface microstructure figure of comparative example；
Fig. 7 is 1 laser ablation super-hydrophobic aluminum alloy surface contact angle schematic diagram of comparative example；
Fig. 8 is the automatically cleaning lab diagram on 1 laser ablation super-hydrophobic aluminum alloy surface of comparative example.
Fig. 9 is the automatically cleaning lab diagram of unprocessed aluminum alloy surface.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
The method of the compound etching super-hydrophobic automatic cleaning aluminum alloy surface of the infrared laser and aqueous slkali of the present embodiment, including such as
Lower step:
(1) pre-process: by 1060 aluminum alloy sample of 20mm × 20mm × 2mm successively use dehydrated alcohol and distilled water into
Row ultrasonic cleaning, cleaning temperature are 60 DEG C, and single cleans 4min, and the drying condition is to do in 120 DEG C of constant temperature oven
Dry 15min obtains pre-treating aluminium alloy；
(2) pre-treating aluminium alloy surface obtained by step (1) laser ablation: is etched into micro- knot with infrared laser marking machine
Structure, the technological parameter of laser ablation are as follows: laser power 30w, laser frequency 20kHz, optical maser wavelength 1064nm, scanning speed
Degree is 100mm s-1, sweep span be 200 μm, etch raster-like micro-structure, obtain laser ablation aluminium alloy；
(3) alkaline etching pre-treatment: successively use dehydrated alcohol and distilled water ultrasound clear etching aluminium alloy obtained by step (2)
It washes, 55 DEG C of temperature, frequency 36kHz, scavenging period 8min, dry 10min, obtains clean in 115 DEG C of constant temperature oven
Laser ablation aluminium alloy；
(4) etching alkaline solution: laser ablation aluminium alloy clean obtained by step (3) is etched with NaOH solution, NaOH is molten
The concentration of liquid is 0.3mol/L, etch period 6.5min, obtains compound etching aluminium alloy.
(5) it modifies pre-treatment: compound etching aluminium alloy obtained by step (4) is successively used into dehydrated alcohol and distilled water ultrasound
Cleaning, drying, ultrasonic cleaning condition are temperature 60 C, and frequency 36kHz, scavenging period 10min are dried in 120 DEG C of constant temperature
Dry 15min, obtains clean compound etching aluminium alloy in case；
(6) surface modification: compound etching aluminium alloy clean obtained by step (5) is immersed in stearic acid ethanol solution
Constant temperature modification, cleaning, drying, the concentration of dressing agent stearic acid ethanol solution are 0.1mol/L, and the modification time is 2h, constant temperature
The temperature of modification is 60 DEG C, and ultrasonic cleaning condition is that cleaning agent is distilled water, and 55 DEG C of temperature, frequency 36kHz, scavenging period is
4min, drying condition are 30min dry in 130 DEG C of constant temperature ovens to get superhydrophobic surface of aluminum alloy.
The compound etching super-hydrophobic automatic cleaning aluminum alloy surface micro-structure diagram of the present embodiment is as shown in Figure 1, surface is in micro-
Meter level grating coarse structure.The compound etching super-hydrophobic automatic cleaning aluminum alloy surface contact angle of this example is as shown in Fig. 2, water contacts
Angle is 172.18 °.The automatically cleaning result of aluminum alloy surface is as shown in Figure 3.
Embodiment 2
The method of the compound etching super-hydrophobic automatic cleaning aluminum alloy surface of the infrared laser and aqueous slkali of the present embodiment, including such as
Lower step:
(1) pre-process: by 1060 aluminum alloy sample of 20mm × 20mm × 2mm successively use dehydrated alcohol and distilled water into
Row ultrasonic cleaning, cleaning temperature are 70 DEG C, and single cleans 10min, and the drying condition is to do in 145 DEG C of constant temperature oven
Dry 30min obtains pre-treating aluminium alloy；
(2) pre-treating aluminium alloy surface obtained by step (1) laser ablation: is etched into micro- knot with infrared laser marking machine
Structure, the technological parameter of laser ablation are as follows: laser power 30w, laser frequency 20kHz, optical maser wavelength 1064nm, scanning speed
Degree is 100mm s-1, sweep span be 200 μm, etch raster-like micro-structure, obtain laser ablation aluminium alloy；
(3) alkaline etching pre-treatment: successively use dehydrated alcohol and distilled water ultrasound clear etching aluminium alloy obtained by step (2)
It washes, 60 DEG C of cleaning solution temperature, supersonic frequency 36kHz, scavenging period 8min, it is dry in 120 DEG C of constant temperature oven
10min obtains clean laser ablation aluminium alloy；
(4) etching alkaline solution: laser ablation aluminium alloy clean obtained by step (3) is etched with NaOH solution, NaOH is molten
The concentration of liquid is 0.5mol/L, etch period 3min, obtains compound etching aluminium alloy；
(5) it modifies pre-treatment: compound etching aluminium alloy obtained by step (4) is successively used into dehydrated alcohol and distilled water ultrasound
Cleaning, drying, ultrasonic cleaning condition are 55 DEG C of temperature, frequency 36kHz, scavenging period 10min, are dried in 130 DEG C of constant temperature
Dry 15min, obtains clean compound etching aluminium alloy in case；
(6) surface modification: compound etching aluminium alloy clean obtained by step (5) is immersed in stearic acid ethanol solution
Constant temperature modification, cleaning, drying, the concentration of dressing agent stearic acid ethanol solution are 0.15mol/L, and the modification time is 2.5h,
The temperature of constant temperature modification is 65 DEG C, and ultrasonic cleaning condition is that cleaning agent is distilled water, 55 DEG C of temperature, frequency 36kHz, when cleaning
Between be 4min, drying condition be in 130 DEG C of constant temperature ovens dry 40min to get superhydrophobic surface of aluminum alloy.
The compound etching super-hydrophobic automatic cleaning aluminum alloy surface micro-structure diagram of the present embodiment is as shown in figure 4, surface is in micro-
Meter level grating coarse structure.The compound etching super-hydrophobic automatic cleaning aluminum alloy surface contact angle of this example is as shown in figure 5, water contacts
Angle is 169.31 °.
Super hydrophobic surface regular appearance prepared in the above embodiments, water contact angle are respectively 172.18 ° and 169.31 °, are put down
Equal contact angle is higher than 160 °.
Comparative example 1
The comparative example the difference from embodiment 1 is that, lack step (3) and step (4).The compound etching of the comparative example is super
Hydrophobic automatically cleaning aluminum alloy surface micro-structure diagram is as shown in fig. 6, surface is in micron order grating coarse structure.Compound etching is super thin
Water automatically cleaning aluminum alloy surface contact angle is as shown in fig. 7, water contact angle is 156.42 °.Compound etching super-hydrophobic automatic cleaning aluminium closes
Gold surface self-cleaning effect is as shown in Figure 8.
The aluminum alloy surface prepared by comparing embodiment and comparative example, it is known that the surface of embodiment preparation is than comparative example system
High 15 ° of standby surface contact angle or more, there is good ultra-hydrophobicity.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (8)
1. a kind of method of laser and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, it is characterised in that: the following steps are included:
(1) aluminum alloy surface is cleaned and dried, obtains clean aluminium alloy；
(2) micro-structure is etched in clean aluminum alloy surface with infrared laser marking machine, obtains laser ablation aluminium alloy；
(3) laser ablation aluminium alloy is subjected to cleaning, drying, obtains clean laser ablation aluminium alloy；
(4) the laser ablation aluminum alloy surface for using etching alkaline solution cleaning, obtains composite construction aluminium alloy；
(5) composite construction aluminium alloy is subjected to cleaning, drying, obtains clean composite construction aluminium alloy；
(6) clean composite construction aluminium alloy is immersed constant temperature in stearic acid ethanol solution to modify, then cleaning, drying, obtains
Superhydrophobic surface of aluminum alloy.
2. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: aluminum alloy surface is cleaned by ultrasonic respectively using dehydrated alcohol and distilled water in step (1), supersonic frequency 36kHz, cleaning
Temperature is 45-70 DEG C, and single scavenging period is 4-10min, using the constant temperature oven of 115-145 DEG C of operating condition to aluminium alloy table
Dry 8-30min in face.
3. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: etching condition is in step (2), laser frequency 20kHz, laser power 30W, optical maser wavelength 1064nm.
4. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: etching technics scanning speed is 100mms in step (2)-1, sweep span is 200 μm.
5. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: aluminium alloy is cleaned by ultrasonic respectively using dehydrated alcohol and distilled water in step (3) and step (5).
6. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: aqueous slkali is sodium hydroxide solution in step (4), and the concentration of aqueous slkali is 0.3-0.5mol/L, etch period 2.5-
6.5min。
7. the method for laser according to claim 1 and the compound etching super-hydrophobic aluminum alloy surface of aqueous slkali, feature exist
In: the concentration of stearic acid ethanol solution is 0.1-0.15mol/L in step (6), and the modification time is 2-3h, constant temperature modification
Temperature is 55-65 DEG C.
8. a kind of super-hydrophobic aluminum alloy surface is prepared by the described in any item methods of claim 1-7.
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| CN109865949A (en) * | 2019-04-04 | 2019-06-11 | 刘珍 | A kind of aluminum alloy surface hydrophobic treatment technique |
| CN110744200A (en) * | 2019-11-08 | 2020-02-04 | 太原理工大学 | Method for improving surface corrosion resistance of austenitic stainless steel |
| CN112495451A (en) * | 2020-11-24 | 2021-03-16 | 大连理工大学 | Method for manufacturing solid catalyst by using laser processing technology |
| CN113564596A (en) * | 2021-09-26 | 2021-10-29 | 山东裕航特种合金装备有限公司 | Aluminum alloy surface treatment process with good hydrophobic and underwater oleophobic properties |
| CN113667969A (en) * | 2021-08-18 | 2021-11-19 | 南京信息工程大学 | Composite method for regulating and controlling metal surface wettability |
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