CN111318053A - Super-hydrophobic aluminum alloy filter screen and preparation method and application thereof - Google Patents
Super-hydrophobic aluminum alloy filter screen and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a super-hydrophobic aluminum alloy filter screen and a preparation method and application thereof. According to the invention, firstly, focused femtosecond laser is adopted to etch mutually parallel seams on the back of the aluminum alloy in the air to form a seam array, then a nano mastoid structure with controllable density is induced on the front of the aluminum alloy through the focused femtosecond laser with the assistance of sucrose solution, and then polydimethylsiloxane is adopted to treat the front of the aluminum alloy to change the front of the aluminum alloy into super-hydrophobicity, so that the super-hydrophobic aluminum alloy filter screen is prepared, thereby not only solving the problem that the oil-water separation effect is poor due to easy oxidation of the surface of the aluminum alloy, but also realizing the purposes of modifying the surface of the aluminum alloy in a super-hydrophobic manner and underwater in a super-oleophilic.
Description
Technical Field
The invention belongs to the field of comprehensive intersection of integration of light, computers and materials, and relates to a novel material with a wettability-bionic micro-nano structure, a preparation method and application thereof, in particular to a super-hydrophobic aluminum alloy filter screen, and a preparation method and application thereof.
Background
The material with the nano structure on the surface can be widely applied to production and life, for example, silicon with the nano cone-shaped structure on the surface can serve as an antibacterial material in medicine, and metal with the nano protrusion structure on the surface can be applied to water mist collection, frost prevention, freeze prevention, oil-water separation and the like.
The most famous super-hydrophobic surface in nature is the lotus leaf and rose petal surface, a large number of micron-scale mastoid structures are randomly distributed on the rose petal surface, the micron-scale mastoid structures are covered with nanometer-scale fold structures, and a large number of micro-nano structures with low surface energy can store air to form an air cushion, so that super-hydrophobicity is realized. The wettability of the material is determined by the micro-nano structure and the surface free energy of the surface of the material, a special rough structure is induced on the surface of the material through femtosecond laser, and the conversion from the hydrophilicity of the material to the super-hydrophobicity can be realized after the modification treatment with low surface energy.
Since the thermal conductivity of the liquid is higher than that of air, the laser will cool more easily when ablating material in the liquid, thereby reducing the heat affected zone and residual thermal damage, while thermal convection and bubble movement will remove debris and thus a cleaner material surface can be achieved.
With the development of industrial society, the ecological environment is being seriously affected by sewage discharge, marine oil leakage, and the like. The super-hydrophobic and underwater super-oleophylic material has the advantages of high selectivity, high separation efficiency, capability of separating heavy oil and the like when being applied to oil-water separation.
The oil-water separation type based on the special wetting material comprises a filtration type and an absorption type, wherein the filtration type is an oil-water separation system driven by gravity and can be subdivided into two types of super-hydrophilicity, underwater super-oleophobicity, super-hydrophobicity and underwater super-oleophilicity. The filter membrane of the oil-water separation system generally obtains super-hydrophilic and underwater super-oleophobic properties by directly inducing a coarse structure in the air through femtosecond laser, or obtains super-hydrophobic and underwater super-oleophilic properties by modifying with fluorosilane. However, the femtosecond laser ablates metal in air, and the interference effect of the surface plasma wave and the incident laser can cause a sub-wavelength periodic fringe structure perpendicular to the polarization direction of the laser on the surface of the metal, which makes it difficult to obtain a clean special micro-nano structure. Meanwhile, the metal filter screen which realizes super-hydrophilicity and underwater super-lipophobicity after femtosecond laser treatment has the problem of easy oxidation, and the super-hydrophilicity characteristic after oxidation can be weakened to cause the oil-water separation effect to be poor. In addition, the low surface energy modification of the material is usually performed by fluorosilane, and the modification process is complex and toxic.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a super-hydrophobic aluminum alloy filter screen and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, the invention provides a preparation method of a super-hydrophobic aluminum alloy filter screen, which comprises the following steps:
(1) adopting focused femtosecond laser to etch parallel seams on the back of the aluminum alloy in the air to form a seam array;
(2) submerging the aluminum alloy treated in the step (1) in a sucrose solution, and then adopting focused femtosecond laser vertical to the front surface of the aluminum alloy to perform linear array scanning on the front surface of the aluminum alloy to induce a nano mastoid structure to obtain the treated front surface of the aluminum alloy, wherein the linear array scanning direction is vertical to the seam direction;
(3) and drying the front surface of the treated aluminum alloy, and then treating the front surface of the treated aluminum alloy by adopting Polydimethylsiloxane (PDMS) to form a polydimethylsiloxane membrane, thus obtaining the super-hydrophobic aluminum alloy filter screen. According to the preparation method, a large number of nanoscale mastoid structures are successfully induced by femtosecond laser with the assistance of a sucrose solution, the density of the mastoid structures can be adjusted by different laser pulse energies and different sucrose solution concentrations, and then a layer of nontoxic low-surface-energy modifier PDMS is covered on the surface of the mastoid through a thermal evaporation method, so that a special nano structure with controllable density is induced, the roughness of the surface of an aluminum alloy can be adjusted and further the wettability of the aluminum alloy can be adjusted, the problem that the oil-water separation effect is poor due to the fact that the surface of the aluminum alloy is easy to oxidize is solved through a nontoxic surface modification method, the purposes of surface super-hydrophobicity, super-oleophylic in air and super-oleophylic under water are finally achieved, and efficient oil-water separation is achieved.
Preferably, when the line array scanning is performed, the output center wavelength of a laser adopted by the femtosecond laser is 800nm, the pulse width is 100fs, the repetition frequency is 1kHz, the size of a focused light spot is 40 μm, the power of the femtosecond laser is 4-16mW, and the scanning interval is 20 μm.
Preferably, the mass ratio of the sucrose to the water in the sucrose solution is 10:100-55: 100.
More preferably, the mass ratio of sucrose to water in the sucrose solution is 25: 100.
When the mass ratio of the sucrose to the water in the sucrose solution is in the range of 10:100-55:100, the superhydrophobic aluminum alloy filter screen has the tendency that the contact angle of the surface of the polydimethylsiloxane membrane and the water in the air is increased and then decreased along with the increase of the concentration of the sucrose, and the contact angle reaches the maximum value when the mass ratio of the sucrose to the water is 25: 100.
Preferably, the width of the slit is 35 μm, and the slit pitch is 200-350 μm.
Preferably, the liquid level on the front face of the aluminium alloy is 8.9-9.9mm when the line array scan is performed.
Preferably, the method for treating with polydimethylsiloxane comprises the following steps: and placing the front surface of the treated aluminum alloy above a polydimethylsiloxane solution, enabling the front surface of the treated aluminum alloy to face the polydimethylsiloxane solution, heating and evaporating the polydimethylsiloxane solution, and then cooling to form a polydimethylsiloxane film on the front surface of the treated aluminum alloy, wherein the polydimethylsiloxane solution contains a curing agent. The PDMS adopted by the preparation method is non-toxic, has good chemical inertness, simple use method and low cost; different from a common soaking method, a vapor deposition method, a grafting method and the like, the PDMS heat treatment method adopted by the preparation method is simple, the modification time is short, a material with a large area can be modified, the modification efficiency is high, other special equipment is not needed, the professional requirement on operators is not high, the applicability is strong, and various materials including but not limited to silicon, ceramic and aluminum alloy can be modified.
Preferably, when the polydimethylsiloxane is adopted for treatment, the front surface of the treated aluminum alloy is 2mm above the polydimethylsiloxane solution; the heating and evaporating temperature is 100-300 ℃, and the heating and evaporating time is 60-90 min.
More preferably, the heating evaporation temperature is 300 ℃, and the heating evaporation time is 90 min.
In a second aspect, the invention provides a super-hydrophobic aluminum alloy filter screen prepared by the preparation method.
Preferably, the surface of the superhydrophobic aluminum alloy filter screen with the polydimethylsiloxane membrane has a contact angle with water of 155 degrees in air, a contact angle with oil in water of 0 degrees and a contact angle with oil in air of 0 degrees.
In a third aspect, the invention further provides an application of the super-hydrophobic aluminum alloy filter screen, and specifically relates to the application of the super-hydrophobic aluminum alloy filter screen in oil-water separation.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the density-controllable nano-scale mastoid structure is successfully induced by the femtosecond laser under the assistance of the sucrose solution, but not the common periodic stripe induced by the femtosecond laser in the air, compared with the periodic stripe induced in the air, the density of the nano-scale mastoid structure can be simply regulated and controlled by changing the mass ratio of the sucrose solution and the laser power, so that the roughness of the aluminum alloy surface is regulated and controlled to further realize the regulation of wettability, which is difficult to realize by the periodic stripe induced in the air;
(2) the invention realizes simple and nontoxic super-hydrophobic modification on the hydrophilic aluminum alloy with the micro-nano structure by a nontoxic PDMS thermal evaporation method, instead of a complicated and toxic fluorosilane modifier modification method;
(3) the super-hydrophobic aluminum alloy filter screen has high oil-water separation efficiency because a large number of nano-scale mastoid structures are covered with a layer of PDMS with low surface energy, so that air can be stored between the nano-scale mastoid structures to form an air cushion to realize super-hydrophobic transformation, and good super-hydrophobicity is a necessary condition for high-efficiency oil-water separation.
Drawings
FIG. 1 is a flow chart of a superhydrophobic aluminum alloy filter screen from preparation to application;
FIG. 2 is an SEM (scanning Electron microscope) image of the slot array structure and mastoid structure of the superhydrophobic aluminum alloy filter screen of the present invention, wherein (a) is the slot array structure and (b) is the mastoid structure;
FIG. 3 is a schematic diagram or physical diagram of the preparation and application of the superhydrophobic aluminum alloy filter screen of the present invention, wherein (a) is a schematic diagram of thermal evaporation treatment of PDMS, b is a schematic diagram of an oil-water separation device, and c is a physical diagram of the oil-water separation device.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Examples
The embodiment is an embodiment of a method for preparing a super-hydrophobic aluminum alloy filter screen, and the method comprises the following steps:
(1) respectively ultrasonically cleaning the aluminum alloy for 3-5 minutes by using acetone, ethanol and water, and then carving parallel slits on the back surface of the aluminum alloy in the air by adopting focused femtosecond laser to form a slit array (shown in figure 2(a), wherein the slit width is kept at 35 mu m, the slit interval is 200-350 mu m, the aluminum alloy thickness is 100 mu m, the output center wavelength of an adopted amplification laser (manufacturer: American Coherent company, model: Legend) is 800nm, the pulse width is 100fs, the repetition frequency is 1kHz, the femtosecond laser is focused by a lens with the focal length of 15cm, and the size of a focused light spot is about 40 mu m;
(2) immersing the aluminum alloy treated in the step (1) in a sucrose solution, and performing line array scanning on the front surface of the aluminum alloy by adopting a focused femtosecond laser perpendicular to the front surface of the aluminum alloy to induce a nano mastoid structure (specifically shown in fig. 2 (b)), so as to obtain the treated front surface of the aluminum alloy, wherein the scanning direction of the line array is perpendicular to the direction of a seam, the output center wavelength of an adopted amplification laser (manufacturer: American Coherent company, model: Legend) is 800nm, the pulse width is 100fs, the repetition frequency is 1kHz, the femtosecond laser is focused by a lens with the focal length of 15cm, the size of a focused spot is about 40 microns, the power of the femtosecond laser is 4-16mW, the scanning distance is 20 microns, the depth of the sucrose solution is 9-10mm, and the mass ratio of sucrose to water in the sucrose solution is mSucrose：mWater (W)＝10:100-55:100。
(3) Drying the front surface of the treated aluminum alloy obtained in the step (1), and then modifying by adopting a PDMS heat treatment technology, wherein the method specifically comprises the following steps: preparing a polydimethylsiloxane solution (prepared by SYLGARD184 of Dow Corning company, specifically, uniformly mixing a prepolymer (A solution) and a curing agent (B solution) according to a weight ratio of 10: 1), paving the solution on a glass flat plate, then placing the front surface of the treated aluminum alloy at a position 2mm above the surface of the polydimethylsiloxane solution, enabling the front surface of the treated aluminum alloy to face the polydimethylsiloxane solution, then placing the combination in a muffle furnace, drying at the temperature of 100 ℃ and 300 ℃ for 60-90min, cooling to room temperature, and taking out to obtain the super-hydrophobic aluminum alloy filter screen.
Effect example 1: influence of laser power
Under the premise of keeping the mass ratio of the cane sugar to the water in the cane sugar solution to be 25:100 and other conditions unchanged, the number of the nano papillae on the surface of the aluminum alloy is increased from 1.08 × 10 per square centimeter along with the increase of the laser power from 4mW to 16mW9Increased to 1.8 × 109The mass ratio of other sucrose solutions also shows the same rule that the density of mastoid increases with the increase of laser power.
Effect example 2: effect of sucrose solution concentration
In keepingUnder the premise that the laser power is 16mW and other conditions are not changed, the number of mastoids is increased from 1.22 × 10 per square centimeter as the mass ratio of the sucrose to the water in the sucrose solution is increased from 10:100 to 25:1009Increased to 1.8 × 109When the mass ratio of the sucrose to the water in the sucrose solution is increased from 25:100 to 55:100, the number of mastoids is increased from 1.8 × 10 per square centimeter9Is reduced to 1.06 × 109The same law that the density of the mastoid increases and then decreases with the increase of the mass ratio of the sucrose solution is presented under other laser powers.
The parameters for obtaining the maximum papilla density obtained by the effect examples 1 and 2 are that the mass ratio of sucrose to water in the sucrose sugar solution is 25:100 and the laser power is 16 mW;
effect example 3: effect of PDMS Heat treatment conditions
On the premise of keeping other parameters consistent, the contact angle of the aluminum alloy surface baked at 300 ℃ for 90min is obviously increased in air compared with that baked at 100 ℃ for 60min, which indicates that baking at 300 ℃ for 90min is more beneficial to evaporating PDMS to the aluminum alloy surface.
Effect example 4: performance of aluminum alloy filter screen prepared under optimal conditions
Under the optimal parameters that the laser power is 16mW, the mass ratio of the cane sugar to the water in the cane sugar solution is 25:100, and other ablation conditions are the same as the embodiment, the aluminum alloy surface with the maximum density of nano papilla is obtained, and the aluminum alloy surface is 1.8 × 10 per square centimeter9The more the mastoid density is, the more the surface is rough, the more hydrophobic the surface is after modification, under the optimal PDMS evaporation parameter, namely the parameter of baking for 90min at 300 ℃, the aluminum alloy filter screen has the super-hydrophobic characteristic, the contact angle with water in the air reaches 155 degrees, the contact angle with oil in the air is 0 degree, meanwhile, the contact angle with oil in water is also 0 degree, and the super-oleophilic property in the air and the super-oleophilic property under water are realized.
Effect example 5: oil-water separation effect
The super-hydrophobic aluminum alloy filter screen with the overall effective area of 10 × 10mm is obtained by the embodiment, the filter screen is clamped in two plastic pipes through two sealing rings, so that the filtering type oil-water separation device capable of separating heavy oil and water with a simple structure is prepared, as shown in (b) and (c) of fig. 3, the oil-water separation efficiency of the oil-water separation method is within the range of 99.57-99.65%, the water invasion pressure is within the range of 5742-6533Pa, and the oil-water separation efficiency is still within the range of 99.15-99.26% after more than 20 times of circulation use, in order to simulate the condition that the salt content of ocean is high, after water is replaced by brine with the mass fraction of 10-25 wt%, the oil-water separation efficiency is still as high as 99.45-99.54%.
The aluminum alloy filter screens with different seam intervals keep similar good performances in the aspects of oil-water separation efficiency, water intrusion pressure, reusability and environmental adaptability with different salt contents, and the only parameter with larger change in the test is the flux of oil; the oil flux increased from 5.28L-m as the slot pitch increased from 200 μm to 350 μm, with other conditions being unchanged-2·s-1Reduced to 4.08 L.m-2·s-1This indicates that the optimum slit pitch is 200 μm.
It should be finally noted that the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the super-hydrophobic aluminum alloy filter screen is characterized by comprising the following steps:
(1) adopting focused femtosecond laser to etch parallel seams on the back of the aluminum alloy in the air to form a seam array;
(2) submerging the aluminum alloy treated in the step (1) in a sucrose solution, and then adopting focused femtosecond laser vertical to the front surface of the aluminum alloy to perform linear array scanning on the front surface of the aluminum alloy to induce a nano mastoid structure to obtain the treated front surface of the aluminum alloy, wherein the linear array scanning direction is vertical to the seam direction;
(3) and drying the front surface of the treated aluminum alloy, and then treating the front surface of the treated aluminum alloy by adopting polydimethylsiloxane to form a polydimethylsiloxane membrane, thus obtaining the super-hydrophobic aluminum alloy filter screen.
2. The method of claim 1, wherein the linear array scan is performed using a femtosecond laser having an output center wavelength of 800nm, a pulse width of 100fs, a repetition frequency of 1kHz, a focused spot size of 40 μm, a femtosecond laser power of 4-16mW, and a scan pitch of 20 μm.
3. The method according to claim 1, wherein the sucrose solution contains sucrose and water at a mass ratio of 10:100 to 55: 100.
4. The method as claimed in claim 1, wherein the width of the slit is 35 μm and the pitch of the slit is 200-350 μm.
5. A method of making as claimed in claim 1 wherein the liquid level on the front face of the aluminium alloy is 8.9-9.9mm when the line array scan is performed.
6. The method of claim 1, wherein the polydimethylsiloxane is treated by: and placing the front surface of the treated aluminum alloy above a polydimethylsiloxane solution, enabling the front surface of the treated aluminum alloy to face the polydimethylsiloxane solution, heating and evaporating the polydimethylsiloxane solution, and then cooling to form a polydimethylsiloxane film on the front surface of the treated aluminum alloy, wherein the polydimethylsiloxane solution contains a curing agent.
7. The method of claim 6, wherein, when treated with polydimethylsiloxane, the treated aluminum alloy front face is 2mm above the polydimethylsiloxane solution; the heating and evaporating temperature is 100-300 ℃, and the heating and evaporating time is 60-90 min.
8. The super-hydrophobic aluminum alloy filter screen prepared by the preparation method of any one of claims 1 to 7.
9. The superhydrophobic aluminum alloy screen of claim 8, wherein the surface of the superhydrophobic aluminum alloy screen having a polydimethylsiloxane membrane has a contact angle with water of 155 ° in air, a contact angle with oil of 0 ° in water, and a contact angle with oil of 0 ° in air.
10. Use of the superhydrophobic aluminum alloy screen of claim 8 or 9 in oil-water separation.
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