CN109626317B - Composite structure film based on double-gradient tapered hole array and preparation method thereof - Google Patents
Composite structure film based on double-gradient tapered hole array and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite structure film based on a double-gradient tapered hole array and a preparation method thereof, relates to a composite structure film and a preparation method thereof, and aims to solve the problems that the self-driving effect of self-driven water mist collecting film water drops is not ideal, the self-driving energy source is single and the like. The invention adopts the femtosecond laser drilling technology and the low surface energy modification technology, and realizes the high-efficiency and rapid processing of the conical hole array with the morphology gradient and the surface energy gradient by adjusting the laser pulse impact parameters and the focal point space position. The structure can spontaneously change the state of the water drop to finish the self-driven transportation process from the upper surface to the lower surface. The upper surface and the lower surface of the composite-structure aluminum foil prepared by the invention respectively have super-hydrophobic and super-hydrophilic properties. Three gradient elements, roughness, surface energy and section radius, exist from top to bottom in the micropores, and the three gradients endow the liquid drops with the capability of spontaneously transferring from the upper surface to the lower surface of the aluminum foil. The invention is applied to the field of fog water treatment.
Description
Technical Field
The invention relates to a composite structure-based membrane and a preparation method thereof.
Background
With the continuous growth of population and the increasing shortage of fresh water resources, how to rapidly acquire fresh water resources becomes a difficult problem for researchers. Fresh water resources in the air can be continuously supplemented through the atmospheric circulation, and are inexhaustible fresh water resources. Inspired by the epidermal structure of some living organisms in the nature, the moisture collection from the air by utilizing the wettability of the material to water attracts attention. For example: the unique multi-stage water drop condensation-collection-transportation-absorption structure of cactus can effectively absorb water from air and transport the water to roots; the super-hydrophobic/super-hydrophilic composite wettability surface on the back of the desert beetle can enable moisture in the air to be condensed in the super-hydrophilic area and conveyed to the body through the super-hydrophobic area, and the like. The structures capable of achieving a series of fog drop collecting functions can have potential application scenes in the fields of heat transfer efficiency, liquid directional transportation and the like. One summarizes the overall process of these biological collections of misty water, and presents several functional requirements for composite structures: including hydrophobic interfaces, continuous collection and transfer, while allowing for relatively low rates of re-evaporation, etc. Among these functions, how to achieve self-driven transport of water droplets is a key challenge for the entire collection process.
In biological characteristics, self-driven directional transportation of liquid drops mainly has two forms of driving forces, wherein the liquid has a curved surface morphology structure, the tension difference (Laplace pressure difference) formed on the liquid/gas interface at two sides of the liquid/gas interface is different from the surface energy of a solid, and the formed surface energy gradient force generates a directional driving force (wettability gradient force). How to design microstructure morphology gradient and micro-area surface energy structure becomes a main difficult problem facing people. At present, people prepare periodic spindle-shaped nodes on fibers by an electrostatic spinning technology, and liquid drops can realize a one-way transportation process on the appearance gradient with gradually changed diameters; the super-hydrophilic material such as copper mesh and the super-hydrophobic material such as sponge are combined to prepare a' double-sided structure with composite wettability, the two materials in the double-sided structure have surface energy difference, so that water forms wettability gradient force between the two materials, and the water is promoted to spontaneously and directionally move from the super-hydrophobic surface to the super-hydrophilic surface.
The research on the directional water drop transportation focuses on the research of a single driving force, and no self-driven transportation device with two acting forces acting on the water drop together is reported in the published literature.
Disclosure of Invention
The invention aims to solve the problems of non-ideal self-driving effect of water drops of a self-driven water mist collecting membrane, single self-driving energy source and the like, and provides a high-efficiency self-driven composite structure membrane structure which can integrate multiple functions of condensation, collection, transfer, storage and the like of water mist.
The invention provides an aluminum foil membrane (composite structure membrane) based on a double-gradient conical hole array, which can finish a series of processes of condensation, collection, transportation, storage and the like of water drops.
The invention relates to a composite structure film based on a double-gradient conical hole array, which is an aluminum foil filmThe aluminum foil membrane is provided with a taper hole, the section of the taper hole is in an equilateral trapezoid shape, the hole radius of the taper hole is gradually increased from the upper surface to the lower surface of the aluminum foil membrane, and the upper surface of the aluminum foil membrane is provided with a low surface energy material C10H4Cl3F17Si, the lower surface material is Al2O3。
The invention relates to a preparation method of a composite structure film based on a double-gradient tapered hole array, which is carried out according to the following steps:
firstly, flatly placing an aluminum foil on a three-dimensional moving platform, firstly setting laser single pulse energy, moving a laser focus to the upper surface of the aluminum foil, setting a two-dimensional point array structure through scanning galvanometer software, and changing pulse impact times by setting focus retention time to prepare a double-sided super-hydrophilic micropore array structure;
secondly, placing the super-hydrophilic tapered hole array membrane in a modifying solution to be soaked for 24 hours, and then heating the membrane on a hot plate at the temperature of 60 ℃ for 30 minutes to obtain a double-sided super-hydrophobic membrane;
and thirdly, flatly placing the double-sided super-hydrophobic membrane on a three-dimensional moving platform, setting a laser focus at a position of 0.7mm above the upper surface, setting raster scanning at an interval of 25 microns, laser pulse energy of 75 muJ and a scanning speed of 10mm/s, and obtaining the composite structure membrane after scanning.
The invention provides a micropore array aluminum foil with surface energy gradient and morphology gradient. This structure has the following functions (as shown in fig. 3): the upper surface has a super-hydrophobic characteristic, and can condense fog drops in air in a certain humidity environment, and the liquid drops can grow slowly until the liquid drops contact the edges of the micropores. Thereafter, the droplet was transferred to the lower surface in an extremely short time (droplet 5. mu.l, pore diameter 30 μm, transfer time 0.363s) by being subjected to two kinds of driving forces. The lower surface of the membrane may be attached to a container and sealed. The rate of re-evaporation of the collected water decreases as the water droplets collected on the upper surface are transferred to the lower surface. In the self-driven transfer process of the water drops, the self-driven transfer device is subjected to two forces, namely wettability gradient force formed by liquid film tension difference and surface energy difference generated at two ends of the water drops in the conical shape, and is an improved design aiming at the unsatisfactory driving effect caused by single self-driven energy source of the liquid at present. In addition, the parameters such as the size, the interval, the morphology structure and the like of the double-gradient micropores can be adjusted through processing conditions, and meanwhile, the optimal structure can be designed according to different external environments (such as humidity and temperature). The composite structure film provides a new design idea and a new research scheme for the research of mist water collection and transportation, heat transfer efficiency improvement and the like.
The invention has the following beneficial effects:
the upper surface and the lower surface of the composite wettability aluminum foil prepared by the invention respectively have super-hydrophobic and super-hydrophilic properties. Three gradient elements, roughness, surface energy and section radius, exist from top to bottom in the micropores, and the three gradients endow the liquid drops with the capability of spontaneously transferring from the upper surface to the lower surface of the aluminum foil. The composite structure membrane with the conical hole array has unique advantages in heat transfer, fog collection and the like. In addition, the shape gradient and the surface energy gradient can be precisely tuned by adjusting the processing parameters, and an optimal liquid self-transportation structure is designed in different environments.
The composite structure membrane prepared by the invention can improve the fog collection rate by 209 percent in a saturated water vapor environment compared with a completely super-hydrophilic membrane structure. Provides a new idea and implementation scheme for the fields of future acquisition of fresh water resources, heat transfer efficiency and the like.
Drawings
FIG. 1 is an electron micrograph of the topographical structure of a film of the present invention; wherein, a is an electron microscope picture with a rough structure on the upper surface, and b is a petal-shaped structure on the lower surface; c is an equilateral trapezoid diagram of the section of the single conical hole;
FIG. 2 is a graph of the wetting characteristics of water on the upper and lower surfaces of a composite wetting membrane of the present invention;
FIG. 3 is a graph of the collection performance test of a composite wetting film; wherein the dashed box is the composite wetting film.
Detailed Description
The first embodiment is as follows: the composite structure film based on the double-gradient taper hole array of the embodiment is an aluminum foil film, and the aluminum foil film is provided with the aluminum foil filmA conical hole with an equilateral trapezoid cross section, wherein the hole radius of the conical hole is gradually increased from the upper surface to the lower surface of the aluminum foil membrane, and the upper surface of the aluminum foil membrane is provided with a low surface energy material C10H4Cl3F17Si, the lower surface material is Al2O3。
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the nano particles on the inner wall of the conical hole are gradually increased from the upper surface to the lower surface of the aluminum foil membrane, C10H4Cl3F17The Si material composition ratio gradually decreases. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the periphery of the upper surface of the conical hole is of a rough structure, and the periphery of the lower surface of the conical hole is of a petal-shaped rough structure. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the contact angle of the top end of the conical hole exceeds 150 degrees, and the contact angle of the bottom end of the conical hole is less than 10 degrees. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the water contact angle of the water drop on the upper surface of the conical hole of the composite structure film is about 155 degrees, and the water contact angle of the lower surface is less than 10 degrees. The rest is the same as the first embodiment.
The sixth specific implementation mode: the preparation method of the composite structure membrane based on the double-gradient tapered hole array is carried out according to the following steps:
a preparation method of a composite structure film based on a double-gradient tapered hole array is characterized by comprising the following steps:
firstly, an aluminum foil is flatly placed on a three-dimensional moving platform, laser single pulse energy W (150 mu J) is set firstly, a laser focus is moved to the upper surface of the aluminum foil, a two-dimensional point array structure (h is 100 mu m) is set through scanning galvanometer software, the pulse impact frequency (n is 60) is changed by setting the focus dwell time, a double-sided super-hydrophilic micropore array structure can be prepared, and the micropore interface is trapezoidal (a conical hole array).
Secondly, the super-hydrophilic conical hole array membrane is placed in a modification liquid (ethanol: C)10H4Cl3F17Si 1:100) for 24h, heated on a 60 degree hotplate for 30min, the film wetting becomes double-sided superhydrophobic.
Thirdly, the super-hydrophobic membrane is flatly placed on a three-dimensional moving platform (the large pore surface faces upwards), a laser focus is arranged at the position of 0.7mm of the upper surface, raster scanning (stripe shape) is arranged, the interval is 25 microns, the laser pulse energy is 75 muJ, the scanning speed is 10mm/s, after scanning is finished, the wettability of the scanning surface is changed into super-hydrophilic, and the reverse surface is super-hydrophobic, namely the composite structure membrane.
The composite structure membrane prepared by the embodiment has the temperature of 25 ℃ and the pressure of 1.013 × 105Introducing saturated steam under the Pa condition, wherein the interval of micropores is 100-500 mu m, the minimum diameter of the micropores is 30-100 mu m, and the effective collection area of the sample is 3 × 3cm2。
As shown in fig. 1, it can be seen from fig. 1 that the top surface of the film of the present embodiment is a rough structure, and the bottom surface thereof is a petal-shaped structure. The section of the single taper hole is in an equilateral trapezoid, and the roughness is gradually increased.
FIG. 2 shows the wetting characteristics of water on the upper and lower surfaces with composite wettability, the left graph shows that the upper surface has super-hydrophobic characteristics, and the right graph shows that the lower surface has super-hydrophilic characteristics.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: the laser single pulse energy is 60-300 muJ. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the sixth embodiment is different from the sixth embodiment in that: the two-dimensional point array structure is as follows: h is 100 μm. The rest is the same as the sixth embodiment.
The specific implementation method nine: the sixth embodiment is different from the sixth embodiment in that: the modification liquid is ethanol: c10H4Cl3F17The Si is mixed according to the volume ratio of 1: 100. The rest is the same as the sixth embodiment.
The detailed implementation mode is ten: the sixth embodiment is different from the sixth embodiment in that: the number of pulse impact is 20-100. The rest is the same as the sixth embodiment.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The preparation method of the composite structure film based on the double-gradient tapered hole array specifically comprises the following operations:
the temperature is 25 ℃, and the pressure is 1.013 × 105Pa, introducing saturated water vapor, processing the sample by adopting the following parameters that the micropore interval is 100 mu m, the minimum diameter of the micropore is 30 mu m, and the effective collection area of the sample is 3 × 3cm2And preparing the composite structure film based on the double-gradient tapered hole array.
The composite wettability collecting membrane can collect water with 4.6m L in 8min and water with 8.1m L in 15min, and the collecting speed reaches 0.068 ml/min-1·cm-2。
Example 2
The preparation method of the composite structure film based on the double-gradient tapered hole array specifically comprises the following operations:
the temperature is 25 ℃, and the pressure is 1.013 × 105Pa, introducing saturated water vapor, processing the sample by adopting the following parameters that the micropore interval is 100 mu m, the minimum diameter of the micropore is 30 mu m, and the effective collection area of the sample is 3 × 3cm2And preparing the composite structure film based on the double-gradient tapered hole array.
The composite wettability collecting membrane can collect water with 4.6m L in 8min and water with 8.1m L in 15min, and the collecting speed reaches 0.068 ml/min-1·cm-2The liquid-gas interface area was reduced by 93%.
Example 3
The preparation method of the composite structure film based on the double-gradient tapered hole array specifically comprises the following operations:
the following conditions were set: temperature 25 ℃ and pressure1.013×105Pa, introducing saturated water vapor, processing the sample by adopting the following parameters that the micropore interval is 100 mu m, the minimum diameter of the micropore is 40 mu m, and the effective collection area of the sample is 3 × 3cm2And preparing the composite structure film based on the double-gradient tapered hole array.
The composite wettability collecting membrane can collect 6.3m L water in 8min and 10.9m L water in 15min, and the collecting speed reaches 0.081ml min-1·cm-2The liquid-gas interface area is reduced by 87%.
Example 4
The preparation method of the composite structure film based on the double-gradient tapered hole array specifically comprises the following operations:
the temperature is 25 ℃, and the pressure is 1.013 × 105Pa, introducing saturated water vapor, processing the sample by adopting the following parameters that the micropore interval is 50 mu m, the minimum diameter of the micropore is 10 mu m, and the effective collection area of the sample is 3 × 3cm2And preparing the composite structure film based on the double-gradient tapered hole array.
The composite wettability collecting film can collect 3m L water in 8min and 5.4m L water in 15min, and the collecting speed reaches 0.040 ml.min-1·cm-2The liquid-gas interface area is reduced by 88%.
Example 5
The preparation method of the composite structure film based on the double-gradient tapered hole array specifically comprises the following operations:
the temperature is 25 ℃, and the pressure is 1.013 × 105Pa, introducing saturated water vapor, processing the sample by adopting the following parameters that the interval of the micropores is 500 mu m, the minimum diameter of the micropores is 100 mu m, and the effective collection area of the sample is 3 × 3cm2And preparing the composite structure film based on the double-gradient tapered hole array.
The composite wettability collecting membrane can collect water with 2.3m L in 8min and water with 4.1m L in 15min, and the collecting rate reaches 0.030 ml.min-1·cm-2The liquid-gas interface area is reduced by 88%.
Claims (7)
1. Composite based on double-gradient conical hole arrayThe structure membrane, its characterized in that composite structure membrane be the aluminium foil membrane, there is the bell mouth on the aluminium foil membrane, the bell mouth cross-section be equilateral trapezoid, the hole radius of bell mouth is crescent from aluminium foil membrane upper surface to lower surface, aluminium foil membrane upper surface has low surface energy material C10H4Cl3F17Si, the lower surface material is Al2O3(ii) a The nano particles on the inner wall of the conical hole are gradually increased from the upper surface to the lower surface of the aluminum foil membrane, C10H4Cl3F17The component proportion of the Si material is gradually reduced; the periphery of the upper surface of the outer wall of the conical hole is of a non-petal-shaped rough structure, and the periphery of the lower surface of the outer wall of the conical hole is of a petal-shaped rough structure.
2. The composite structural membrane based on the double-gradient conical hole array as claimed in claim 1, wherein the contact angle of the top end of the outer wall of the conical hole exceeds 150 degrees, and the contact angle of the bottom end of the outer wall is less than 10 degrees.
3. The composite structure film based on the dual-gradient conical hole array as claimed in claim 1, wherein the water contact angle of a water drop on the upper surface of the outer wall of the conical hole of the composite structure film is 155 degrees, and the water contact angle on the lower surface of the outer wall is less than 10 degrees.
4. A preparation method of a composite structure film based on a double-gradient tapered hole array is characterized by comprising the following steps:
firstly, flatly placing an aluminum foil on a three-dimensional moving platform, firstly setting laser single pulse energy, moving a laser focus to the upper surface of the aluminum foil, setting a two-dimensional point array structure through scanning galvanometer software, and changing pulse impact times by setting focus retention time to prepare a double-sided super-hydrophilic micropore array structure;
secondly, placing the double-sided super-hydrophilic micropore array structure in a modifying solution to be soaked for 24 hours, and then heating the double-sided super-hydrophilic micropore array structure on a hot plate at the temperature of 60 ℃ for 30 minutes to obtain a double-sided super-hydrophobic membrane;
and thirdly, flatly placing the double-sided super-hydrophobic membrane on a three-dimensional moving platform, setting a laser focus at a position of 0.7mm above the upper surface, setting raster scanning at an interval of 25 microns, laser pulse energy of 75 muJ and a scanning speed of 10mm/s, and obtaining the composite structure membrane after scanning.
5. The method for preparing a composite structural film based on a dual gradient tapered hole array as claimed in claim 4, wherein the laser single pulse energy is 60-300 μ J.
6. The preparation method of the composite structure membrane based on the double-gradient tapered hole array as claimed in claim 4, wherein the modification liquid is ethanol: c10H4Cl3F17The Si is mixed according to the volume ratio of 1: 100.
7. The method for preparing the composite structure film based on the dual-gradient tapered hole array as claimed in claim 4, wherein the number of pulse impact times is 20-100.
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| CN112090710B (en) * | 2020-09-01 | 2022-09-02 | 安徽大学 | Multi-biological-characteristic inspired 'fog collection' composite double-sided miracle membrane and preparation method thereof |
| CN112487635B (en) * | 2020-11-26 | 2022-03-08 | 吉林大学 | Method for designing bionic gradient super-hydrophobic structure based on Marangoni effect |
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