CN112250033A - Super-oleophobic surface preparation method based on structure dipping-in-situ dragging forming - Google Patents
Super-oleophobic surface preparation method based on structure dipping-in-situ dragging forming Download PDFInfo
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Abstract
The invention discloses a method for preparing a super-oleophobic surface based on structural dipping-in-situ dragging forming, and relates to the technical field of functional surface preparation. The method comprises the following steps: (1) preparing a common polymer material micro-nano columnar structure surface by a replication molding method or a hot-press forming method, and treating the micro-nano structure surface by plasma to improve the surface energy of the surface; (2) coating a certain thickness of polymer material on the auxiliary smooth plane subjected to the silanization treatment; dipping the surface of the micro-nano columnar structure treated by the plasma into a polymer material, lifting the surface of the micro-nano columnar structure to enable the dipped polymer material to be simultaneously in contact with the micro-nano columnar structure and an auxiliary smooth plane and to realize necking, curing the polymer material, and separating the surface to realize preparation of a secondary groove structure. The secondary groove structure prepared by the invention is arranged at the top end of the micro-nano columnar structure, so that the distance from the oil liquid to the root position of the micro-nano columnar structure can be ensured when the oil liquid is contacted.
Description
Technical Field
The invention relates to the technical field of functional surface preparation, in particular to a structure dipping-in-situ dragging forming method for preparing a super-oleophobic surface, which is suitable for preparing the polymer super-oleophobic surface, and is particularly suitable for preparing the super-oleophobic surface under simple conditions.
Background
A superoleophobic surface is a surface that enables a droplet of liquid having a low surface tension to exhibit a large contact angle on its surface. With this function, superoleophobic surfaces have gained widespread attention in recent years.
Superoleophobic surfaces typically perform their function in a particular structural form. In order to achieve the Superoleophobic function of the surface, patents (201210569918.9, 201210569815.2) propose a series of Superoleophobic surface preparation methods, which achieve the secondary oleophobic function of the surface prepared by the secondary surface groove 1622 described in the literature (Ahuja A, Taylor J A, Lifton V, Sidorenko AA, Salamon T R, Lobaton E J, Kolodner P, Krupenkin T N.Nanonails: A Simple geometry Approach to electric tubular Superoleophobic surface 2008,24:9-14. and Tuteja A, Choi W, M, Mabry J M, Mazzella S A, forged G C, McKinley G H, Cohen R E.design Superoleophobic surface 2007,318: 1618). The two-step forming method (201210569918.9) is characterized in that on the basis of one-step forming, polydimethylsiloxane PDMS (Sylgard 184, Dow Corning) is selectively dipped on the surface of a microstructure, the surface of the microstructure dipped with the PDMS is pressed on a smooth surface to realize a secondary groove structure, the dipping amount of the PDMS is required to be accurately controlled when the groove structure is realized by adopting the method, the primary structure is easily blocked by too large amount of the PDMS, and the secondary groove structure is difficult to realize by too small amount of the PDMS. Furthermore, the pressure action in the two-step forming process can cause the existing microstructure to deform, rendering the process ineffective. The capillary forming method (201210569815.2) adopts a primary microstructure to guide a thin layer of PDMS to realize a secondary groove structure, but because the thickness of the PDMS needs to be controlled, the height of the groove structure realized at the moment is limited, which easily causes the failure of the performance of the super oleophobic surface.
In a word, various existing methods for preparing the super-oleophobic surface are available, but in terms of the existing method for preparing the super-oleophobic surface, the failure of the prepared super-oleophobic surface is easily caused by the small amount of secondary forming PDMS in the two-step forming method, and the super-oleophobic performance is not easily ensured because the structure height formed by the small amount of PDMS in the capillary forming method is too small. In order to realize the preparation of the super-oleophobic surface, the invention provides a structure dipping-in-situ dragging forming method.
Disclosure of Invention
The invention aims to provide a structure dipping-in-situ dragging forming method for preparing a super oleophobic surface, which realizes controllable preparation of the super oleophobic surface of a polymer material under simple conditions.
The invention is realized according to the following technical scheme:
a structural dipping-in-situ dragging forming method for preparing a super oleophobic surface comprises the following steps:
(1) preparing a common polymer material micro-nano columnar structure surface by a replication molding method or a hot-press forming method, and treating the micro-nano structure surface by plasma to improve the surface energy of the surface;
(2) coating a certain thickness of polymer material on the auxiliary smooth plane subjected to the silanization treatment; dipping the surface of the micro-nano columnar structure treated by the plasma into a polymer material, lifting the surface of the micro-nano columnar structure to enable the dipped polymer material to be simultaneously in contact with the micro-nano columnar structure and an auxiliary smooth plane and to realize necking, curing the polymer material, and separating the surface to realize preparation of a secondary groove structure.
In the step (1), a common polymer material micro-nano columnar structure surface is required to be prepared firstly, the preparation can be realized by a thermosetting polymer material replica molding method, and a liquid thermosetting polymer material is poured on a hole template to be heated and cured to obtain the micro-nano columnar structure surface; or the micro-column structure is prepared by a hot-press forming process of a thermoplastic polymer material, the thermoplastic polymer material is pressed on the hole template, the hole template is heated to realize micro-structure forming, and the thermoplastic polymer material is taken down after cooling to obtain the surface of the micro-column structure.
In the step (1), the obtained surface of the micro-nano columnar structure needs to be subjected to plasma treatment to improve the surface energy and enhance the bonding strength between the secondary groove structure to be formed and the columnar structure, the treatment process is to place the prepared micro-nano columnar structure in a vacuum cavity of a common plasma treatment machine, the micro-nano columnar surface is irradiated by radio frequency plasma of 13.56MHz, the plasma power is 100W-600W, and the treatment time is 10 s-600 s.
In step (2), the silanized auxiliary smooth surface is coated with a polymer to a certain thickness, and the process comprises: depositing a layer of silane with small surface energy on an auxiliary smooth surface by a vacuum vapor deposition method, dropping a liquid polymer material PDMS on the treated auxiliary smooth surface and spreading the polymer to a required thickness, wherein the thickness of the polymer material can be controlled by a spin coater, the rotating speed of the spin coater is set to be 600-4000 rpm, the spin coater time is set to be 10-60 s, and the thickness range of the polymer material is 1-10 μm.
In the step (2), the surface of the micro-nano columnar structure after plasma treatment needs to be dipped into a polymer material, the surface of the micro-nano columnar structure is lifted to enable the dipped polymer material to be simultaneously in contact with the micro-nano columnar structure and an auxiliary smooth plane and to realize necking, then the polymer material is cured, and finally the surface of the secondary groove structure is obtained.
In the step (2), the requirement for lifting the surface of the micro-nano columnar structure is as follows: the lifting height of the surface of the micro-nano columnar structure is 3-10 times of the thickness of the liquid polymer material.
In the step (2), the lifting height of the surface of the micro-nano columnar structure refers to the distance between the micro-nano columnar structure and the auxiliary smooth surface.
In the step (2), the polymer material is cured by selecting a curing method according to the performance of the material, and when the thermosetting material is used, the thermosetting method is selected, the liquid polymer PDMS is heated to 60-90 ℃, is kept warm for 60-120 minutes, and is slowly cooled along with a furnace.
The invention has the following technical advantages:
(1) the prepared secondary groove structure is arranged at the top end of the micro-nano columnar structure, so that the distance from the root position of the micro-nano columnar structure when oil is contacted can be ensured.
(2) And (3) deforming the material by adopting a dragging method, and removing uncertainty caused by deformation of the micro-nano structure under the action of pressure in a two-step forming method.
Drawings
FIG. 1 is a flow chart of a structure dipping-in-situ dragging forming super-oleophobic preparation method;
the structure comprises a micro-nano columnar structure surface 1, an auxiliary smooth surface 2, a silane hydrophobic layer 3, a hydrophilic layer 4, a liquid polymer film 5, a necking liquid polymer 6 and a super oleophobic surface 7 with a secondary groove structure.
Detailed Description
The details of the implementation and operation of the specific process proposed by the present invention are described below with reference to fig. 1.
The structure dipping-in-situ dragging forming method for preparing the super oleophobic surface is shown as the attached figure 1 and mainly comprises two steps: preparing a common micro-nano structure surface; constructing a surface with a secondary groove structure on the surface of a common micro-nano structure.
Firstly, a common polymer material micro-nano columnar structure surface 1 is prepared by a certain method, and the preparation method of the surface can adopt a replication molding method or a hot-pressing deformation method. When a replication molding method is adopted, firstly, a hole template which is complementary to the structure of the common polymer material micro-nano columnar structure surface 1 to be processed is prepared, a solidified polymer material is poured on the template and polymerized and solidified, and then demolding treatment is carried out to obtain the common polymer material micro-nano columnar structure surface 1. When a hot-pressing deformation method is adopted, firstly, a hole template which is complementary to the structure of the common polymer material micro-nano columnar structure surface 1 to be processed is prepared, a thermoplastic polymer sheet is pressed on the template and heated to deform the thermoplastic polymer sheet, the heating temperature is selected as the softening temperature of the polymer material, the heat preservation and pressure maintenance are carried out for 5 minutes after the softening temperature is reached, then, the hole template is cooled to the room temperature, and then, the demolding treatment is carried out to obtain the common polymer material micro-nano columnar structure surface 1
In order to realize the structure dipping-in-situ dragging forming method, the surface of the prepared common micro-nano columnar structure needs to be subjected to hydrophilic treatment so as to improve the bonding strength between the secondary groove structure to be formed and the existing structure, and the realization process is as follows: and (3) sending the prepared micro-nano columnar structure surface into a plasma irradiation part in a cavity of a plasma processing machine, vacuumizing the cavity, injecting a small amount of inert gas, generating plasma under a higher voltage, and acting the plasma on the micro-nano columnar structure surface to improve the surface energy of the surface to form a hydrophilic layer 4. And taking the micro-nano columnar structure surface subjected to the plasma treatment out of the vacuum cavity for later use. Preparing an auxiliary smooth surface 2, and performing silanization treatment on the auxiliary smooth surface 2, wherein the treatment process comprises the following steps: placing the auxiliary smooth surface 2 in a surface dish, dropwise adding 1 microliter of silane into the space not occupied by the auxiliary smooth surface in the surface dish, sending the prepared surface dish together with the auxiliary smooth surface 2 into a vacuum drying oven, vacuumizing and heating to 80 ℃, keeping the temperature for 1 hour, naturally cooling, taking out the auxiliary smooth surface 2, attaching a silane hydrophobic layer 3 on the auxiliary smooth surface, reducing the bonding strength between the secondary groove structure to be prepared and the auxiliary smooth surface 2, and facilitating the subsequent separation process.
And coating a liquid polymer film 5 with the thickness of 1-10 mu m on the auxiliary smooth surface 2 after the hydrophobic treatment by a spin coater, pouring a trace amount of the liquid polymer film 5 (with the volume of 1 mu L < V <20 mu L) on the smooth flat surface 2 with the hydrophobic layer 3 for the polymer which is usually in a liquid state, and spreading the liquid polymer film to the required thickness (1-10 mu m) by the spin coater. The prepared micro-nano columnar structure surface 1 with the hydrophilic layer 4 is contacted with a liquid polymer film 5 on the auxiliary smooth surface 2, then the micro-nano columnar structure surface 1 is lifted, the liquid polymer film is deformed under the dragging action of the micro-nano columnar structure surface to form a necking liquid polymer 6, the necking liquid polymer 6 is heated and solidified and is separated from the auxiliary smooth surface 2, and the surface 7 with the secondary groove structure can be obtained. Known analytical results indicate that (Ahuja A, Taylor J A, Lifton V, Sidorenko AA, Salamon T R, Lobaton E J, Kolodner P, Krupenkin T N.Nanonails: A Simple geological application to electric tubular Superlyotropic surface 2008,24:9-14. and Tuteja A, Choi W, Ma M, Mabry J M, Mazzella S A, Rutledge G C, McKiley G H, Cohen R E.design Superrophobic surfaces 2007,318: 1618-.
Example 1 (PDMS for the liquid Polymer film 5 and smooth Si for the smooth Flat surface 2)
Preparing a common micro-nano columnar structure surface 1 by adopting a replication molding method, wherein a pore array template is selected as the template, pores are circular holes, the pore diameter is 50 micrometers, the pore spacing is 100 micrometers, the material adopted by the replication molding is PDMS, and the replication molding process comprises the following steps: pouring a small amount of polydimethylsiloxane PDMS (which is purchased from Corning corporation of America under the trade name of Sylgard 184A) onto a template, then sending the template with spread PDMS into a vacuum drying oven, placing the vacuum drying oven in an environment with the temperature of 60 ℃ for reaction for 2 hours, and taking a PDMS replica from the template after curing, wherein the replica is the surface of the common micro-nano columnar structure. And (3) processing the obtained PDMS micro-nano columnar structure surface for 3 minutes by using 13.56MHz radio frequency plasma at the power of 200W, so as to improve the hydrophilicity of the micro-nano columnar structure surface.
Performing silanization treatment on the surface of a smooth silicon wafer, wherein the used silane is 1H,1H,2H, 2H-perfluorodecyl triethoxysilane, and the treated surface has a hydrophobic thin layer. And then dripping a small amount of PDMS (the volume is less than 20 mu L) on the smooth silicon wafer, and enabling the rotating speed of the silicon wafer to reach 2000 r/m through a spin coater, so that the smooth and straight silicon wafer coated with the liquid PDMS film can be obtained. Immersing the surface of the obtained micro-nano columnar structure into a PDMS film and quickly lifting the surface to 50 micrometers, keeping the state, sending the smooth and flat surface of the silicon wafer and the surface of the micro-nano columnar structure into a vacuum drying oven, heating the surface to 60 ℃, and taking down the surface of the PDMS microstructure from the surface of the silicon wafer after curing for 2 hours. The microstructure surface prepared at this time is the microstructure surface with the secondary grooves. According to the existing theory and experimental results (Tuteja A, Choi W, Ma M, Mabry J M, Mazzella S A, Rutledge G C, McKinley G H, Cohen R E.designing Superoleophobic surfaces 2007,318:1618 + 1622.), the secondary groove structure can effectively control the spreading of the oil liquid among the microstructures, so that a composite interface between the oil liquid and the microstructures is constructed, and the oil liquid is in a Cassie contact state on the surfaces of the microstructures, namely the surfaces of the microstructures with the secondary groove structure have super oleophobic property. Therefore, the surface with the secondary groove microstructure prepared in this example theoretically has superoleophobic properties.
Claims (8)
1. A structural dipping-in-situ dragging forming method for preparing a super oleophobic surface is characterized by comprising the following steps:
(1) preparing a common polymer material micro-nano columnar structure surface by a replication molding method or a hot-press forming method, and treating the micro-nano structure surface by plasma to improve the surface energy of the surface;
(2) coating a certain thickness of polymer material on the auxiliary smooth plane subjected to the silanization treatment; dipping the surface of the micro-nano columnar structure treated by the plasma into a polymer material, lifting the surface of the micro-nano columnar structure to enable the dipped polymer material to be simultaneously in contact with the micro-nano columnar structure and an auxiliary smooth plane and to realize necking, curing the polymer material, and separating the surface to realize preparation of a secondary groove structure.
2. The dipping-in-situ dragging forming method of the structure for preparing the super oleophobic surface according to the claim 1 is characterized in that in the step (1), firstly, a common polymer material micro-nano columnar structure surface is prepared, the preparation can be carried out by a duplication molding method of a thermosetting polymer material, and the liquid thermosetting polymer material is poured on a hole template to be heated and cured to obtain the micro-nano columnar structure surface; or the micro-column structure is prepared by a hot-press forming process of a thermoplastic polymer material, the thermoplastic polymer material is pressed on the hole template, the hole template is heated to realize micro-structure forming, and the thermoplastic polymer material is taken down after cooling to obtain the surface of the micro-column structure.
3. The structure dipping-in-situ dragging forming method for preparing the super oleophobic surface according to claim 1 is characterized in that in the step (1), plasma treatment is carried out on the obtained micro-nano columnar structure surface to improve the surface energy and enhance the bonding strength between the secondary groove structure to be formed and the columnar structure, the treatment process is to place the prepared micro-nano columnar structure in a vacuum cavity of a general plasma treatment machine, the micro-nano columnar surface is irradiated by radio frequency plasma of 13.56MHz, the plasma power is 100W-600W, and the treatment time is 10 s-600 s.
4. The dip-in-situ drag forming process for preparing super oleophobic surface according to claim 1, wherein in step (2), a polymer is coated on the silanized auxiliary smooth surface to a certain thickness, and the process is as follows: depositing a layer of silane with small surface energy on an auxiliary smooth surface by a vacuum vapor deposition method, dropping a liquid polymer material PDMS on the treated auxiliary smooth surface and spreading the polymer to a required thickness, wherein the thickness of the polymer material can be controlled by a spin coater, the rotating speed of the spin coater is set to be 600-4000 rpm, the spin coater time is set to be 10-60 s, and the thickness range of the polymer material is 1-10 μm.
5. The structure dipping-in-situ dragging forming method for preparing the super-oleophobic surface according to claim 1 is characterized in that in the step (2), the surface of the micro-nano columnar structure after plasma treatment is dipped into a polymer material, the surface of the micro-nano columnar structure is lifted to enable the dipped polymer material to simultaneously contact with the micro-nano columnar structure and an auxiliary smooth plane and realize necking, then the polymer material is cured, and finally the surface of a secondary groove structure is obtained.
6. The structure dipping-in-situ dragging forming method for preparing the super oleophobic surface according to claim 1, characterized in that in step (2), the requirement for lifting the micro-nano columnar structure surface is as follows: the lifting height of the surface of the micro-nano columnar structure is 3-10 times of the thickness of the liquid polymer material.
7. The dipping-in-situ dragging forming method for preparing the structure of the super oleophobic surface according to claim 1, wherein in step (2), the lifting height of the micro-nano columnar structure surface refers to the distance between the micro-nano columnar structure and the auxiliary smooth surface.
8. The dipping-in-situ dragging forming method for preparing the structure of the super oleophobic surface according to the claim 1, characterized in that in the step (2), the curing method is selected according to the property of the material by curing the polymer material, and when the thermosetting material is used, the thermosetting method is selected, the liquid polymer PDMS is heated to 60-90 ℃, kept for 60-120 minutes and slowly cooled with the furnace.
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| CN202011046931.7A CN112250033A (en) | 2020-09-29 | 2020-09-29 | Super-oleophobic surface preparation method based on structure dipping-in-situ dragging forming |
| PCT/CN2021/112955 WO2022068441A1 (en) | 2020-09-29 | 2021-08-17 | Structure dipping-in situ drag forming based method for preparing super-oleophobic surface |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113148944A (en) * | 2021-02-02 | 2021-07-23 | 南京航空航天大学 | Precise dipping mechanism and method for manufacturing mushroom head micro-column array |
| WO2022068441A1 (en) * | 2020-09-29 | 2022-04-07 | 江苏大学 | Structure dipping-in situ drag forming based method for preparing super-oleophobic surface |
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