CN105220185A - A kind of preparation method of super oleophobic micro-pillar array Surface Texture - Google Patents
A kind of preparation method of super oleophobic micro-pillar array Surface Texture Download PDFInfo
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- CN105220185A CN105220185A CN201510714921.9A CN201510714921A CN105220185A CN 105220185 A CN105220185 A CN 105220185A CN 201510714921 A CN201510714921 A CN 201510714921A CN 105220185 A CN105220185 A CN 105220185A
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Abstract
The invention discloses a kind of preparation method of super oleophobic micro-pillar array Surface Texture, it comprises the following steps: S1, carry out cleaning and drying to metal base; The even glue of S2, photoresist material, front baking Procuring; S3, resist exposure, be placed in above photoresist material by the mask plate with specific pierced pattern, and copy mask plate pattern is to photoresist material; The development of S4, photoresist material and rear baking, make photoresist material produces microwell array; S5, a micro-pillar array electroforming produce metal micro-pillar array; S6, remove certain thickness photoresist material, make all microtrabeculaes will expose the top ends of local; S7, the electroforming of micro-pillar array secondary, form super oleophobic head of a nail structure; Wet method is removed photoresist completely; Low surface energy is modified.After building microwell array by photoresist material, electroforming forms straight body micro-pillar array, and removal unit divides photoresist material to expose microtrabeculae top, carries out secondary electroforming and builds microtrabeculae cap body, thus builds evenly regular and be applicable to the shaping super oleophobic surface texture of scale.
Description
Technical field
The present invention relates to a kind of micro-texture technical field, particularly relate to a kind of preparation method of super oleophobic micro-pillar array Surface Texture.
Background technology
Wettability is the universal phenomenon that there is occurring in nature, and the phenomenon that such as rainwater forms spherical drop after dropping on lotus leaf surface and tumbles and the self_cleaning effect that lotus leaf " goes out mud and do not contaminate ", be super-hydrophobic phenomenon.In addition the pin of many animals and plants as water skipper, the wing, Rice Leaf etc. of butterfly, also have ultra-hydrophobicity.Research shows, all these surfaces there is superhydrophobic characteristic formed due to micro-nano coarse structure and low-surface energy substance acting in conjunction.
Wettability is also the importance in Materials science and Surface Engineering field simultaneously, in daily life, industrial production, has many important application in agriculture production.So-called super-hydrophobicly refers to that the static contact angle of water droplet at solid surface is more than 150 °, in like manner, super oleophobic and oil droplet at the static contact angle of solid surface more than 150 °.But the surface tension of oil droplet is much smaller than the surface tension of water droplet, and therefore, prepare the solid surface with super oleophobic property, its difficulty is larger than super hydrophobic surface, more difficult realization.Correlative study shows, prepare super oleophobic surface in air and, except needing the modification of low surface energy molecule, also micro-nano coarse structure will be with to introduce recessed surface curvature on the surface at it, make micro-nano coarse structure be indent or cantilever.This proposes larger challenge to manufacturing process.
At present, a large amount of documents has reported artificial bionic super hydrophobic surface, and these materials are at self-cleaning surface, anti-icing, antifog, anti-pollution, and anticorrosive metal is widely used in fluid drag-reduction.Report about oleophobic surface is relatively less, but super oleophobic surface such as grease proofness coating in industrial and agricultural production, the antifouling process of seawater, petroleum pipe line is grease proofing creeps, and has huge application space in oily water separation.Metallic substance is widely applied in engineering, use face extremely extensive, but the antipollution Corrosion Protection of metal is poor, and therefore on metal, preparation has super oleophobic property surface and is significant.
So-called Surface Texture (Surfacetexture) refers to that body surface has the array of the patterns such as the pit of certain size and arrangement, indenture or convex closure.The surface with micro-nano-scale microcosmic texture shows distinct feature with smooth surface in surface energy, optical characteristics, bionical characteristic, mechanical characteristics, hydrodynamic characteristics and friction and wear behavior etc., this is filled with new vitality for numerous disciplinary study, and shows huge application potential at many engineering fields.
The preparation method of oleophobic surface follows from bottom to top or top-to-bottom method usually.The processing method that existing preparation surpasses oleophobic surface mainly contains following several: (1) nothing/have template wet etching (2) femtosecond laser etching method (3) method of electrostatic spinning (4) electrodip process (5) sol-gel method etc.
Wherein there is following corresponding defect in aforesaid method: (1) can etch silicon and metallic surface without template wet etching, and efficiency is high and cost is low, but etching surface morphology controllable is poor, and the method easily obtains super hydrophobic surface, but the not easily super oleophobic surface of acquisition; Oleophobic surface can be obtained by Bosch etching method, but complex process and be only suitable for silicon materials.(2) femtosecond laser etching method can prepare the micro-nano nesting structure surface that precision is high, pattern is regular, but this process efficiency is low, be not suitable for extensive manufacture, and equipment is extremely expensive.(3) method of electrostatic spinning is by utilizing micro-/ nano filament at surface construction coarse structure, and easily by controlling to produce oleophobic surface desired structure, but prepared surperficial mechanical mechanics property is poor, and do not possess good wear resistance etc., work-ing life is shorter; (4) electrodip process can metal refining or polymkeric substance, efficiently can prepare easily and have micro-nano coarse structure surface, but pattern randomness is strong, wayward, and not easily produces indent or cantilever design.
Summary of the invention
Not enough for prior art, the technical problem to be solved in the present invention is to provide a kind of preparation method with the super oleophobic micro-pillar array Surface Texture of excellent abrasive resistance obtaining even rule, morphology controllable and be also applicable to scale production.
In order to overcome prior art deficiency, the technical solution used in the present invention is: a kind of preparation method of super oleophobic micro-pillar array Surface Texture, for building super oleophobic surface texture in metal base, the preparation method of described super oleophobic micro-pillar array Surface Texture comprises the following steps:
S1, carry out cleaning and drying to metal base, remove surface and oil contaminant and impurity;
The even glue of S2, photoresist material, front baking, photoresist material is positive glue, is evenly spun on the forward surface of metal base, then utilizes baking oven to carry out front baking Procuring to workpiece by sol evenning machine;
S3, resist exposure, be placed in above photoresist material by the mask plate with specific pierced pattern, the irradiation of the openwork part of UV light permeability mask plate is carried out exposure to it on a photoresist and makes it produce photochemical reaction, thus copy mask plate pattern is to photoresist material;
The development of S4, photoresist material and rear baking, be placed in developing solution by the photoresist material replicating mask plate pattern, removes the photoresist material being exposed part, make photoresist material produces microwell array; Workpiece is taken out developing solution to be placed on baking oven and to carry out rear baking technique, it is solidified further;
S5, a micro-pillar array electroforming, using workpiece as negative electrode, nickel block is as anode, be connected with positive pole with the negative pole of electroforming power supply respectively, and the electroforming system being placed in suitable electroforming liquid pool formation one complete carries out electroforming, after energising, under the domination of cathodic deposition principle, make nickel ion be reduced into metallic nickel bottom micropore, make metallic nickel fill up all micropores, produce metal micro-pillar array;
S6, dry method are removed photoresist and are removed certain thickness photoresist material, make all microtrabeculaes expose the top ends of local;
S7, the electroforming of micro-pillar array secondary, be placed in electroforming system by workpiece and carry out secondary electroforming, under the domination of cathodic deposition principle, nickel ion is reduced into be greater than the metallic nickel pier block of the hat shape of microtrabeculae basis root at microtrabeculae top, forms super oleophobic head of a nail structure;
S8, wet method are removed photoresist completely, workpiece are immersed in the solution that removes photoresist and carry out isotropy wet method and remove photoresist, make photoresist material generation chemical reaction, be washed and remove completely, finally obtain micro-pillar array Surface Texture after formation reaction thing;
S9, low surface energy are modified, and having the carrying tablet of silicon fluoride to be jointly placed in encloses container the workpiece through secondary eletroforming, then putting into 65 DEG C of baking ovens and toasting 1 hour, putting to room temperature, complete the preparation of workpiece after taking-up with dripping.
The one surpassing the technical scheme of the preparation method of oleophobic micro-pillar array Surface Texture as the present invention is improved, in step sl, the metal base of effects on surface flat smooth utilizes alkali lye to remove metal surface greasy dirt, then be placed in the Ultrasonic Cleaners filling ethanolic soln and clean, recycling removal of surfactant oxidation on metal surface layer, finally dries by washed with de-ionized water juxtaposition and removes surface-moisture in baking oven.
The one surpassing the technical scheme of the preparation method of oleophobic micro-pillar array Surface Texture as the present invention is improved, in step s 6, dry method is utilized not exclusively to remove photoresist, utilize plasma body to carry out anisotropic dry to workpiece surface to remove photoresist, make top layer photoresist material certain thickness scope generation polymer reaction, thus be removed after generating the reactant of easy volatile.
The invention has the beneficial effects as follows: form straight body micro-pillar array by then carrying out an electroforming at metal base attachment photoresist material structure microwell array, then removal unit divides photoresist material to expose microtrabeculae top, carry out secondary electroforming again and build microtrabeculae top cap body, form the micro-pillar array of head of a nail shape, thus build super oleophobic surface texture in metallic surface.This Surface Texture as assist medium, because photoresist material is easy to accurately processing thus the Surface Texture built is convenient to reach evenly rule to be applicable to scale shaping, uses nickel material electroforming to make micro-texture surface of component have good wear resistance by photoresist material.
Accompanying drawing explanation
Fig. 1 is the Workpiece structure schematic diagram in each stage of the preparation process of a kind of super oleophobic micro-pillar array Surface Texture of the present invention.
Fig. 2 is the perspective view of the metal base being built with Surface Texture.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the present invention are specifically described.
Fig. 1 illustrates the structure in each stage of workpiece in technological process of the present invention, the preparation method of a kind of super oleophobic micro-pillar array Surface Texture of the present invention, for building super oleophobic surface texture in metal base, the preparation method of described super oleophobic micro-pillar array Surface Texture comprises the following steps:
S1, carry out cleaning and drying to metal base 1, remove surface and oil contaminant and impurity; Make metal base 1 surface cleaning clean, be convenient to carry out follow-up texture component technique and carry out, texture and metal base 1 are connected firmly.
The even glue of S2, photoresist material, front baking, photoresist material is positive glue, is evenly spun on the forward surface of metal base 1, then utilizes baking oven to carry out front baking Procuring to workpiece by sol evenning machine; Thus form the photoresist material 2 of sheet of Procuring, follow-uply build vertical core for building micro-pillar array at this photoresist material 2, therefore the thickness of this photoresist material 2 determines the height of micro-pillar array.
S3, resist exposure, the mask plate 3 with specific pierced pattern is placed in above photoresist material, UV-light 4 is radiated at through the openwork part of mask plate 3 and photoresist material 2 carries out exposure to it makes it produce photochemical reaction, thus copy mask plate pattern is to photoresist material 2; By the design to mask plate 3 pattern, the different texture of size, pattern, arrangement and density can be obtained on photoresist material 2, by the control to these parameters, final metallic surface can be controlled and surpass oleophobic energy.
The development of S4, photoresist material and rear baking, be placed in developing solution by the photoresist material 2 replicating mask plate pattern, removes and be exposed photoresist material 2 partly until bottom makes its flood photoresist material 2 penetrate, make photoresist material to produce micropore 10 and form microwell array; Workpiece is taken out developing solution to be placed on baking oven and to carry out rear baking technique, it is solidified further; Thus form the straight body microwell array with required specified shape, structure and arranging density.
S5, a micro-pillar array electroforming, using workpiece as negative electrode, nickel block is as anode, be connected with positive pole with the negative pole of electroforming power supply respectively, and the electroforming system being placed in suitable electroforming liquid pool formation one complete carries out electroforming, after energising, under the domination of cathodic deposition principle, nickel ion is reduced into metallic nickel bottom micropore, makes metallic nickel fill up all micropores, thus the straight body metal microtrabeculae 5 that structure has required specified shape, structure and arranging density forms micro-pillar array.
S6, dry method are removed photoresist and are removed certain thickness photoresist material, make all microtrabeculaes 5 by exposing the top ends of local, for follow-up secondary electroforming.
S7, the electroforming of micro-pillar array secondary, workpiece is placed in electroforming system and carries out secondary electroforming, under the domination of cathodic deposition principle, microtrabeculae 5 top of protruding is respectively to the nickel ion accepting electroforming equably, namely end face and periphery all grow generation electroforming device, nickel ion is reduced into be greater than the metallic nickel pier block 7 of the hat shape of microtrabeculae basis root at microtrabeculae 5 top, forms super oleophobic head of a nail structure; The cantilever design of different characteristics size can be obtained by the control of process period, electrical parameter (current density, frequency, dutycycle) and electroforming solution parameter (temperature and concentration) etc., thus affect the super oleophobic energy of final workpiece surface.
S8, wet method are removed photoresist completely, workpiece are immersed in the solution 8 that removes photoresist and carry out isotropy wet method and remove photoresist, make photoresist material 2 that chemical reaction occur, be washed and remove completely, finally obtain micro-pillar array Surface Texture, as shown in Figure 2 after formation reaction thing.
S9, low surface energy are modified, and having the carrying tablet of silicon fluoride to be jointly placed in encloses container the workpiece through electrochemical machining, then putting into 65 DEG C of baking ovens and toasting 1 hour, putting to room temperature, complete the preparation of workpiece after taking-up with dripping.In baking engineering, silicon fluoride 9 will form the low-surface energy substance of one deck nano thin-layer at workpiece surface by adsorption, make metallic surface reach super oleophobic energy.
This processing method forms straight body micro-pillar array by then carrying out an electroforming at metal base attachment photoresist material structure microwell array, then removal unit divides photoresist material to expose microtrabeculae top, carry out secondary electroforming again and build microtrabeculae top cap body, form the micro-pillar array of head of a nail shape, thus build super oleophobic surface texture in metallic surface.This Surface Texture is by photoresist material as assist medium, and because photoresist material is easy to accurately processing thus the Surface Texture built is convenient to reach evenly rule to be applicable to scale shaping, the use of nickel metal makes surface have good wear resistance.
More preferably, in step sl, the metal base 1 of effects on surface flat smooth utilizes alkali lye to remove metal surface greasy dirt, then be placed in the Ultrasonic Cleaners filling ethanolic soln and clean, recycling removal of surfactant oxidation on metal surface layer, finally dries by washed with de-ionized water juxtaposition and removes surface-moisture in baking oven.Make metal base 1 surface cleaning clean inclusion-free non-oxidation layer, be convenient in its surface construction micro-pillar array.
More preferably, in step s 6, dry method is utilized not exclusively to remove photoresist, utilize plasma body or other materials removing Other substrate materials to carry out anisotropic dry to workpiece surface to remove photoresist, make top layer photoresist material certain thickness scope generation polymer reaction, thus be removed after generating the reactant of easy volatile, after removing the photoresist material of certain thickness layer, microtrabeculae top gauge height is more consistent.
Above disclosedly be only the preferred embodiments of the present invention, certainly can not limit the interest field of the present invention with this, therefore according to the equivalent variations that the present patent application the scope of the claims is done, still belong to the scope that the present invention is contained.
Claims (3)
1. a preparation method for super oleophobic micro-pillar array Surface Texture, for building super oleophobic surface texture in metal base, it is characterized in that, the preparation method of described super oleophobic micro-pillar array Surface Texture comprises the following steps:
S1, carry out cleaning and drying to metal base, remove surface and oil contaminant and impurity;
The even glue of S2, photoresist material, front baking, photoresist material is positive glue, is evenly spun on the forward surface of metal base, then utilizes baking oven to carry out front baking Procuring to workpiece by sol evenning machine;
S3, resist exposure, be placed in above photoresist material by the mask plate with specific pierced pattern, the irradiation of the openwork part of UV light permeability mask plate is carried out exposure to it on a photoresist and makes it produce photochemical reaction, thus copy mask plate pattern is to photoresist material;
The development of S4, photoresist material and rear baking, be placed in developing solution by the photoresist material replicating mask plate pattern, removes the photoresist material being exposed part, make photoresist material produces microwell array; Workpiece is taken out developing solution to be placed on baking oven and to carry out rear baking technique, it is solidified further;
S5, a micro-pillar array electroforming, using workpiece as negative electrode, nickel block is as anode, be connected with positive pole with the negative pole of electroforming power supply respectively, and the electroforming system being placed in suitable electroforming liquid pool formation one complete carries out electroforming, after energising, under the domination of cathodic deposition principle, make nickel ion be reduced into metallic nickel bottom micropore, make metallic nickel fill up all micropores, produce metal micro-pillar array;
S6, dry method are removed photoresist and are removed certain thickness photoresist material, make all microtrabeculaes expose the top ends of local;
S7, the electroforming of micro-pillar array secondary, be placed in electroforming system by workpiece and carry out secondary electroforming, under the domination of cathodic deposition principle, nickel ion is reduced into be greater than the metallic nickel pier block of the hat shape of microtrabeculae basis root at microtrabeculae top, forms super oleophobic head of a nail structure;
S8, wet method are removed photoresist completely, workpiece are immersed in the solution that removes photoresist and carry out isotropy wet method and remove photoresist, make photoresist material generation chemical reaction, be washed and remove completely, finally obtain micro-pillar array Surface Texture after formation reaction thing;
S9, low surface energy are modified, and having the carrying tablet of silicon fluoride to be jointly placed in encloses container the workpiece through secondary eletroforming, then putting into 65 DEG C of baking ovens and toasting 1 hour, putting to room temperature, complete the preparation of workpiece after taking-up with dripping.
2. the preparation method of super oleophobic micro-pillar array Surface Texture according to claim 1, it is characterized in that: in step sl, the metal base of effects on surface flat smooth utilizes alkali lye to remove metal surface greasy dirt, then be placed in the Ultrasonic Cleaners filling ethanolic soln and clean, recycling removal of surfactant oxidation on metal surface layer, finally dries by washed with de-ionized water juxtaposition and removes surface-moisture in baking oven.
3. the preparation method of super oleophobic micro-pillar array Surface Texture according to claim 1, it is characterized in that: in step s 6, dry method is utilized not exclusively to remove photoresist, namely utilize plasma body to carry out anisotropic dry to workpiece surface to remove photoresist, make top layer photoresist material certain thickness scope generation polymer reaction, thus be removed after generating the reactant of easy volatile.
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Cited By (13)
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| CN106048665A (en) * | 2016-07-07 | 2016-10-26 | 广东工业大学 | Method for preparing metal-base super-oleophobic composite casting layer by using hot compression deformation process |
| CN107574464A (en) * | 2017-08-31 | 2018-01-12 | 华侨大学 | A kind of preparation method with hierarchical structure mushroom-shaped metal column array surface |
| CN108287227A (en) * | 2017-12-25 | 2018-07-17 | 新兴铸管（浙江）铜业有限公司 | A kind of diameter 8mm continuous casting and rolling low oxygens copper bar high oxygen content accuracy checking method |
| CN108751125A (en) * | 2018-06-07 | 2018-11-06 | 皖西学院 | A method of improving photoresist glue-line and electroforming metal bed boundary binding force |
| CN111054918A (en) * | 2019-12-26 | 2020-04-24 | 武汉大学 | Method for accurately preparing superfine metal micro-pillar array suitable for controllable biosensor spacing |
| CN111115548A (en) * | 2019-11-25 | 2020-05-08 | 广东工业大学 | Mushroom-shaped super-hydrophobic-super-oleophobic PDMS micro-nano composite array and preparation method and application thereof |
| CN111268640A (en) * | 2020-03-04 | 2020-06-12 | 电子科技大学 | Adaptive super-hydrophobic surface and preparation method thereof |
| CN112624032A (en) * | 2020-12-14 | 2021-04-09 | 南京工业大学 | Preparation method of composite reentrant angle micrometer structure with super-amphiphobicity |
| 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 |
| CN113319387A (en) * | 2021-06-18 | 2021-08-31 | 南京航空航天大学 | Large-scale preparation method of heat exchange enhancement microstructure |
| CN115122549A (en) * | 2022-06-22 | 2022-09-30 | 西北工业大学 | Flexible umbrella-shaped micro-structure array super surface and manufacturing method thereof |
| CN115390167A (en) * | 2022-09-02 | 2022-11-25 | 中国科学院上海微***与信息技术研究所 | Flexible micro-lens array and preparation method thereof |
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| CN106048665A (en) * | 2016-07-07 | 2016-10-26 | 广东工业大学 | Method for preparing metal-base super-oleophobic composite casting layer by using hot compression deformation process |
| CN107574464A (en) * | 2017-08-31 | 2018-01-12 | 华侨大学 | A kind of preparation method with hierarchical structure mushroom-shaped metal column array surface |
| CN108287227A (en) * | 2017-12-25 | 2018-07-17 | 新兴铸管（浙江）铜业有限公司 | A kind of diameter 8mm continuous casting and rolling low oxygens copper bar high oxygen content accuracy checking method |
| CN108287227B (en) * | 2017-12-25 | 2020-10-13 | 新兴铸管（浙江）铜业有限公司 | High-precision detection method for oxygen content of 8 mm-diameter continuous casting and rolling low-oxygen copper rod |
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| CN112624032A (en) * | 2020-12-14 | 2021-04-09 | 南京工业大学 | Preparation method of composite reentrant angle micrometer structure with super-amphiphobicity |
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| CN113319387A (en) * | 2021-06-18 | 2021-08-31 | 南京航空航天大学 | Large-scale preparation method of heat exchange enhancement microstructure |
| CN113319387B (en) * | 2021-06-18 | 2022-04-12 | 南京航空航天大学 | Large-scale preparation method of heat exchange enhancement microstructure |
| TWI825470B (en) * | 2021-08-26 | 2023-12-11 | 達運精密工業股份有限公司 | Method of fabricating metal mask |
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| CN115390167A (en) * | 2022-09-02 | 2022-11-25 | 中国科学院上海微***与信息技术研究所 | Flexible micro-lens array and preparation method thereof |
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