CN105220185B - A kind of preparation method of superoleophobic micro-pillar array Surface Texture - Google Patents
A kind of preparation method of superoleophobic micro-pillar array Surface Texture Download PDFInfo
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- CN105220185B CN105220185B CN201510714921.9A CN201510714921A CN105220185B CN 105220185 B CN105220185 B CN 105220185B CN 201510714921 A CN201510714921 A CN 201510714921A CN 105220185 B CN105220185 B CN 105220185B
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- photoresist
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- electroforming
- superoleophobic
- pillar array
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Abstract
The invention discloses a kind of preparation method of superoleophobic micro-pillar array Surface Texture, it comprises the following steps：S1, metallic substrates are cleaned and dried；S2, photoresist spin coating, front baking precuring；S3, photoresist exposure, the mask plate with specific pierced pattern are placed in above photoresist, copy mask plate pattern to photoresist；S4, the development of photoresist and rear baking, make to produce microwell array on photoresist；S5, electroforming of micro-pillar array produce metal micro-pillar array；S6, the certain thickness photoresist of removal, make all microtrabeculaes to expose local top ends；The secondary electroforming of S7, micro-pillar array, forms superoleophobic head of a nail structure；Wet method is removed photoresist completely；Low-surface-energy is modified.Electroforming after microwell array is built by photoresist and forms straight body micro-pillar array, part photoresist is removed and exposes microtrabeculae top, secondary electroforming is carried out and builds microtrabeculae cap body, so as to build uniform rule and be adapted to the superoleophobic Surface Texture of scale shaping.
Description
Technical field
The present invention relates to a kind of micro- texture technical field, more particularly to a kind of preparation of superoleophobic micro-pillar array Surface Texture
Method.
Background technology
Wetability is the presence of the universal phenomenon in nature, and such as rainwater falls to be formed spherical drop and roll after lotus leaf surface
The self_cleaning effect of the phenomenon and lotus leaf " going out mud without dye " that fall, as super-hydrophobic phenomenon.In addition many animals and plants such as water
Mian pin, the wing of butterfly, Rice Leaf etc., it may have ultra-hydrophobicity.Research shows that all these surfaces have super-hydrophobic
Characteristic is due to formed by micro-nano coarse structure and low-surface energy substance collective effect.
Wetability is also the importance in material science and Surface Engineering field simultaneously, in daily life, industrial production, agriculture
There are many important applications in industry production.The so-called super-hydrophobic static contact angle for referring to water droplet in the surface of solids is more than 150 °, similarly,
It is superoleophobic i.e. oil droplet the surface of solids static contact angle more than 150 °.However, the surface tension of oil droplet is much smaller than the table of water droplet
Face tension force, therefore, prepares the surface of solids with superoleophobic characteristic, its difficulty is bigger than super hydrophobic surface, it more difficult to realize.Phase
Close research to show, to prepare superoleophobic surface in air, will also be in its band micro-nano in addition to needing the modification of low-surface-energy molecule
Rice coarse structure introduces concave surface curvature on surface so that micro-nano coarse structure is in indent or cantilever.This gives manufacturing process
Propose bigger challenge.
At present, substantial amounts of document is it has been reported that artificial bionic super hydrophobic surface, these materials are prevented in self-cleaning surface
It is widely used in ice, antifog, anti-pollution, anticorrosive metal, fluid drag-reduction.Report on oleophobic surface is relatively fewer,
But superoleophobic surface such as grease proofness coating, seawater antifouling process in industrial and agricultural production, petroleum pipeline is grease proofing to creep, profit point
There is huge application space from.Metal material is widely applied in engineering, extremely extensive using face, but the anti-soil of metal
Contaminate Corrosion Protection poor, therefore being prepared on metal, there is superoleophobic characteristic surface to be significant.
So-called Surface Texture (Surface texture) refers to that body surface has the pit, recessed of certain size and arrangement
The array of the pattern such as trace or convex closure.Surface with the microcosmic texture of micro-nano-scale surface energy, optical characteristics, bionical characteristic,
The characteristics of showing completely different with smooth surface in terms of mechanical property, hydrodynamic characteristics and friction and wear behavior, this
New vitality is filled with for numerous disciplinary studies, and shows in many engineering fields huge application potential.
The preparation method of oleophobic surface is generally followed from bottom to top or top-to-bottom method.It is existing to prepare superoleophobic surface
Process mainly have following several：（1）Without/there is template wet etching（2）Femtosecond laser etching method（3）Method of electrostatic spinning
（4）Electrodeposition process（5）Sol-gel process etc..
Wherein there is following corresponding defect in the above method：（1）Silicon and metal surface can be etched without template wet etching,
Efficiency high and cost is low, but etching surface morphology controllable is poor, and this method is readily obtained super hydrophobic surface, but is difficult to obtain super thin
Oil meter face；Oleophobic surface can be obtained by Bosch etching methods, but complex process and be only suitable for silicon materials.（2）Femtosecond laser is carved
Erosion method can prepare the micro-nano nested structure surface that precision is high, pattern is regular, but the process efficiency is low, be not suitable for extensive system
Make, and equipment is extremely expensive.（3）Method of electrostatic spinning by using micro-/ nano filament in surface construction coarse structure, easily by
Control produces structure needed for oleophobic surface, but prepared surface mechanical mechanics property is poor, does not possess good wearability etc.,
Service life is shorter；（4）Electrodeposition process efficiently can be prepared easily with micro-nano coarse with deposited metal or polymer
Body structure surface, but pattern randomness is strong, is difficult to control, and be not likely to produce indent or cantilever design.
The content of the invention
Can in view of the shortcomings of the prior art, obtaining uniform rule, pattern the technical problem to be solved in the present invention is to provide one kind
Control and be adapted to the preparation method of the superoleophobic micro-pillar array Surface Texture with excellent abrasive resistance of large-scale production.
In order to overcome prior art not enough, the technical solution adopted by the present invention is：Knit on a kind of superoleophobic micro-pillar array surface
The preparation method of structure, for building superoleophobic Surface Texture, the system of the superoleophobic micro-pillar array Surface Texture in metallic substrates
Preparation Method comprises the following steps：
S1, metallic substrates are cleaned and dried, remove surface and oil contaminant and impurity；
S2, photoresist spin coating, front baking, photoresist is positive photoresist, and the positive table of metallic substrates is uniformly spun on by sol evenning machine
Face, then carries out front baking precuring using baking oven to workpiece；
S3, photoresist exposure, the mask plate with specific pierced pattern is placed in above photoresist, UV light permeability is covered
The openwork part irradiation of diaphragm plate is exposed to it on a photoresist makes it produce photochemical reaction, so that copy mask plate pattern
To photoresist；
S4, the development of photoresist and rear baking, the photoresist for replicating mask plate pattern are placed in developer solution, removal is exposed
The photoresist of light part, makes to produce microwell array on photoresist；Workpiece is taken out to be placed in after developer solution after baking oven is carried out and dries technique,
To its further solidification；
S5, electroforming of micro-pillar array, using workpiece as negative electrode, nickel block is as anode, respectively with the negative pole of electroforming power supply
It is connected with positive pole, is placed in constituting a complete electroforming system progress electroforming in suitable electroforming liquid pool, after energization, in the moon
Under the domination of pole deposition principle, nickel ion is reduced into metallic nickel in micropore bottom, metallic nickel is filled up all micropores, produce gold
Belong to micro-pillar array；
S6, dry method, which are removed photoresist, removes certain thickness photoresist, all microtrabeculaes is exposed local top ends；
The secondary electroforming of S7, micro-pillar array, workpiece is placed in electroforming system and carries out secondary electroforming, in negative electrode deposition principle
Under domination, nickel ion is reduced into the metallic nickel pier block of the hat shape more than the basic root of microtrabeculae at the top of microtrabeculae, form superoleophobic nail
Cap；
S8, wet method are removed photoresist completely, and workpiece is immersed in into sol solution progress isotropism wet method removes photoresist, and makes photoresist
Complete removal is washed after chemical reaction, reaction of formation thing, micro-pillar array Surface Texture is finally given；
S9, low-surface-energy modification, the carrying tablet that workpiece and drop by secondary eletroforming have silicon fluoride is collectively disposed at
In closed container, it is then placed in 65 DEG C of baking ovens and toasts 1 hour, the preparation that workpiece is completed to room temperature is put after taking-up.
Improved as a kind of the of technical scheme of the preparation method of superoleophobic micro-pillar array Surface Texture of the invention, in step
In S1, metallic substrates smooth to surfacing remove metal surface greasy dirt using alkali lye, are then placed on that to fill ethanol molten
Cleaned in the supersonic wave cleaning machine of liquid, recycle removal of surfactant oxidation on metal surface layer, finally use deionized water
Cleaning is placed in drying in baking oven and removes surface moisture.
Improved as a kind of the of technical scheme of the preparation method of superoleophobic micro-pillar array Surface Texture of the invention, in step
In S6, not exclusively removed photoresist using dry method, carrying out anisotropic dry to workpiece surface using plasma removes photoresist, and makes top layer photoetching
Polymer reaction occurs for glue certain thickness scope, so as to be removed after generating the reactant of effumability.
The beneficial effects of the invention are as follows：Microwell array and then progress once electricity are built by adhering to photoresist in metallic substrates
Cast Cheng Zhishen micro-pillar arrays, then remove part photoresist and expose at the top of microtrabeculae, then carry out at the top of secondary electroforming structure microtrabeculae
Cap body, forms the micro-pillar array of head of a nail shape, so as to build superoleophobic Surface Texture in metal surface.The Surface Texture passes through photoetching
Glue is as assist medium, because photoresist is easy to accurate processing so as to which the Surface Texture built is easy to reach uniform rule and is adapted to
Scale is molded, and uses nickel material electroforming so that micro- texture surface of component has good wearability.
Brief description of the drawings
Fig. 1 shows for a kind of Workpiece structure in each stage of the preparation process of superoleophobic micro-pillar array Surface Texture of the present invention
It is intended to.
Fig. 2 is the dimensional structure diagram for the metallic substrates for being built with Surface Texture.
Embodiment
Embodiments of the present invention are specifically described below in conjunction with the accompanying drawings.
Fig. 1 illustrates the structure in each stage of workpiece in technical process of the invention, a kind of superoleophobic microtrabeculae of the present invention
The preparation method of array surface texture, for building superoleophobic Surface Texture, the superoleophobic micro-pillar array table in metallic substrates
The preparation method of plane texture comprises the following steps：
S1, metallic substrates 1 are cleaned and dried, remove surface and oil contaminant and impurity；So that the surface cleaning of metallic substrates 1
Totally, it is convenient for follow-up texture component technique to carry out so that texture is connected firmly with metallic substrates 1.
S2, photoresist spin coating, front baking, photoresist is positive photoresist, and the positive table of metallic substrates 1 is uniformly spun on by sol evenning machine
Face, then carries out front baking precuring using baking oven to workpiece；So that the photoresist 2 of the sheet of precuring is formed, subsequently in the light
Photoresist 2, which builds vertical core, to be used to build micro-pillar array, therefore the height of the thickness decision micro-pillar array of the photoresist 2.
S3, photoresist exposure, the mask plate 3 with specific pierced pattern is placed in above photoresist, ultraviolet light 4 is passed through
The openwork part of mask plate 3, which is radiated on photoresist 2 to be exposed it, makes it produce photochemical reaction, so that copy mask plate
Pattern is to photoresist 2；By the design to the pattern of mask plate 3, size, pattern, arrangement and close can be obtained on photoresist 2
The different texture of degree, by the control to these parameters, can control the superoleophobic energy in final metal surface.
S4, the development of photoresist and rear baking, the photoresist 2 for replicating mask plate pattern is placed in developer solution, quilt is removed
The photoresist 2 of exposed portion makes to produce the formation micropore battle array of micropore 10 on photoresist up to bottom penetrates its flood photoresist 2
Row；Workpiece is taken out to be placed in after developer solution after baking oven is carried out and dries technique, to its further solidification；So as to be formed with required specific
The straight body microwell array of shape, structure and arranging density.
S5, electroforming of micro-pillar array, using workpiece as negative electrode, nickel block is as anode, respectively with the negative pole of electroforming power supply
It is connected with positive pole, is placed in constituting a complete electroforming system progress electroforming in suitable electroforming liquid pool, after energization, in the moon
Under the domination of pole deposition principle, nickel ion is reduced into metallic nickel in micropore bottom, metallic nickel is filled up all micropores, so as to build
Straight body metal microtrabeculae 5 formation micro-pillar array with required given shape, structure and arranging density.
S6, dry method, which are removed photoresist, removes certain thickness photoresist, all microtrabeculaes 5 is exposed local top ends, after being used for
Continue secondary electroforming.
The secondary electroforming of S7, micro-pillar array, workpiece is placed in electroforming system and carries out secondary electroforming, in negative electrode deposition principle
Under domination, the top of microtrabeculae 5 of protrusion respectively all grows generation electroforming to the nickel ion for equably receiving electroforming, i.e. top surface and periphery
Body so that nickel ion is reduced into the metallic nickel pier block 7 of the hat shape more than the basic root of microtrabeculae at the top of microtrabeculae 5, forms superoleophobic nail
Cap；Pass through process time, electrical parameter（Current density, frequency, dutycycle）With electroforming solution parameter（Temperature and concentration）Deng
Control can obtain the cantilever design of different characteristic size, so as to influence the superoleophobic energy of final workpiece surface.
S8, wet method are removed photoresist completely, workpiece is immersed in into sol solution 8 carries out isotropism wet method and remove photoresist, send out photoresist 2
Complete removal is washed after biochemical reaction, reaction of formation thing, micro-pillar array Surface Texture is finally given, as shown in Figure 2.
S9, low-surface-energy modification, the carrying tablet that the workpiece and drop Jing Guo Electrolyzed Processing have silicon fluoride are collectively disposed at closed
In container, it is then placed in 65 DEG C of baking ovens and toasts 1 hour, the preparation that workpiece is completed to room temperature is put after taking-up.In baking engineering,
Silicon fluoride 9, in the low-surface energy substance of workpiece surface one layer of nano thin-layer of formation, will reach metal surface by suction-operated
Super superoleophobic energy.
The process is formed directly by adhering to photoresist structure microwell array in metallic substrates and then carrying out an electroforming
Body micro-pillar array, then removes part photoresist and exposes at the top of microtrabeculae, then carries out cap body at the top of secondary electroforming structure microtrabeculae, is formed
The micro-pillar array of head of a nail shape, so as to build superoleophobic Surface Texture in metal surface.The Surface Texture is used as auxiliary by photoresist
Help medium, due to photoresist be easy to accurate processing so as to the Surface Texture built is easy to reach uniform rule and be adapted to scale into
Type, nickel metal is used so that surface has good wearability.
More preferably, in step sl, the metallic substrates 1 smooth to surfacing remove metal surface greasy dirt using alkali lye,
Then it is placed in the supersonic wave cleaning machine for fill ethanol solution and is cleaned, recycles removal of surfactant metal surface
Oxide layer, is finally cleaned with deionized water and is placed in drying removal surface moisture in baking oven.So that the surface cleaning of metallic substrates 1 is dry
Net free from admixture non-oxidation layer, is easy in its surface construction micro-pillar array.
More preferably, in step s 6, not exclusively removed photoresist using dry method, utilize plasma or other removal Other substrate materials
Material anisotropic dry carried out to workpiece surface removed photoresist, top layer photoresist certain thickness scope is occurred polymer reaction,
It is removed after reactant so as to generate effumability, after the photoresist for removing certain thickness layer, exposed portion is high at the top of microtrabeculae
Degree is more consistent.
Above disclosed is only the preferred embodiments of the present invention, can not limit the right of the present invention with this certainly
Scope, therefore the equivalent variations made according to scope of the present invention patent, still belong to the scope that the present invention is covered.
Claims (2)
1. a kind of preparation method of superoleophobic micro-pillar array Surface Texture, for building superoleophobic Surface Texture in metallic substrates,
Characterized in that, the preparation method of the superoleophobic micro-pillar array Surface Texture comprises the following steps：
S1, metallic substrates are cleaned and dried, remove surface and oil contaminant and impurity；
S2, photoresist spin coating, front baking, photoresist is positive photoresist, the positive surface of metallic substrates is uniformly spun on by sol evenning machine, so
Front baking precuring is carried out to workpiece using baking oven afterwards；
S3, photoresist exposure, the mask plate with specific pierced pattern are placed in above photoresist, by UV light permeability mask plate
Openwork part irradiation it is exposed its is produced photochemical reaction on a photoresist so that copy mask plate pattern is to light
Photoresist；
S4, the development of photoresist and rear baking, the photoresist for replicating mask plate pattern are placed in developer solution, removal is exposed portion
The photoresist divided, makes to produce microwell array on photoresist；Workpiece is taken out to be placed in after developer solution after baking oven is carried out and dries technique, to it
Further solidification；
S5, electroforming of micro-pillar array, using workpiece as negative electrode, nickel block is as anode, respectively with the negative pole of electroforming power supply and just
Pole is connected, and is placed in constituting a complete electroforming system progress electroforming in suitable electroforming liquid pool, heavy in negative electrode after energization
Under the domination of product principle, nickel ion is reduced into metallic nickel in micropore bottom, metallic nickel is filled up all micropores, produce metal micro-
Post array；
S6, dry method, which are removed photoresist, removes certain thickness photoresist, all microtrabeculaes is exposed local top ends；
The secondary electroforming of S7, micro-pillar array, workpiece is placed in electroforming system and carries out secondary electroforming, in the domination of negative electrode deposition principle
Under, nickel ion is reduced into the metallic nickel pier block of the hat shape more than the basic root of microtrabeculae at the top of microtrabeculae, form superoleophobic head of a nail knot
Structure；
S8, wet method are removed photoresist completely, and workpiece is immersed in into sol solution progress isotropism wet method removes photoresist, and photoresist is occurred chemistry
Complete removal is washed after reaction, reaction of formation thing, micro-pillar array Surface Texture is finally given；
S9, low-surface-energy modification, the carrying tablet that workpiece and drop by secondary eletroforming have silicon fluoride are collectively disposed at closed
In container, it is then placed in 65 DEG C of baking ovens and toasts 1 hour, the preparation that workpiece is completed to room temperature is put after taking-up；
In step sl, the metallic substrates smooth to surfacing remove metal surface greasy dirt using alkali lye, are then placed on
Cleaned in the supersonic wave cleaning machine for filling ethanol solution, recycle removal of surfactant oxidation on metal surface layer, finally
Cleaned with deionized water and be placed in drying removal surface moisture in baking oven.
2. the preparation method of superoleophobic micro-pillar array Surface Texture according to claim 1, it is characterised in that：In step S6
In, not exclusively removed photoresist using dry method, i.e., carrying out anisotropic dry to workpiece surface using plasma removes photoresist, and makes top layer photoetching
Polymer reaction occurs for glue certain thickness scope, so as to be removed after generating the reactant of effumability.
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| CN106048665B (en) * | 2016-07-07 | 2018-04-06 | 广东工业大学 | A kind of method that the superoleophobic compound cast layer of Metal Substrate is prepared using hot compression deformation method |
| CN107574464B (en) * | 2017-08-31 | 2019-05-03 | 华侨大学 | A kind of preparation method with hierarchical structure mushroom-shaped metal column array surface |
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| 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 |
| 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 |
| CN111054918B (en) * | 2019-12-26 | 2021-01-19 | 武汉大学 | Method for accurately preparing superfine metal micro-pillar array suitable for controllable biosensor spacing |
| CN111268640A (en) * | 2020-03-04 | 2020-06-12 | 电子科技大学 | Adaptive super-hydrophobic surface and preparation method thereof |
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| 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 |
| CN115122549B (en) * | 2022-06-22 | 2023-06-16 | 西北工业大学 | Flexible umbrella-shaped microstructure array super-surface and manufacturing method thereof |
| CN115390167A (en) * | 2022-09-02 | 2022-11-25 | 中国科学院上海微系统与信息技术研究所 | Flexible micro-lens array and preparation method thereof |
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| JPH09136422A (en) * | 1995-11-14 | 1997-05-27 | Kyushu Hitachi Maxell Ltd | Method for forming micropore |
| CN1778505A (en) * | 2004-11-19 | 2006-05-31 | 中国科学院高能物理研究所 | Production of extremely profiled fine electrode for processing electric spark |
| CN102020237A (en) * | 2010-03-24 | 2011-04-20 | 江苏大学 | Novel method for designing super oleophobic surface structure |
| CN101817500B (en) * | 2010-03-24 | 2014-04-09 | 江苏大学 | Hydrophilic material surface super hydrophobic functional shift micro structure design method |
| CN104627952B (en) * | 2015-01-13 | 2016-06-22 | 华中科技大学 | A kind of flexible super-hydrophobic superoleophobic structure preparation method |
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