CN104627952B - A kind of flexible super-hydrophobic superoleophobic structure preparation method - Google Patents
A kind of flexible super-hydrophobic superoleophobic structure preparation method Download PDFInfo
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Abstract
The invention discloses a kind of flexible super-hydrophobic superoleophobic structure preparation method, this preparation method comprises the steps: that (1) makes flexible super-hydrophobic superoleophobic structure bottom: one layer of negative photoresist of spin coating in substrate, is exposed without mask；(2) one layer of negative photoresist of spin coating on the negative photoresist after step (1) exposes, utilizes array pattern mask to be exposed；(3) structure sheaf photoresist second time exposure: adopt the mask with step (2) is corresponding to carry out alignment exposure；(4) development: the structure after exposure in above-mentioned steps is developed；(5) plating film: the body structure surface obtained in step (4) forms layer protecting film；(6) peel off: the structure that will obtain after step (5) processes is peeled off from substrate, obtains the super-hydrophobic superoleophobic structure of described flexibility。According to the preparation method of the present invention, technique is simple, with low cost, and the popularization and application of the super-hydrophobic superoleophobic structure of this flexibility is had the effect of greatly facilitating。
Description
Technical field
The invention belongs to field of micro-Na manufacture, more particularly, to a kind of flexible super-hydrophobic superoleophobic structure preparation technology。
Background technology
Super hydrophobic material is one of focus of Recent study, and the structure and material preparing super hydrophobic surface emerges in an endless stream。The hydrophobic principle of super hydrophobic material mainly makes liquid be in Cassie-Baxter state at micro-structure surface, namely liquid level can be held by surface micro-structure and air and incomplete contact between to the surface of solids, as it is shown in figure 1, drop suspends in surface of solids micro structure。The surface being under Cassie-Baxter state has superhydrophobic characteristic, and roll angle is only small, and drop is easy to tumble from surface, thus has automatically cleaning effect。Existing super hydrophobic surface is mainly Fig. 1 (a) and the structure shown in Fig. 1 (b), and θ is the liquid intrinsic hydrophobic angle at the surface of solids。Column structure in Fig. 1 (a) requires θ > 90 °, and namely material itself has hydrophobic property, prepares the surface after this structure and just has ultra-hydrophobicity。Structure in Fig. 1 (b) can allow less θ value, but must also is fulfilled for θ > 30 °。, there is certain allowed band on the surface of preparation both the above structure to drop intrinsic contact angle, and super-hydrophobic superoleophobic " super-amphiphobic " surface, it is desirable to water and oil are had bigger contact angle by material simultaneously, seldom have this characteristic in existing material。And the structure shown in Fig. 1 (c), super-hydrophobic superoleophobic characteristic is still possessed when θ=0, the hydrophobic oleophobic characteristic of this body structure surface is unrelated with material, suitable in any material, and all liq (including water and oil) all can be easy on its surface tumble in theory, thus there is application prospect widely。
And prepare the structure shown in Fig. 1 (c), the technical process existed in prior art is extremely complex, the techniques such as photoetching, sense coupling, wet method silicon etching, thermal oxidation silicon plated film need to be used, the equipment used is much more expensive, costly, technology difficulty is big, and the structure prepared in fashion described above does not have flexibility, bring bottleneck thus to the generally utilization of this structure, therefore, a kind of with low cost, simply flexible super-hydrophobic superoleophobic structural manufacturing process method of technique of exploitation it is badly in need of。
Summary of the invention
For disadvantages described above or the Improvement requirement of prior art, the invention provides the preparation technology of a kind of super-hydrophobic superoleophobic structure, the preparation method that its object is to the super-hydrophobic superoleophobic structure providing technique simple and with low cost。
The preparation method that the invention provides the super-hydrophobic superoleophobic structure of a kind of flexibility, it is characterised in that this preparation method comprises the steps:
(1) make flexible super-hydrophobic superoleophobic structure bottom: one layer of negative photoresist of spin coating in substrate, directly expose without mask and make photochemical reaction region and retain and become bottom；
(2) structure sheaf photoresist first time exposure: in the described step (1) on negative photoresist after exposure again one layer of negative photoresist of spin coating as in structure sheaf, array pattern mask is utilized to be exposed, photochemically reactive region corresponding in unit figure in described array pattern mask is: internal circular for printing opacity, and outside is printing opacity annular；
(3) structure sheaf photoresist second time exposure: adopt and carry out alignment exposure with printing opacity circular array mask corresponding in described step (2), namely corresponding in the unit figure of described mask photochemically reactive region is: the region between inner circular and outer annular, and uses less exposure dose to make the photochemically reactive degree of depth of generation lower than the annular region photochemical reaction degree of depth；
(4) development: the structure obtained after exposure in above-mentioned steps is developed；
(5) plating film: the body structure surface obtained in described step (4) forms layer protecting film；
(6) peel off: the photoresist structure with matcoveredn film that will obtain after described step (5) processes is peeled off from substrate, obtains the super-hydrophobic superoleophobic structure of described flexibility。
Further, the thickness of the bottom photoresist in described step (1) is 5～100 μm。
Further, in described step (2), the thickness of the photoresist of spin coating is 10～50 μm。
Further, the centre-to-centre spacing between the array pattern of the mask in described step (2) is 15～100 μm。
Further, the diameter of the inner circular of the array pattern mask in described step (2) is 3～20 μm, and the diameter of the outmost turns of outer annular is 10～50 μm, and the width of annular is 0.5～2 μm。
Further, the exposure dose of described step (3) makes the photochemically reactive degree of depth be 1～5 μm。
Further, the structure sheaf photoresist of described step (2) and (3) is preferably SU8 photoresist
The preparation method that the invention allows for a kind of super-hydrophobic superoleophobic material, it is characterised in that super-hydrophobic for the flexibility prepared by the preparation method in described step 1-6 superoleophobic structure is mounted on material surface, thus makes super-hydrophobic superoleophobic material。
In general, by the contemplated above technical scheme of the present invention compared with prior art, owing to present invention employs new material and preparation method produces the super-hydrophobic superoleophobic structure of complexity, it is possible to obtain following beneficial effect:
(1) present invention takes full advantage of in the feature of negative photoresist and photoetching process by controlling the exposure dose control photochemical reaction degree of depth, adopts the method that multiexposure, multiple exposure once develops, and technical process is very simple；
(2) present invention takes full advantage of the diffraction effect of narrow annulus during contact exposure, is prepared the three dimensional structure of complexity by the regional extent (i.e. photochemical reaction regional extent) being exposed in the width control system photoresist of narrow annulus；
(3) process costs of the present invention is cheap, and the super-hydrophobic superoleophobic structure produced by which is flexible structure, and can facilitate to stick to the surface of material, has using value widely。
Accompanying drawing explanation
Fig. 1 is three kinds of forms of several super hydrophobic surface micro structure being in Cassie-Baxter state of the prior art, (a) column, and (b) is "T"-shaped, (c) super-hydrophobic superoleophobic structure；
Fig. 2 (a) is the mask pattern used according to the structure sheaf photoresist first time exposure in the preparation method in the present invention；
Fig. 2 (b) exposes the optical field distribution sectional view below the mask pattern used according to the structure sheaf photoresist first time in the preparation method in the present invention；
Fig. 3 is according to the mask array arrangement schematic diagram in the preparation method of the present invention；
Fig. 4 is the process flow diagram of the preparation method according to the present invention。
In all of the figs, identical accompanying drawing labelling is used for representing identical element or structure, wherein:
Exposure area 6-structure sheaf second time exposure area 7-corresponding to exposure area (photochemical reaction region) 5-central circular corresponding to 1-bottom photoresist 2-substrate 3-structure sheaf photoresist 4-outer annular protects tunic
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated。Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention。As long as just can be mutually combined additionally, technical characteristic involved in each embodiment of invention described below does not constitute conflict each other。
The present invention is the lithography performance utilizing negative photoresist, the material of negative photoresist is directly adopted to form super-hydrophobic superoleophobic structure, below in an example, mainly have employed SU8 negative photoresist, but other negative photoresists can also be adopted in principle, and carry out similar operation at mask with steps such as developments, do not repeat them here。
SU8 photoresist is a kind of negative photoresist conventional in semiconductor applications, and namely after exposure imaging, cross-linking reaction (photochemical reaction) occurs in the region of exposure, and unexposed region can be removed by developed liquid after development。SU8 photoresist has very excellent performance, it is possible to the structure that preparation depth-to-width ratio significantly high (depth-to-width ratio is up to 50:1), sidewall edge are vertical, and technological parameter is very sensitive。Owing to SU8 photoresist general thickness is bigger, the exposure intensity of top layer photoresist is bigger than the photoresist of bottom, when exposure dose is inadequate, cross-linking reaction (being namely exposed) can be there is in the photoresist on top layer, and the photoresist of bottom does not reach required exposure dose and can get rid of by developed liquid, it is easy to cause photoresist structure to come off。But utilize this characteristic of SU8 photoresist, it is possible to prepare suspension structure by controlling the dosage of exposure。Other negative photoresists with identical characteristics are equally applicable to the process in the present invention, for instance also have NR26-25000P photoresist。Especially, as long as bottom photoresist negative photoresist, it does not have particular/special requirement, technical process only serves the effect connecting and supporting, it is possible to structure sheaf photoresist is identical can also be different。
In contact photolithography process, when the yardstick of mask graph is close to exposure light source wavelength, diffraction can clearly, and along with the distance from mask graph increases, the intensity of light field can die down gradually。As shown in Figure 2, Fig. 2 (a) is mask graph schematic diagram, dash area is transmission region, when center, printing opacity border circular areas diameter is 10 microns, the width of peripheral circles shape transmission region is 1 micron, when optical wavelength is 365nm, under mask, the optical field distribution of square section is such as shown in Fig. 2 (b)。It will be seen that the light field below the printing opacity border circular areas of center can keep good column, and below narrow annulus transmission region, diffraction of light is very serious, and optical field distribution increases along with distance and weakens gradually。Utilize this feature of narrow annulus printing opacity mask graph, it is possible on thicker negative photoresist, prepare the three dimensional structure of complexity。
In present embodiment, namely the preparation method of labyrinth is based on the feature of above-mentioned negative photoresist and the diffraction of photoetching process Small and Medium Sized figure, adopt the method once developed of multiexposure, multiple exposure, have with low cost, technique is simple, super-hydrophobic superoleophobic characteristic。
Embodiment one
(1) exposure bottom photoresist: one layer of SU-82000 photoresist of spin coating in substrate, thickness is 5 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of SU-82000 photoresist of spin coating on the SU-82000 photoresist after exposing in step (1), thickness is 10 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 3 μm, and the diameter of outer annular outmost turns is 10 μm, and the width of annular is 0.5 μm, and the centre-to-centre spacing between array pattern is 15 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 1 μm of top layer will not developed fall；Wherein the circular mask pattern distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask pattern is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the methods such as plated film, dip-coating, collosol and gel to produce layer protecting film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film obtained in step (5) is peeled off, obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment two
(1) exposure bottom photoresist: one layer of NR26-25000P of spin coating in substrate, thickness is 10 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of SU-8GM1070 of spin coating on the SU-8GM1070 after exposing in step (1), thickness is 12 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 6 μm, and outer annular diameter is 10 μm, and the width of annular is 0.8 μm, and the centre-to-centre spacing between array pattern is 30 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 1.5 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method sputtering gold-plated film to produce layer protective layer gold film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment three
(1) exposure bottom photoresist: one layer of NR26-25000P photoresist of spin coating in substrate, thickness is 20 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of NR26-25000P photoresist of spin coating on the NR26-25000P photoresist after exposing in step (1), thickness is 18 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 9 μm, and outer annular diameter is 20 μm, and the width of annular is 1 μm, and the centre-to-centre spacing between array pattern is 42 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 2 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method for sputtering applying silicon oxide to produce layer protective layer silicon dioxide film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment four
(1) exposure bottom photoresist: one layer of SU-82000 of spin coating in substrate, thickness is 40 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of SU-82000 of spin coating on the SU-82000 after exposing in step (1), thickness is 26 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 12 μm, and outer annular diameter is 30 μm, and the width of annular is 1.2 μm, and the centre-to-centre spacing between array pattern is 65 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 2.8 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method for sputtering applying silicon oxide to produce layer protective layer silicon dioxide film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment five
(1) exposure bottom photoresist: one layer of NR26-25000P of spin coating in substrate, thickness is 60 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of SU-8GM1070 of spin coating on the SU-8GM1070 after exposing in step (1), thickness is 34 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 15 μm, and outer annular diameter is 40 μm, and the width of annular is 1.5 μm, and the centre-to-centre spacing between array pattern is 75 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 3.2 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method for sputtering applying silicon oxide to produce layer protective layer silicon dioxide film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment six
(1) exposure bottom photoresist: one layer of NR26-25000P photoresist of spin coating in substrate, thickness is 80 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of NR26-25000P photoresist of spin coating on the NR26-25000P photoresist after exposing in step (1), thickness is 40 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 18 μm, and outer annular diameter is 50 μm, and the width of annular is 1.8 μm, and the centre-to-centre spacing between array pattern is 90 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 4.5 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method for sputtering applying silicon oxide to produce layer protective layer silicon dioxide film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
Embodiment seven
(1) exposure bottom photoresist: one layer of NR26-25000P photoresist of spin coating in substrate, thickness is 100 μm, is exposed without mask；
(2) structure sheaf photoresist first time exposure: one layer of NR26-25000P photoresist of spin coating on the NR26-25000P photoresist after exposing in step (1), thickness is 50 μm, is exposed；Adopting array pattern mask as shown in Figure 3 during exposure, wherein inner circular diameter is 20 μm, and outer annular diameter is 50 μm, and the width of annular is 2 μm, and the centre-to-centre spacing between array pattern is 100 μm；
(3) structure sheaf photoresist second time exposure: adopt the mask of the printing opacity circular array corresponding with step (2) to carry out alignment exposure, use less exposure dose so that only the photoresist generation cross-linking reaction on 5 μm of top layer will not developed fall；Wherein the circular mask graph distribution adopted with step (2) of printing opacity is unanimously, and diameter is identical with outer annular regions diameter, and during alignment exposure, mask graph is with the pattern alignment exposed in step (2)；
(4) development: the print after step (3) being exposed develops, and obtains the shape such as array of structures shown in Fig. 1 (c)；
(5) plating film: adopt the method for sputtering applying silicon oxide to produce layer protective layer silicon dioxide film on the body structure surface that step (4) obtains；
(6) peel off: the photoresist structure with matcoveredn film step (5) obtained is peeled off, and obtains the super-hydrophobic superoleophobic structure of required flexibility。
According to the super-hydrophobic superoleophobic material of flexibility that the present embodiment prepares, due to the particularity in its material and structure, the surface of various material can be mounted on so that these materials become super-hydrophobic superoleophobic material, these materials are specifically as follows the smooth surfaces such as glass, quartz, metal, pottery, it is also possible to for flexible organic polymer surfaces such as PDMS (polydimethylsiloxane), PMMA (polymethyl methacrylate)。
Those skilled in the art will readily understand; the foregoing is only presently preferred embodiments of the present invention; not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention。
Claims (8)
1. the preparation method of the super-hydrophobic superoleophobic structure of flexibility, it is characterised in that this preparation method comprises the steps:
(1) making flexible super-hydrophobic superoleophobic structure bottom: one layer of negative photoresist of spin coating in substrate, directly exposure makes the reservation of photochemical reaction region becomes bottom；
(2) structure sheaf photoresist first time exposure: in the described step (1) on negative photoresist after exposure again one layer of negative photoresist of spin coating as structure sheaf photoresist, array pattern mask is utilized to be exposed, photochemically reactive region corresponding in unit figure in described array pattern mask is: internal circular for printing opacity, and outside is printing opacity annular；
(3) structure sheaf photoresist second time exposure: adopt and carry out alignment exposure with printing opacity circular array mask corresponding in described step (2), namely corresponding in the unit figure of described mask photochemically reactive region is: the region between inner circular and outer annular, and uses less exposure dose to make the photochemically reactive degree of depth photochemical reaction degree of depth lower than annular region of generation；
(4) development: the structure obtained after exposure in above-mentioned steps is developed；
(5) plating film: the body structure surface obtained in described step (4) forms layer protecting film；
(6) peel off: the photoresist structure with matcoveredn film that will obtain after described step (5) processes is peeled off from substrate, obtains the super-hydrophobic superoleophobic structure of described flexibility。
2. the preparation method of flexible super-hydrophobic superoleophobic structure as claimed in claim 1, it is characterised in that the thickness of the bottom photoresist in described step (1) is 5～100 μm。
3. the preparation method of flexible super-hydrophobic superoleophobic structure as claimed in claim 2, it is characterised in that in described step (2), the thickness of the photoresist of spin coating is 10～50 μm。
4. the preparation method of flexible super-hydrophobic superoleophobic structure as claimed in claim 3, it is characterised in that the centre-to-centre spacing between the array pattern of the mask in described step (2) is 15～100 μm。
5. the preparation method of flexible super-hydrophobic superoleophobic structure as described in claim 4, it is characterized in that, the diameter of the inner circular of the array pattern mask in described step (2) is 3～20 μm, the diameter of the outmost turns of outer annular is 10～50 μm, and the width of annular is 0.5～2 μm。
6. the preparation method of flexible super-hydrophobic superoleophobic structure as claimed in claim 5, it is characterised in that the exposure dose of described step (3) makes the photochemically reactive degree of depth be 1～5 μm。
7. the preparation method of the super-hydrophobic superoleophobic structure of flexibility as described in any one in claim 1-6, it is characterised in that the structure sheaf photoresist of described step (2) and (3) is SU8 photoresist。
8. the preparation method of a super-hydrophobic superoleophobic material, it is characterised in that super-hydrophobic for the flexibility prepared by the preparation method described in any one in claim 1-7 superoleophobic structure dress is affixed on material surface, thus makes super-hydrophobic superoleophobic material。
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| CN105480939A (en) * | 2015-12-03 | 2016-04-13 | 中国科学院物理研究所 | Preparation method of three-dimensional structure with liquid full super-hydrophobic function |
| CN106433545B (en) * | 2016-09-08 | 2019-08-13 | 中国科学院深圳先进技术研究院 | A kind of ultraviolet cured adhesive, preparation method and application |
| CN108017035A (en) * | 2016-10-28 | 2018-05-11 | 中国科学院深圳先进技术研究院 | A kind of bionic gecko dry glue and preparation method thereof |
| CN108134208B (en) * | 2017-12-18 | 2020-11-24 | 中国科学院长春光学精密机械与物理研究所 | Method for manufacturing composite patch type curved surface frequency selection surface array |
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