CN105084306A - Controllable preparation method of large-area laminated micro-nano composite structure - Google Patents
Controllable preparation method of large-area laminated micro-nano composite structure Download PDFInfo
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- CN105084306A CN105084306A CN201510459280.7A CN201510459280A CN105084306A CN 105084306 A CN105084306 A CN 105084306A CN 201510459280 A CN201510459280 A CN 201510459280A CN 105084306 A CN105084306 A CN 105084306A
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Abstract
The invention provides a controllable preparation method of a large-area laminated micro-nano composite structure. According to the method, a micro-structure is obtained through photoetching, and a nano-structure is grown through a water bath method. Then a laminated micro-nano composite structure is formed. Through adoption of the ways of photoetching, corrosion and water bath in the method, the preparation of the micro-structure and the preparation of the nano-structure become controllable. Through the method, super hydrophilicity can be achieved by a shape change of a surface structure without surface modification. According to the micro-nano structure prepared through the method, a contact angle at a contact moment is about 15 degrees; full spreading can be realized within 2 seconds; and the contact angle is less than 5 degrees. In the micro-nano structure prepared through the method, the whole contact area can be made to a decimeter scale and even larger as required, so that large-area preparation is realized. The preparation method is low in cost, and a shape-controllable micro-nano composite structure can be obtained. Meanwhile, the preparation method is compatible with a microelectronic process. In combination with a water bath technology, a novel preparation method of the micro-nano composite structure is implemented.
Description
Technical field
The invention belongs to nano surface field of material technology, be specifically related to a kind of controllable method for preparing of large area sheet micro-nano compound structure.
Background technology
People are in the process of observation of nature circle biology, many super hydrophilic blade constructions are found to also exist in plant kingdom, sunglo pineapple and bog moss etc. are by the direct derive nutrients of sclay texture on its surface and water, and moisture can be sprawled by the super water-wet behavior on its surface and evaporate by some tropical plants fast.Conventional ultra-hydrophilic surface of preparing mainly realizes by following two kinds of approach: one, by light-initiated super hydrophilic; Two, by building coarse structure at water-wetted surface.Artificial Control technology can be used, by constructing distinctive micron scale structures to strengthen the roughness on surface at substrate surface, completed the growth of hydrophilic nano structure afterwards by certain manufacturing process, the super hydrophilic micro-nano compound structure surface with Superhydrophilic, automatic cleaning action and rapid draing feature can be prepared.
Relative to super hydrophobic material, the research of super water wetted material aspect is relatively less, but ultra-hydrophilic surface also has unique advantage, resistance to fogging, rapid draing etc., in addition, super water wetted material is fixed in heat trnasfer, biomolecule and is also had potential application in drag reduction etc.As the typical interfacial phenomenon of one, the research of surface wettability is in again the aspects such as surface chemistry, physics, materialogy, biology to be had high research and explores value.
The technology preparing inorganic matter ultra-hydrophilic surface at present mainly contains collosol and gel, oxidation-reduction method, phase separation method, hydro-thermal method, plasma technique, the methods such as electrochemical deposition, but, although said method is with low cost, the micro-nano compound structure morphology controllable obtained is too poor, technique and the more difficult control of micro-nano structure dimensional stability.
Summary of the invention
Based on problems of the prior art, the invention provides a kind of controllable method for preparing of large area sheet micro-nano compound structure, make the preparation process of micro-nano compound structure controlled, and the sheet micro-nano compound structure of area stable existence can be prepared.
In order to solve the problems of the technologies described above, the application adopts following technical scheme to be achieved:
A controllable method for preparing for large area sheet micro-nano compound structure, the method lithographically obtains micrometer structure, by immersion method growth of nanostructures, forms sheet micro-nano compound structure.
The present invention also has and distinguishes technical characteristic as follows:
Described micro-nano compound structure is using aluminium flake as matrix.
During described formation sheet micro-nano compound structure, by mode growth of nanostructures on micrometer structure of first photoetching water-bath again; Or corroded again by first photoetching, mode growth of nanostructures on micrometer structure of last water-bath; Or by first water-bath, then photoetching, the mode of final etching forms micrometer structure on the nanostructure.
The NaOH solution of the corrosive liquid of described corrosion to be concentration be 5wt%.
After described photoetching completes, during photoresist demoulding cleaning, make stripper with photoresist, at 80 DEG C, ultrasonic process 15min; Then with after deionized water rinsing, acetone normal temperature ultrasonic process 10min is adopted, removal photoresist stripper, ethanol purge, then with deionized water normal temperature ultrasonic process 10min.
The detailed process of described immersion method is: sample is put into water-bath and heats poach, and under bath temperature is 80 DEG C ~ 100 DEG C conditions, lasting water bath time is not less than 1h.
Compared with prior art, useful technique effect is in the present invention:
This method adopts the mode of photoetching, corrosion and water-bath, makes the preparation of the preparation of micrometer structure and nanostructured all reach controlled; Micro-nano structure prepared by this method, Contact contact angle about 15 °, can sprawl in 2s completely, and contact angle is less than 5 °, and this method is without the need to carrying out finishing, and the pattern by means of only surface texture changes just can obtain Superhydrophilic.Micro-nano structure prepared by this method, total area can be accomplished decimeter grade as required, even more greatly, realize large area preparation.This preparation method's cost is comparatively cheap, can obtain the micro-nano compound structure of morphology controllable, and this preparation method is mutually compatible with microelectronic technique simultaneously, in conjunction with water-bath technology, completes a kind of new method prepared for micro-nano compound structure.
Accompanying drawing explanation
Fig. 1 is micrometer structure top view.
Fig. 2 is the profile of micro-nano compound structure in example 1.
Fig. 3 is the profile of micro-nano compound structure in example 2.
Fig. 4 is the profile of micro-nano compound structure in example 3.
Multiplication factor when Fig. 5 is a=10 μm is the SEM figure of 1.10K.
Multiplication factor when Fig. 6 is a=10 μm is the SEM figure of 60.0K.
Micro-nano compound structure Contact contact angle resolution chart in example 1 when Fig. 7 is a=10 μm.
Below in conjunction with drawings and Examples, particular content of the present invention is described in more detail.
Detailed description of the invention
Defer to technique scheme, below provide specific embodiments of the invention, it should be noted that the present invention is not limited to following specific embodiment, all equivalents done on technical scheme basis all fall into protection scope of the present invention.Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1:
The present embodiment provides a kind of controllable method for preparing of large area sheet micro-nano compound structure, carries out according to following steps:
Step one: make mask plate:
The structural parameters of microarray are made to be respectively a=5 μm, a=10 μm, a=15 μm, a=20 μm by the design of mask plate.
Step 2: photoetching:
Photoetching is carried out, by the graph copying of mask plate on the photoresist on high-purity polished aluminum surface, as shown in Figure 1 by techniques such as even glue, front baking, exposure, development, rear bakings.
Photoresist model is SU8-1070 photoresist, and carries out diluting (SU8: diluent=1:3).Even adhesive tape part is: low speed 600r/s continues 10s, and high speed 4000r/s continues 30s; Front baking condition is: hot plate 85 DEG C, dries 25 ~ 30min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm2; Time for exposure, 10s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 85 DEG C are dried 15min.
Photoresist model also can select the photoresist of other models, as BN303 photoresist.Front baking condition is: hot plate 85 DEG C, and hot plate dries 3min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm
2; Time for exposure, 1s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 135 DEG C are dried 15min.
Step 3, corrosion:
Carry out wet etching by the NaOH solution that concentration is 5wt%, or adopt dry etching, that is, the method such as reactive ion beam etching (RIBE) RIE, sense coupling ICP.Corrosion depth is h, obtains micrometer structure.
Step 4, the photoresist demoulding is cleaned:
Step 4.1, makes stripper with photoresist, at 80 DEG C, and ultrasonic process 15min;
Step 4.2, after deionized water rinsing, adopts acetone normal temperature ultrasonic process 10min, removal photoresist stripper, ethanol purge, then with deionized water normal temperature ultrasonic process 10min.
Step 5, immersion method:
Step 5.1, puts into water-bath and uses deionized water heating poach by sample;
Step 5.2, under bath temperature is 80 DEG C ~ 100 DEG C conditions, lasting water bath time is not less than 1h; Repeatedly, 80 DEG C of oven dry, obtain the micro-nano compound structure based on aluminium flake, section of structure as shown in Figure 2 for deionized water rinsing.SEM figure under different amplification as shown in Figure 5 and Figure 6, obviously can find out that from figure the micro-nano compound structure of the application is sheet.Micro-nano compound structure Contact contact angle resolution chart when Fig. 7 is a=10 μm, as can be seen from the figure, Contact contact angle about 15 °, can sprawl in 2s completely, and contact angle is less than 5 °.
Embodiment 2:
The present embodiment provides a kind of controllable method for preparing of large area sheet micro-nano compound structure, carries out according to following steps:
Step one: make mask plate:
The structural parameters of microarray are made to be respectively a=5 μm, a=10 μm, a=15 μm, a=20 μm by the design of mask plate.
Step 2: photoetching:
Photoetching is carried out, by the graph copying of mask plate on the photoresist on high-purity polished aluminum surface, as shown in Figure 1 by techniques such as even glue, front baking, exposure, development, rear bakings.
Photoresist model is SU8-1070 photoresist, and carries out diluting (SU8: diluent=1:3).Even adhesive tape part is: low speed 600r/s continues 10s, and high speed 4000r/s continues 30s; Front baking condition is: hot plate 85 DEG C, dries 25 ~ 30min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm2; Time for exposure, 10s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 85 DEG C are dried 15min.
Photoresist model also can select the photoresist of other models, as BN303 photoresist.Front baking condition is: hot plate 85 DEG C, and hot plate dries 3min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm
2; Time for exposure, 1s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 135 DEG C are dried 15min.
Step 3, corrosion:
The present embodiment does not carry out etching process.
Step 4, immersion method:
Step 4.1, puts into water-bath and uses deionized water heating poach by sample;
Step 4.2, under bath temperature is 80 DEG C ~ 100 DEG C conditions, lasting water bath time is not less than 1h; Repeatedly, 80 DEG C of oven dry, obtain the micro-nano compound structure based on aluminium flake, section of structure as shown in Figure 3 for deionized water rinsing.
Step 5, the photoresist demoulding is cleaned:
Step 5.1, makes stripper with photoresist, at 80 DEG C, and ultrasonic process 15min;
Step 5.2, adopts acetone with after deionized water rinsing, normal temperature ultrasonic process 10min, removes photoresist stripper, ethanol purge, then with deionized water normal temperature ultrasonic process 10min.
Embodiment 3:
The present embodiment provides a kind of controllable method for preparing of large area sheet micro-nano compound structure, carries out according to following steps:
Step one, immersion method:
Step 1.1, puts into water-bath and uses deionized water heating poach by sample;
Step 1.2, under bath temperature is 80 DEG C ~ 100 DEG C conditions, lasting water bath time is not less than 1h; Repeatedly, 80 DEG C of oven dry, obtain the nanostructured based on aluminium flake to deionized water rinsing.
Step 2: make mask plate:
The structural parameters of microarray are made to be respectively a=5 μm, a=10 μm, a=15 μm, a=20 μm by the design of mask plate.
Step 3: photoetching:
Photoetching is carried out, by the graph copying of mask plate on the photoresist on high-purity polished aluminum surface, as shown in Figure 1 by techniques such as even glue, front baking, exposure, development, rear bakings.
Photoresist model is SU8-1070 photoresist, and carries out diluting (SU8: diluent=1:3).Even adhesive tape part is: low speed 600r/s continues 10s, and high speed 4000r/s continues 30s; Front baking condition is: hot plate 85 DEG C, dries 25 ~ 30min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm2; Time for exposure, 10s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 85 DEG C are dried 15min.
Photoresist model also can select the photoresist of other models, as BN303 photoresist.Front baking condition is: hot plate 85 DEG C, and hot plate dries 3min; Exposure: exposure machine power 11.5 ~ 12.5mw/cm
2; Time for exposure, 1s; Development: developing time, 60s; Rinsing: rinsing time, 60s; Post bake: 135 DEG C are dried 15min.
Step 4, corrosion:
Carry out wet etching by the NaOH solution that concentration is 5wt%, corrosion depth is h, obtains the micro-nano compound structure based on aluminium flake, and section of structure as shown in Figure 4.
Step 5, the photoresist demoulding is cleaned:
Step 5.1, makes stripper with photoresist, at 80 DEG C, and ultrasonic process 15min;
Step 5.2, adopts acetone with after deionized water rinsing, normal temperature ultrasonic process 10min, removes photoresist stripper, ethanol purge, then with deionized water normal temperature ultrasonic process 10min.
Claims (6)
1. a controllable method for preparing for large area sheet micro-nano compound structure, is characterized in that: the method lithographically obtains micrometer structure, by immersion method growth of nanostructures, forms sheet micro-nano compound structure.
2. the method for claim 1, is characterized in that: described micro-nano compound structure is using aluminium flake as matrix.
3. the method for claim 1, is characterized in that: during described formation sheet micro-nano compound structure, by mode growth of nanostructures on micrometer structure of first photoetching water-bath again; Or corroded again by first photoetching, mode growth of nanostructures on micrometer structure of last water-bath; Or by first water-bath, then photoetching, the mode of final etching forms micrometer structure on the nanostructure.
4. method as claimed in claim 3, is characterized in that: the NaOH solution of the corrosive liquid of described corrosion to be concentration be 5wt%.
5. the method for claim 1, is characterized in that: after described photoetching completes, and during photoresist demoulding cleaning, makes stripper with photoresist, at 80 DEG C, and ultrasonic process 15min; Then with after deionized water rinsing, acetone normal temperature ultrasonic process 10min is adopted, removal photoresist stripper, ethanol purge, then with deionized water normal temperature ultrasonic process 10min.
6. the method for claim 1, is characterized in that: the detailed process of described immersion method is: sample is put into water-bath and heats poach, and under bath temperature is 80 DEG C ~ 100 DEG C conditions, lasting water bath time is not less than 1h.
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Cited By (3)
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| CN106185792A (en) * | 2016-07-22 | 2016-12-07 | 西北工业大学 | A kind of population parameter controllable method for preparing of super-hydrophobic micro-nano compound structure |
| CN111204702A (en) * | 2019-07-11 | 2020-05-29 | 浙江精筑环保科技有限公司 | Method for selectively and controllably preparing nano-silver structure on surface of copper sheet |
| CN112934282A (en) * | 2021-03-26 | 2021-06-11 | 西北大学 | Self-feedback high-flux microfluidic system and method |
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| CN104445054A (en) * | 2014-12-30 | 2015-03-25 | 西安建筑科技大学 | Self-cleaning film preparation method |
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| CN101225510A (en) * | 2008-01-11 | 2008-07-23 | 东华大学 | Plasma preparation method of super-hydrophobic and super-hydrophilic titanium oxide film |
| CN102154672A (en) * | 2008-04-09 | 2011-08-17 | 北京航空航天大学 | Non-metallic film with high heat conduction efficiency and anti-fouling capability and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106185792A (en) * | 2016-07-22 | 2016-12-07 | 西北工业大学 | A kind of population parameter controllable method for preparing of super-hydrophobic micro-nano compound structure |
| CN111204702A (en) * | 2019-07-11 | 2020-05-29 | 浙江精筑环保科技有限公司 | Method for selectively and controllably preparing nano-silver structure on surface of copper sheet |
| CN111204702B (en) * | 2019-07-11 | 2023-03-28 | 浙江精筑环保科技有限公司 | Method for selectively and controllably preparing nano-silver structure on surface of copper sheet |
| CN112934282A (en) * | 2021-03-26 | 2021-06-11 | 西北大学 | Self-feedback high-flux microfluidic system and method |
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