CN107416765A - The method that nano concavo-convex structure is formed in plane or curved surface - Google Patents
The method that nano concavo-convex structure is formed in plane or curved surface Download PDFInfo
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- CN107416765A CN107416765A CN201710469398.7A CN201710469398A CN107416765A CN 107416765 A CN107416765 A CN 107416765A CN 201710469398 A CN201710469398 A CN 201710469398A CN 107416765 A CN107416765 A CN 107416765A
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- curved surface
- convex structure
- plane
- polystyrene microsphere
- nano concavo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
Abstract
The present invention relates to a kind of method that nano concavo-convex structure is formed in plane or curved surface, comprise the following steps：Polystyrene microsphere is formed into monomolecular film by gas-liquid interface self-assembly method；Using vertical czochralski method, monomolecular film is transferred in substrate, then etches monomolecular film, the polystyrene microsphere size in monomolecular film is diminished, forms substrate expose portion；Continue to etch substrate expose portion, form nano concavo-convex structure.Using the method for the present invention, rigid plane or flexible curved surface can be handled, preparation technology is simple, controllability is high, cost is low, has broad application prospects preparing the fields such as the optics with micro-nano structure, sensor, photovoltaic device, luminescent device.
Description
Technical field
The present invention relates to optics preparing technical field, more particularly to one kind to form nano concavo-convex in plane or curved surface
The method of structure.
Background technology
At present, many micro-nano technology technologies can be realized prepares patterned nanostructure on planar substrate surface, still
These technologies are not suitable for nonplanar substrate surface mostly.Laser writing technology not only can in the plane but also can be complicated bent
Micro-nano structure is made on face, but the technical costs is very high, and efficiency is low, and can only make the structure of micron order yardstick.Nanometer pressure
Micro-nano structure pattern can be transferred to planar substrate surface by print technology, in theory can be real by splicing on complex-curved
It is existing, but the accurate control for stitching error has very big difficulty.
Prepared on curved surface and complex topography surface nanostructured be artificial compound eye, flexible photovoltaic devices, luminescent device,
The technology of the optics field such as hemispherical electronic eyes camera, image sensor array and fibre optical sensor most critical.For example,
Microlens array is made on lens can manufacture compound eye camera, make it have 160 degree of the visual field, and can focus on simultaneously
The different depth of object.Nano concavo-convex array is made in flexible photovoltaic or luminescent device can be used as light adjusted and controlled, promote
The absorption or extraction of light, so as to greatly improve device performance.Therefore need that a kind of cost of exploitation is cheap, nano junction of reliable in quality badly
Preparation Method is configured, it is applied to the processing of plane or curved surface.
The Chinese patent of Application No. 201310551957.0 discloses one kind and utilizes soft nano-imprint stamp combination wet method
The method that metal pattern is prepared on curved surface is etched, layer of metal is deposited on curved surface first, then passes through transfer on metal
Method imprinted pattern, carved by the method for reactive ion etching after removing remnant layer, metal carved as mask using imprinting glue
Erosion is to substrate, then the impressing glue with reactive ion etching removing metal pattern upper strata, obtains metal pattern.This method is mainly used in
Patterned process is carried out to substrate, it is necessary to be etched repeatedly, process is more complicated.And the polydimethylsiloxanes used in method
Alkane soft template is difficult to seamless fitting and uniformly applies pressure, therefore is difficult to be imprinted on complex-curved.
The Chinese patent of Application No. 201610855702.7 discloses one kind and uses Computerized three-dimensional reconstructed surface object
Surface, the method that then making thermoplasticity shape-memory polymer stamp matching body surface is imprinted manufacture micro- on curved surface
Micro-nano structure.This method overcomes the problem of impression block and application of a surface to a certain extent, but each template can only correspond to
A kind of curved surface, flexibility are poor.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide one kind to form nano concavo-convex knot in plane or curved surface
The method of structure, this method is applied to rigid plane or the micro-nano structure of flexible curved surface makes, and preparation technology is simple, controllability
Height, cost are low.
The invention provides a kind of method that nano concavo-convex structure is formed in plane or curved substrate, including following step
Suddenly：
(1) polystyrene microsphere is formed into monomolecular film by gas-liquid interface self-assembly method；
(2) vertical czochralski method is utilized, monomolecular film is transferred in substrate, then etches monomolecular film, makes monomolecular film
In polystyrene microsphere size diminish, formed substrate expose portion；The surface of substrate is in plane or curved-surface structure；
(3) continue to etch substrate expose portion, residual polystyrene microsphere is washed off, forms nano concavo-convex structure.
Further, in step (1), the particle diameter of polystyrene microsphere is 200-3000nm.Further, in step
(1) in, gas-liquid interface self-assembly method comprises the following steps：
Carrier with hydrophilic surface is placed in water, the ethanol solution of instillation polystyrene microsphere into water, then to
Surfactant is wherein added, forms monomolecular film；Wherein, carrier provides planar support for polystyrene microsphere.Carrier is silicon
Piece or cover glass；Alcohol is ethanol, and surfactant is lauryl sodium sulfate.
Due to the diffusion of ethanol and the surface tension of water, polystyrene microsphere can form single layer structure, between microballoon
Stronger adelphotaxy makes it spontaneously form ordered arrangement.The ordered arrangement completely can easily be transferred to arbitrary shape
Substrate on, provide possibility for follow-up micro-nano technology.
Further, in step (2), substrate is flexible curved surface substrate or rigid plane substrate.
Further, in step (2), the material of substrate is polyethylene terephthalate (PET), poly- naphthalenedicarboxylic acid
Glycol ester (PEN), makrolon (PC), polyether sulfone (PES), polyimides (PI), glass, silicon (Si), silica
(SiO2) and sapphire (Al2O3) in one or more.
Further, in step (2), vertical czochralski method comprises the following steps：
Substrate is put into the solution containing monomolecular film, then slowly translates out from solution, solution evaporation is fallen,
Substrate surface forms the film of densification.
Further, in step (2) and step (3), using plasma lithographic technique, reactive ion etching technology or
Inductively coupled plasma technology performs etching.
Wherein, polyethylene terephthalate (PET), PEN (PEN), makrolon (PC),
Polyether sulfone (PES), the substrate of polyimides (PI) material need using plasma lithographic technique or reactive ion etching technology.
Glass, Si, SiO2、Al2O3The substrate of material is, it is necessary to using inductively coupled plasma technology, and material corresponds to etching gas not
Together.Si needs SF6Etching gas, SiO2Need to use C2F6Etching gas, C3F8Deng etching gas, Al2O3Need to use BCl3Etch gas
Body.At this time, it may be necessary to first with O2Plasma etching bead 30s or so, then etch substrate by above-mentioned technology.
Further, in step (2), before etching, mask plate is additionally provided with the surface of the monomolecular film away from substrate.
The patterning etching of substrate surface can be achieved in the use of mask plate.
Further, in step (2) and step (3), performed etching under the conditions of power is 50-2000W.
Further, in step (2) and step (3), etch period sum is 30-900s.
Further, in step (2) and step (3), etching instrument is a cavity, is full of etching gas in cavity.
Further, nano concavo-convex structure is the periodicity hemispherical dome structure of periodicity hemispherical dome structure or patterning.Receive
The cycle of rice concaveconvex structure and groove depth can be adjusted by changing particle diameter, the etching condition of polystyrene microsphere.
By such scheme, the present invention at least has advantages below：
(1) gas-liquid interface self-assembly method and vertical czochralski method are combined, can plane and it is complex-curved on formed it is fine and close
Individual layer polystyrene microsphere film, the compatible a variety of rigidity of the film or flexible material substrate.
(2) diminish after being etched using polystyrene microsphere, the characteristics of so as to expose substrate, self-assembling formation polystyrene
The substrate of microballoon mask, further etching exposure, so as to obtain periodic nano concavo-convex structure.
(3) present invention only needs a step to etch, and manufacture craft is simple, controllability is high, cost is low, various has micro-nano preparing
The fields such as the optics of structure, sensor, photovoltaic device, luminescent device have broad application prospects.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 is the schematic flow sheet that the embodiment of the present invention 1 makes nanostructured method on curved surface；
Fig. 2 is that the SEM of the polystyrene microsphere film formed in the embodiment of the present invention 1 on PET curved surfaces is surveyed
Attempt；
Fig. 3 is that the SEM structure of nano concavo-convex structure on the surface of PET curved surfaces in the embodiment of the present invention 1 is shown
It is intended to；
Fig. 4 is the AFM cycle schematic diagram of nano concavo-convex structure in the embodiment of the present invention 1；
Fig. 5 is the AFM cycle schematic diagram of nano concavo-convex structure in the embodiment of the present invention 2.
Embodiment
With reference to the accompanying drawings and examples, the embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment 1 prepares nanostructured on flexible PET curved surfaces
It is carrier to choose Si pieces, UV ozone processing 15min, improves its hydrophily.As shown in Fig. 1 (a), after processing
Si pieces 11 are placed horizontally in large area tank 10, its upper surface was not had just by water, and plane is provided for polystyrene microsphere
Support.
Isometric ethanol solution is added in polystyrene microsphere (particle diameter 500nm) aqueous solution that concentration is 3wt%,
As the spreading agent of microballoon, then ice-bath ultrasonic process 15min, make microballoon dispersed in ethanol, it is 1.5wt% to obtain concentration
Polystyrene microsphere alcohol-water mixed solution 13.
Mixed using dropper 12 to dropwise addition polystyrene microsphere alcohol-water on the large area water surface for be placed with hydrophilic surface
Solution 13, makes it spread on gas-liquid interface, and due to the diffusion of ethanol and the surface tension of water, microballoon can form individual layer
Structure, stronger adelphotaxy makes it spontaneously form ordered arrangement between microballoon.
Referring to Fig. 1 (b), Surfactant SDS 14 is added into water, forms microballoon even closer
Monomolecular film 15.Curved surface PET base 16 is put into water, the water surface is slowly translated out using vertical czochralski method.
Referring to Fig. 1 (c), after the water natural evaporation in substrate, polystyrene microsphere can form one layer of densification on curved surface
Film.
Curved surface PET base 16 is transferred to O2Perform etching 17 in reactive ion etching device, power selection 90W, vacuum
Degree control is 275mTorr, O2Flow control is 40sccm, etch period 90s.Etching process is referring to Fig. 1 (d), polystyrene
Microballoon is tapered into by original dense arrangement, forms smaller microballoon 18, so as to expose part of substrate surface, is further etched
The substrate surface exposed, so as to form micro-nano structure.
Curved surface PET base 16 is transferred to soaking and washing 15s in toluene solution, removes the polystyrene microsphere of residual, i.e.,
Obtain the curved substrate with periodicity hemispherical nano concavo-convex structure.
Fig. 2 is given in the present embodiment after vertical lifting, the scanning electricity of the polystyrene microsphere film formed on PET curved surfaces
Sub- microscope test chart.The polystyrene microsphere obtained as seen from the figure using vertical czochralski method forms the periodicity row of densification
Row.After etching, the surface of PET curved surfaces forms periodic hemispherical dome structure (Fig. 3), using AFM to the cycle
Property hemispherical dome structure pattern further characterization (Fig. 4), Fig. 4 shows that the cycle of the structure is about 430nm, and groove depth is about 70nm.
Embodiment 2 prepares nanostructured on flexible PET curved surfaces
The present embodiment is identical with the method and step of embodiment 1, and difference is, O2The reactive ion etching time is 60s.So that
Similar periodic structure has been obtained in PET curved substrates, it was found from the AFM schematic diagram (Fig. 5) of the structure, its
Cycle is about 480nm, and groove depth is about 30nm.
, can be by changing the parameter such as etch period, polystyrene microsphere particle diameter knowable to the result of comparative example 1 and 2, profit
The micro-nano structure of different-shape is made on curved surface of the method for the present invention, so as to for preparing the various light with micro-nano structure
Learn device, sensor, photovoltaic device, luminescent device etc..
Embodiment 3 prepares nanostructured on flexible PC curved surfaces
Selection slide is carrier, UV ozone processing 20min, improves its hydrophily.Slide after processing is horizontal positioned
In large area tank, its upper surface was not had just by water, planar support is provided for polystyrene microsphere.
It is molten that isometric ethanol is added in polystyrene microsphere (particle diameter 1000nm) aqueous solution that concentration is 2wt%
Liquid, as the spreading agent of microballoon, then ice-bath ultrasonic process 15min, make microballoon dispersed in ethanol, obtaining concentration is
1wt% polystyrene microsphere alcohol-water mixed solution.
It is molten to dropwise addition polystyrene microsphere alcohol-water mixing on the large area water surface for be placed with hydrophilic surface using dropper
Liquid, it is set to spread on gas-liquid interface.Xiang Shuizhong adds Surfactant SDS, forms microballoon even closer
Monomolecular film.Curved surface PC substrates are put into water, the water surface is slowly translated out using vertical czochralski method.
Curved surface PC substrates are transferred to O2Performed etching in reactive ion etching device, power selection 90W, vacuum degree control
For 275mTorr, O2Flow control is 40sccm, etch period 120s.Polystyrene microsphere is gradually become by original dense arrangement
It is small, smaller microballoon is formed, so as to expose part of substrate surface, the substrate surface exposed is further etched, so as to be formed
Micro-nano structure.
Curved surface PC substrates are transferred to soaking and washing 15s in toluene solution, the polystyrene microsphere of residual is removed, that is, obtains
Curved substrate with periodicity hemispherical nano concavo-convex structure.
Embodiment 4 prepares nanostructured in rigid plane sapphire substrates
Selection silicon chip is carrier, UV ozone processing 10min, improves its hydrophily.Slide after processing is horizontal positioned
In large area tank, its upper surface was not had just by water, planar support is provided for polystyrene microsphere.
It is molten that isometric ethanol is added in polystyrene microsphere (particle diameter 1000nm) aqueous solution that concentration is 2wt%
Liquid, as the spreading agent of microballoon, then ice-bath ultrasonic process 15min, make microballoon dispersed in ethanol, obtaining concentration is
1wt% polystyrene microsphere alcohol-water mixed solution.
Using dropper to dropwise addition polystyrene microsphere alcohol-water mixed solution on the large area water surface for be placed with carrier, make
It is spread on gas-liquid interface.Xiang Shuizhong adds Surfactant SDS, microballoon is formed even closer list
Molecular film.Plane sapphire substrate is put into water, the water surface is slowly translated out using vertical czochralski method.
Plane sapphire substrate is transferred to O2Performed etching in reactive ion etching device, power selection 90W, vacuum
Control as 275mTorr, O2Flow control is 40sccm, etch period 30s, polystyrene microsphere by original dense arrangement by
Gradual change is small, smaller microballoon is formed, so as to expose part of substrate surface.The substrate after processing is further transferred to BCl3Electricity
Performed etching in sense coupled plasma etch device, etch the substrate surface exposed, power selection 1500W, vacuum control
It is made as 50mTorr, BCl3Flow control is 20sccm, etch period 15min, so as to form micro-nano structure.Before etching, may be used also
With away from substrate monomolecular film surface cover on figuratum mask plate.In the presence of mask plate, base can be achieved
The patterning etching of basal surface.
Plane sapphire substrate is transferred to soaking and washing 15s in toluene solution, removes the polystyrene microsphere of residual, i.e.,
Obtain the planar substrates with periodicity hemispherical nano concavo-convex structure.
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and
Modification, these improvement and modification also should be regarded as protection scope of the present invention.
Claims (9)
- A kind of 1. method that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that comprise the following steps：(1) polystyrene microsphere is formed into monomolecular film by gas-liquid interface self-assembly method；(2) vertical czochralski method is utilized, the monomolecular film is transferred in substrate, then etches the monomolecular film, is made described Polystyrene microsphere size in monomolecular film diminishes, and forms substrate expose portion；(3) continue to etch the substrate expose portion, form the nano concavo-convex structure.
- 2. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly after (3), in addition to the step of polystyrene microsphere is washed off will be remained.
- 3. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (1), the particle diameter of the polystyrene microsphere is 200-3000nm.
- 4. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that in step Suddenly in (1), the gas-liquid interface self-assembly method comprises the following steps：Carrier with hydrophilic surface is placed in water, the alcoholic solution of polystyrene microsphere is instilled into water, then add thereto Enter surfactant, form monomolecular film；Wherein, the carrier provides planar support for the polystyrene microsphere.
- 5. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (2), the material of the substrate is polyethylene terephthalate, PEN, makrolon, polyethers One or more in sulfone, polyimides, glass, silicon, silica and sapphire.
- 6. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (2) and step (3), using plasma lithographic technique, reactive ion etching technology or inductively coupled plasma technology Perform etching.
- 7. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (2), before etching, mask plate is additionally provided with the surface of the monomolecular film away from substrate.
- 8. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (2) and step (3), performed etching under the conditions of power is 50-2000W.
- 9. the method according to claim 1 that nano concavo-convex structure is formed in plane or curved surface, it is characterised in that：In step Suddenly in (2) and step (3), etch period sum is 30-900s.
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Cited By (5)
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| CN108844924A (en) * | 2018-07-17 | 2018-11-20 | 河南师范大学 | Capillary pipe structure local surface plasma resonance biochemical sensor |
| CN109632711A (en) * | 2019-01-10 | 2019-04-16 | 金华伏安光电科技有限公司 | A kind of PS bead number of plies detection device |
| CN109963409A (en) * | 2019-04-10 | 2019-07-02 | 京东方科技集团股份有限公司 | The manufacturing method and board structure of substrate side surfaces conducting wire |
| CN113921392A (en) * | 2021-09-03 | 2022-01-11 | 南京信息工程大学 | PS (polystyrene) pellet circular etching process based on oxygen plasma etching |
| CN115894079A (en) * | 2022-11-14 | 2023-04-04 | 季华实验室 | Polystyrene microsphere film and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108844924A (en) * | 2018-07-17 | 2018-11-20 | 河南师范大学 | Capillary pipe structure local surface plasma resonance biochemical sensor |
| CN109632711A (en) * | 2019-01-10 | 2019-04-16 | 金华伏安光电科技有限公司 | A kind of PS bead number of plies detection device |
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| CN113921392A (en) * | 2021-09-03 | 2022-01-11 | 南京信息工程大学 | PS (polystyrene) pellet circular etching process based on oxygen plasma etching |
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| CN115894079B (en) * | 2022-11-14 | 2024-01-26 | 季华实验室 | Polystyrene microsphere membrane and preparation method and application thereof |
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Application publication date: 20171201 |