CN101177237A - Nanometer array and method for forming the same - Google Patents
Nanometer array and method for forming the same Download PDFInfo
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- CN101177237A CN101177237A CN 200610144590 CN200610144590A CN101177237A CN 101177237 A CN101177237 A CN 101177237A CN 200610144590 CN200610144590 CN 200610144590 CN 200610144590 A CN200610144590 A CN 200610144590A CN 101177237 A CN101177237 A CN 101177237A
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Abstract
The invention provides a method forming nanometer array, which comprises a template with a plurality of nanometer holes; which is characterized in that pressing art is performed on a macromolecule base material for the template; the template is stripped, thereby a plurality of bulges on the macromolecule base material are formed.
Description
Technical field
The present invention relates to a kind of formation method of nano-array, and particularly relate to the method that a kind of mode with impression forms nano-array.
Background technology
The nanostructured surface of systematicness has special effect, the compound eye structural that for example has ultralow reflectivity moth eye, the insect wing structure that anti-dust attaches, the lotus-effect (lotuseffect) on hydrophobic automatically cleaning lotus flower blade face etc., structure about the about 100nm of yardstick has special nature, how the function with these nanostructureds is applied in the daily life, is the target of present nano-technology techniques development.General macromolecule wants to reach functions such as hydrophobic automatically cleaning, anti-oil or reduction reflectivity, surface chemistry that must be by secondary or physical treatment are to obtain above-mentioned function, quite complicated and cost an arm and a leg on technology, and must use number of chemical product or supplementary equipment therefore.With the photoetching technique is example, and when pattern dimension has its process limitation during less than 90nm, the technology cost is too high also to be unfavorable for general application.
C.G Bernhard people such as (1962) in Acta Physiol Scand magazine, observe the moth compound eye at night the high susceptibility for light, the nanostructured of finding the following approximate circular cone of 250nm diameter has ultralow light reflectivity, Clapham in the wide area wave-length coverage; Hutley goes up in Nature (1973) and proposes Moth Eye Principle, people such as W.barthlott deliver the hydrophobic effect of observing on the lotus leaf (lotus effect) on the Planta magazine, lotus leaf surface is less than the bulge-structure of 50nm, the contact area of the surface nano-structure and the globule is more little, has self-cleaning function more.Yet, how with these function practicability, R.C.Furneaux etc. deliver sull (the anodic alumina oxide of regular porous property at Nature, AAO) production method, people such as M.Steinhard deliver with this structure as duplicating template at 2002 science, the mode of utilizing the nano aperture sidewall to soak into is adsorbed the Polymer Solution that dissolves or is inserted in the specification nano aperture, after treating solvent evaporates, the nano aperture template is dissolved, remaining part is the nanotube-shaped macromolecule of hollow just, and the someone utilizes the method to make nanofiber (United States Patent (USP) 20030089899).
Openly 2004-0126305,2004-0013873 utilize above-mentioned similar notion to United States Patent (USP) in early days, earlier the nano aperture stencil sidewalls is plated layer of material, form the hollow nanofiber, and insert inner layer material again after electrically-conductive backing plate combines, at last the template etching is removed, become compound nanometer cylinder.More than three patents all make anti-rice fiber as the template of duplicating usefulness with anodic oxidation aluminium formwork AAO, no matter be homogenous material or ectonexine composite, after packing material fills up template fully, all the etching of AAO template must be removed the fiber that just can obtain being shaped.
People such as Korean Patent KR20030784279Woo Lee utilize the AAO template to be the basis, the situation of duplicating of four kinds of nanostructureds is described, wherein alumilite process is become porous aluminium oxide structure, according to reaming situation difference, generation has the template of different hole sizes, the macromolecule of fusion is duplicated moulding, obtain high molecular nanometer cylindrical structural after the template etching removed, or the micro-structural hole etching of template upper strata removed become the secondary aluminum alloy pattern plate, can utilize secondary template with Polymer Solution copying nano structural membrane, can also go again with the mode reproduction micro-structural template of electroforming and duplicate, this piece patent is also pointed out in addition, utilize the inorganic nano-particle coating surface, apply one deck Polymer Solution again, obtain the composite nanostructure macromolecule membrane that the surface has irregular distribution nanoparticle after the solvent evaporates, this patent except with this body structure of AAO as duplicating the template, base plate aluminium after also utilizing AAO to remove is as secondary template, be to use the Polymer Solution that dissolves as the material that duplicates equally, after macromolecule fills up fully, must remove and desolvate, again the template etching is removed and directly the macromolecule diaphragm of template with shaping to be separated, in technology, can cause the distortion on the macromolecular structure, the nanostructured of secondary template can be excessive with the nanostructured difference of AAO template, the macromolecule matrix nanostructured function of duplicating out can be different, even destroyedly fall.
Propose to utilize the top layer to have the template of micro-structural oxides coating among the DE10154756 as the nanostructured impression, carry out the moulded section of nano-pillar body, the non-hollow state of template itself utilizes molded (molding) mode can make the nanostructured that the surface has systematicness easily, the formed nanostructured configuration of the method can be consistent with nano-form, just duplicate the shape of template fully, so only a kind of nanometer configuration of a kind of nano-form, can't adjust the variation of configuration according to process conditions, and the nanostructured of top layer moulding is quite fragile, when demoulding, handle as if no interface, can be with the nanostructured damage of moulding, surface nano-structure does not have intensive treatment and forms problem in use.
United States Patent (USP) discloses 2004188874 in early days and is macromolecule membrane anti-reflection structure multiple coating, top layer in surface-coated one floor height reflective particle, the mode of utilizing mould to duplicate forms ripple on the surface, hardened layer is coated on the macromolecule diaphragm, concaveconvex structure combines with the high reflectance particulate, can have the anti-low function of reflecting of dazzling, this optical functional layer is still by the wave lines in tens of μ m cycles of surface to be formed with high refraction particle, the hardened layer that provides support is below optical functional layer, bottommost is only the polymeric membrane plate base, the structure of multilayer will have the interface refractive index, follow the problem of intensity, layer with layer between different thermal coefficient of expansion all must take in, all can need to go especially to solve in environmental testing and use, so difficulty in process degree height, the technology cost is also higher relatively.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of plasticizing shaping nano-array and forming method thereof, have advantages such as quick shaping, technology be simple, with low cost.
For reaching above-mentioned purpose, the invention provides a kind of nano-array, comprising: a base material, have a plurality of nano projection things, and integrally formed with this base material, wherein the top of this nano projection thing has a recess or is a curved surfaces.
For reaching above-mentioned purpose, the invention provides a kind of method that forms nano-array, comprising: a template is provided, has a plurality of nano apertures; On a polymer base material, carry out imprint process with this template; And, on this polymer base material, form a plurality of nano projection things with this template demoulding.
On above-mentioned nano-array, can further form organic or inorganic coating, as reinforced nano array scratch resistance, toughness or surperficial close and distant water physical characteristic, and the soft or hard matter coating that reduces nano-array surface reflectivity or increase surface affinity.
Description of drawings
Fig. 1 to Fig. 3 shows the flow chart of imprint process of the present invention.
Fig. 4 a and 4b show the side view of the nano array structure of the embodiment of the invention.
Fig. 5 shows the side view of the nano array structure of another embodiment of the present invention.
Fig. 6 shows the side view of the nano array structure of another embodiment of the present invention.
Fig. 7 a demonstration one embodiment of the invention is utilized the sectional view of the nano-array micro-structural of scanning electron-microscopic observation gained.
Fig. 7 b is the top view of Fig. 7 a nano-array micro-structural.
Fig. 8 a demonstration embodiment of the invention is utilized the micro-structural of the nano-array of scanning electron-microscopic observation gained.
Fig. 8 b shows the top view of Fig. 8 a nano-array micro-structural.
Fig. 9 a shows the contact angle of general thermal plastic high polymer base material and water.
Fig. 9 b shows the contact angle of thermal plastic high polymer base material of the present invention and water.
Figure 10 a shows that thermal plastic high polymer substrate surface gecko pin effect of the present invention grasps the front view of function for the globule.
Figure 10 b shows that thermal plastic high polymer substrate surface gecko pin effect of the present invention grasps the side view of function for the globule.
Figure 11 shows the reflectivity of visible light.
Figure 12 a is presented at thick its adhesive force test result of Au of sputter 100nm on the polymer base material that has the nano projection thing and do not have the nano projection thing.
Figure 12 b is presented at thick its adhesive force test result of Au of sputter 200nm on the polymer base material that has the nano projection thing and do not have the nano projection thing.
The simple symbol explanation
101～alumina formwork;
103～polymer base material;
105～nano aperture;
107,107a, 107b～nano projection thing;
108～recess;
109～organic or inorganic coating;
A, C～the have zone of nano projection thing;
The zone of B, D～do not have nano projection thing.
The specific embodiment
The present invention utilizes the notion of macromolecule diaphragm impression, can be widely used in thermoplastic macromolecule material, and need not be with melt polymer material in organic solvent, exempts following removal of solvents and malformation and environmental issue that solvent evaporates caused.
Fig. 1 to Fig. 3 shows that the present invention utilizes the nano-imprinting method of heat pressing type, is impression block with porous anodised aluminium, forms the flow chart of nano-array.As shown in Figure 1, alumina formwork 101 is handled through anode by fine aluminium and is formed, have a plurality of nano apertures 105, also can utilize the uniformity that secondary anode is handled increases the nano aperture aperture, error with formed nano-array diameter behind the accurate control imprint process, the diameter of nano aperture is approximately less than 200nm, preferably between about 20nm to 150nm in one embodiment.
As shown in Figure 2, earlier polymer base material 103 being heated to proper temperature makes it softening, the visual employed macromolecule kind of heating-up temperature is different and adjust to some extent, and wherein polymer base material 103 can be thermal plastic high polymer, thermosetting polymer or UV curing type macromolecule.For example wherein be preferably thermal plastic high polymer: polymethyl methacrylate (polymethyl methacrylate, be called for short PMMA), Merlon (polycarbonate, be called for short PC), cyclic olefin copolymer (cyclo-olefin copolymers, be called for short COC), polypropylene (polypropylene, be called for short PP), polyethylene (polyethylene, be called for short PE), polyvinyl chloride (polyvinyl chloride, be called for short PVC), polyethylene terephthalate (polyethyleneterephthalate, be called for short PET), liquid crystal polymer (liquid crystal polymer, be called for short LCP) or thermoplasticity pi (thermoplastic polymide is called for short TPI); Thermosetting polymer for example is pi (polymide is called for short PI) or epoxy resin (Epoxy).Then can be with polymer base material 103 upwards towards alumina formwork 101 extruding, or with alumina formwork 101 downwards towards polymer base material 103 extruding carrying out imprint process, alumina formwork 101 slightly is absorbed in the polymer base material 103, polymer base material 103 is entered in more than 101 nano aperture 105 of template through extruding, treat imprint process stable back cooling, make polymer base material 103 shrink typing, import interface treating agent afterwards, directly alumina formwork 101 being imposed external force with polymer base material 103 separates, as shown in Figure 3, on polymer base material 103, form a plurality of nano projection things 107, the diameter of nano projection thing 107 about 20 is to 150nm in one embodiment, highly approximately less than 400nm, and its spacing is approximately less than 50nm, and depth-width ratio is approximately less than 3.The depth-width ratio of nano projection thing 107 about 2 in a preferred embodiment.
As shown in Figure 3, need not handle the organic solvent of polymer base material 103 when carrying out the demoulding, in the time of can avoiding follow-up removal organic solvent, because of solvent evaporates causes nano array structure distortion and environmental issue on the polymer base material 103.Since above-mentioned imprint process can be directly with AAO as template, compare with the technology area less than the required cost of the nanostructured of 100nm with general the making with the photoetching etching mode, has suitable advantage, duplicate formed a plurality of nano projection thing by above-mentioned stamped method in polymer base material 103 shallow structure, depth-to-width ratio is approximately less than 3, and be different from the technology of traditional nanofiber, alumina formwork 101 is after impression is finished, be able to polymer base material 103 releasely by affinity difference, and need alumina formwork 101 do not removed with etched mode.The high molecular cohesive force because macromolecule flows by hole interface adhesive force, when heating, and the contraction situation after the moulding and technology vacuum are controlled the different kenels on nanostructured top, so select to set via the regulation and control of high polymer material plasticizing rheological characteristic, material, just can reach the nano array structure kenel of diverse microcosmic with process conditions.
Fig. 5 and 6 shows in one embodiment of the invention, by the formed nano-array of different process conditions.Use cyclic olefin (cyclo-olefin) macromolecular material of about 130 degree of Tg, with the nano aperture diameter less than the AAO template of 100nm at 150 degree and pressure less than 5bar, under the situation of vacuum less than 1atm, can form nano projection thing 107a as shown in Figure 5, its top has a curved surfaces.In addition, cyclic olefin (cyclo-olefin) macromolecular material that uses about 130 degree of Tg with the nano aperture diameter between the AAO of 100-200nm template at 152 degree and pressure less than 5bar, under the situation of vacuum greater than 1atm, can form nano projection thing 107b as shown in Figure 6, its top is a recess, both nanostructure height are no more than 400nm, the different kenels in its top have different functions, air and macromolecule interfacial present the situation that specific area distributes physically, top has minimum contact area, therefore the contact angle with superelevation, hydrophobic property and Fan Dewa contact force.In addition,, engage, on optics, have the variation characteristic of refractive index gradient, have the effect that reduces transparent polymer base material 103 surface reflectivities and promote the efficiency of light energy utilization less than visible wavelength with coating if polymer base material 103 is a transparent base.
In order to increase the intensity of nanostructured (nano projection thing 107 formed nano-arrays), can form a compliance organic or inorganic coating 109 at body structure surface after the demoulding, its thickness is about 50nm to 10 μ m, preferably approximately less than 100nm, shown in Fig. 4 a and 4b.Wherein this inorganic coating comprises metal, for example: Zr, Ti, Cu, Ag, Au, Al, Ni, W, Fe or Pt; Oxide, for example: SiO
2, TiO
2, ITO, GaAs, InGaAs, non-crystalline silicon or polysilicon; And organic coating comprises polysiloxanes (polysiloxane), silicon, conducting polymer, Organic Light Emitting Diode (organic light emitting diode, abbreviation OLED), polymer LED (polymer light emitting diode, be called for short PLED) or poly-dioxoethyl thiophene (polyethylenedioxythiophene, be called for short PEDOT), in order to strengthen the toughness and the scratch resistance of nanostructured.The hard coat (hard coating) that is used for reducing reflectivity traditionally all is formed in the effectively bottom of layer of optics, and by the integrally formed nanostructured of the present invention and polymer base material 103, it has the elastic strength of macromolecular material, the organic or inorganic coating 109 that forms on its surface is general just like strengthening sugar-coat, can directly the intensity of overlay coating be manifested and have the effect of modification configuration, the nanostructured surface that is formed on owing to compliance can make organic or inorganic coating 109 show the particular configuration of nanostructured.
Fig. 7 a demonstration one embodiment of the invention is utilized the nano-array micro-structural sectional view of scanning electron-microscopic observation gained, utilize alumina formwork that transparent thermal plastic high polymer is carried out micro-embossing technology in the present embodiment, the transparent thermoplastic macromolecule not exclusively fills up the nano aperture of alumina formwork in the moulding process, wherein the nano aperture diameter of alumina formwork is approximately less than 100nm, the about 20nm of each hole spacing, nanostructured sectional view after the impression shaping demoulding is shown in Fig. 7 a, the depth-to-width ratio of nanostructured is about 2, and there is recess as shown in Figure 6 on its structure top.Fig. 7 b is the top view of nano array structure, can see the nano projection thing that is evenly distributed.
Fig. 8 a demonstration another embodiment of the present invention is utilized the nano-array micro-structural sectional view of scanning electron-microscopic observation gained, in the present embodiment, utilize alumina formwork that transparent thermal plastic high polymer base material is carried out micro-embossing technology, the about 100nm of nano aperture diameter of alumina formwork, the about 50nm of each hole spacing, nanostructured side view after the impression shaping demoulding is shown in Fig. 8 a, the depth-to-width ratio of nanostructured about 3, there is curved surfaces as shown in Figure 5 on the structure top, Fig. 8 b is the top view of nanostructured, can see the nano array structure that is evenly distributed.
Fig. 9 b demonstration utilizes imprint process of the present invention formed nano array structure on the thermal plastic high polymer base material, the contact angle that is carried out with water measures experimental result, polymer base material surface and about 144 degree of the contact angle of water, and Fig. 9 a shows that the thermal plastic high polymer base material that utilizes without imprint process of the present invention carries out the result that contact angle measures, the polymer base material surface is about 90 degree with the contact angle of water, hence one can see that, utilize alumina formwork of the present invention to carry out the formed nano array structure of imprint process, can reach super-hydrophobic effect (l0tus effect) really as lotus leaf.
Figure 10 a shows that polymer base material that the present invention has a nano-array has gecko pin effect (gecko ' seffect), the globule can be locked in polymer base material surface with nano array structure, globule volume is no more than 10 μ L, and Figure 10 b can see the situation that the globule is caught by Nanosurface.
Figure 11 shows the reflectivity of a transparency carrier in visible light, and wherein regional A has nano projection thing of the present invention, and area B does not then have nano projection thing of the present invention, and is as shown in figure 11, low in regional A reflection of light luminance ratio area B.Transparency carrier in Figure 11 can be PC or COC, is example with PC, and regional A is about 2～3 at the reflectivity that visible wavelength is about between 400～700nm; With COC is example, and regional A is about 1～2 at the reflectivity that visible wavelength is about between 400～700nm, and the reflectivity of different its regional A of baseplate material is littler.Can learn that thus nano-array of the present invention need not import colour cast (color-shift) can be reduced and dazzle light and reflection.
Experimental study shows that nano projection thing of the present invention can increase polymer base material in fact and covers adhesive force between the coating on it, and Figure 12 a and 12b show respectively and be plated in that thickness is the result of its adhesive force test of Au coating of 100nm and 200nm on the PC polymer base material.Hundred lattice methods of testing are used in the test of this adhesive force, and it cuts out 100 square grid having on base material of coating, and the 3M adhesive tape is attached on this grid, divests fast then, remain in the relative percentage value that grid number on the substrate provides adhesive force.Shown in Figure 12 a and 12b, the zone C with nano projection thing is by the test of hundred lattice, and the region D that does not have the nano projection thing then can't be by the test of hundred lattice.It should be noted that nano projection thing of the present invention can be used to improve the adhesive force of any organic or inorganic coating, for example Si, Au, Cu or the like, in addition, for example the COC substrate is also in the present invention available for the polymeric substrate beyond the PC substrate.
Table one demonstration utilizes the imprint process of the present invention light reflectivity measurement that formed nano array structure carried out on the transparent thermoplastic macromolecule, utilize the equipment Hazemeter that measures the coloured light that looses to record general transparent thermoplastic macromolecule, for example the penetrance of plastic film about 92%, and on its surface with the formed nano array structure of imprint process of the present invention, can make penetrance be promoted to 94%.
Table one
| Penetrance | |
| Traditional transparent thermoplastic macromolecule | 92.51 |
| Transparent thermoplastic macromolecule through imprint process of the present invention | 94.18 |
| Transparent thermoplastic macromolecule through imprint process of the present invention | 93.65 |
Claims (25)
1. nano-array comprises:
Polymer base material has a plurality of nano projection things, and is integrally formed with this base material, and wherein the top of this nano projection thing has recess or is curved surfaces.
2. nano-array as claimed in claim 1, wherein this base material is a same material with these a plurality of nano projection things.
3. nano-array as claimed in claim 2, wherein this polymer base material comprises thermal plastic high polymer, thermosetting polymer or UV curing type macromolecule.
4. nano-array as claimed in claim 3, wherein this thermal plastic high polymer comprises PMMA, PC, COC, PP, PE, PVC, PET, LCP or TPI.
5. nano-array as claimed in claim 3, wherein this thermosetting polymer comprises PI or epoxy resin.
6. nano-array as claimed in claim 1, it is as the automatically cleaning film.
7. nano-array as claimed in claim 1, it is as the anti-reflective film substrate.
8. nano-array as claimed in claim 1, it is as the absorption substrate.
9. nano-array as claimed in claim 1 also comprises organic or inorganic coating, is coated on to compliance on this base material and these a plurality of nano projection things.
10. nano-array as claimed in claim 9, wherein this organic coating comprises: polysiloxanes, silicon, conducting polymer, OLED, PLED or PEDOT.
11. nano-array as claimed in claim 9, wherein this inorganic coating comprises: Zr, Ti, Cu, Ag, Au, Al, Ni, W, Fe, Pt, SiO
2, TiO
2, ITO, GaAs, InGaAs, non-crystalline silicon or polysilicon.
12. nano-array as claimed in claim 9, wherein the thickness of this organic or inorganic coating is 50nm to 10 μ m.
13. nano-array as claimed in claim 9, it is as the coating coating.
14. nano-array as claimed in claim 9, wherein this nano projection thing improves the adhesive force between this polymer base material and this organic or inorganic coating.
15. a method that forms nano-array comprises:
Template is provided, has a plurality of nano apertures;
On polymer base material, carry out imprint process with this template; And
With this template demoulding, on this base material, form a plurality of nano projection things.
16. the method for formation nano-array as claimed in claim 15 also comprises adding interface treating agent in order to this template demoulding.
17. the method for formation nano-array as claimed in claim 15, wherein this template by fine aluminium through one or secondary anode handle obtained.
18. the method for formation nano-array as claimed in claim 15 comprises that also the organic or inorganic coating that forms compliance is on this base material and these a plurality of nano projection things.
19. the method for formation nano-array as claimed in claim 18, wherein this organic coating comprises: polysiloxanes, silicon, conducting polymer, OLED, PLED or PEDOT.
20. the method for formation nano-array as claimed in claim 18, wherein this inorganic coating comprises: Zr, Ti, Cu, Ag, Au, Al, Ni, W, Fe, Pt, SiO
2, TiO
2, ITO, GaAs, InGaAs, non-crystalline silicon or polysilicon.
21. the method for formation nano-array as claimed in claim 18, wherein this organic or inorganic thickness of coating is approximately less than 100nm.
22. the method for formation nano-array as claimed in claim 15, wherein the top of this nano projection thing has recess or is curved surfaces.
23. the method for formation nano-array as claimed in claim 15, wherein this polymer base material comprises thermal plastic high polymer, thermosetting polymer or UV curing type macromolecule.
24. the method for formation nano-array as claimed in claim 23, wherein this thermal plastic high polymer comprises: PMMA, PC, COC, PP, PE, PVC, PET, LCP or TPI.
25. the method for formation nano-array as claimed in claim 23, wherein this thermosetting polymer comprises PI or epoxy resin.
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