CN103253870B - A kind of antireflection and self-cleaning glass and manufacture method thereof - Google Patents
A kind of antireflection and self-cleaning glass and manufacture method thereof Download PDFInfo
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Abstract
The invention discloses a kind of antireflection and self-cleaning glass and manufacture method thereof, the impression materials of glass surface utilizes the nano-imprint process based on band shape soft mold form the nano-cone array structure of sub-wavelength or adopt hard mask and impression materials to etch the nano-cone array structure of sub-wavelength based on the nano impression of band shape soft mold and hard mask transfer etching technics at glass surface.The present invention can be used for the field such as solar panel, glass curtain wall, windshield, optical element and instrument, large size high definition flat pannel display, infrared eye.The advantage that the present invention has anti-reflective and self-cleaning performance is high, good endurance, stability are high, severe environment adapt to by force, productivity is high, cost is low, especially can realize overlarge area antireflection and self-cleaning glass is efficient and low cost mass production.
Description
Technical field
The invention belongs to glass surface processing and technical field of micro-nano manufacture, particularly relate to a kind of antireflection and self-cleaning glass and manufacture method thereof.
Background technology
Antireflection (antireflective) and self-cleaning glass can cut down the reflection of glass itself effectively, and the transmitance adding glass (namely reduces the entire spectrum reflection of incident light, increases transmission, enhance the transparency; Reduce the mirror effect of glass surface, there is anti-dazzle function), and there is antipollution and self-cleaning advantage, it effectively can improve performance and the quality of the products such as solar panel, glass curtain wall, windshield, optical element (lens, micro-eyeglass, camera gun etc.), flat pannel display (touch-screen, television screen, smart mobile phone screen etc.).Such as, solar panel uses antireflection and self-cleaning glass not only effectively can improve photoelectric transformation efficiency (minimizing reflection, increase the absorption of light), and the light efficiency loss that dirt accumulation can be avoided to cause is (although solar panel is through hydrophobic coating process, but solar battery panel surface still easily accumulates dust and dirt, and after 6 months, light efficiency loss in efficiency can reach 40%).The glass curtain wall of Highrise buildings adopts antireflection and self-cleaning glass not only can solve a difficult problem for cleaning glass, but also can solve the light pollution problem caused due to glass-reflected.Out of doors or in bright environment, touch-screen, mobile phone screen, computer monitor screen, digital camera screen etc. all can cause use inconvenience, and (picture is unintelligible due to the reflection of glass interface, there is the projection of surroundings outside, contrast gradient reduction etc.), adopt antireflection and self-cleaning glass not only effectively can eliminate reflection, improve contrast gradient, obtain picture clearly, and its self-cleaning function had effectively can also keep out dust, sweat stain stains.Antireflection and self-cleaning glass are used for the front windshield of automobile, not only can the outside surface dirt of automatically cleaning window and gravel, and can eliminate dazzle, strengthen visibility meter, and prevent internal surface to be atomized.Therefore, antireflection and self-cleaning glass have widely with huge commercial applications prospect.
Glass is made to have antireflection at present and/or self-cleaning performance mainly adopts following methods: (1) multicoating; (2) surface mount anti-reflection film; (3) self-assembling antireflective is coated with or/and automatic cleaning coating.But these structures and method make glass only have antireflection or the single function of automatically cleaning usually, are difficult to have antireflection and self-cleaning function on the one hand simultaneously.But also there is many defects and deficiency.Such as multicoating faces following problems: 1. because the introducing of differing materials causes thermodynamics not mate or the problem such as poor adhesive force reduces its stability; Although 2. the antireflective property of this film usually in certain wave band is better, can not compared with the loss reducing reflected light within the scope of wide band; 3. natural material category is limited, can not meet actual needs, particularly continuously this requirement of specific refraction, if: the specific refraction of magnesium fluoride, silicon nitride, silicon-dioxide is all near 1.4, and does not almost have specific refraction to be in material between 1 and 1.2; 4. two kinds of major technique-physical vapor depositions (PVD) and chemical vapour deposition (CVD) production cost of preparing anti-reflection film are high.Surface mount anti-reflection film exist equally poor adhesive force, poor in timeliness, for environmental compatibility difference etc. problems.Therefore, there is following many problems in the method such as conventional multilayer plated film and surface mount anti-reflection film: rete is to the tack problem between the tack of substrate surface and rete; The resist chemical of rete and weather resistance, stability problem; The expansion mismatch caused due to thermal expansivity difference and condensation lamination problem; Components permeate between rete and rete and between rete and substrate and diffusion problem; Suitable film material can not be found; Short-wave band reflectivity cannot be reduced; For envrionment temperature and humidity bad adaptability, exist and easily come off and the problem such as heat affecting.
Therefore; existing scheme and manufacture method are also difficult to the requirement meeting antireflection and self-cleaning glass performance and actual production; this has become restriction antireflection and the bottleneck of the extensive promotion and application of self-cleaning glass, how to develop new antireflection and self-cleaning glass structure and method that is efficient, low cost large-scale production thereof become current in the urgent need to.
Summary of the invention
The object of the invention is for overcoming above-mentioned the deficiencies in the prior art, a kind of antireflection and self-cleaning glass and manufacture method thereof be provided, it is efficient, low cost, and can scale operation be applied to.
For achieving the above object, the present invention adopts following technical proposals:
A kind of antireflection and self-cleaning glass, the impression materials of glass surface utilizes the nano-imprint process based on band shape soft mold form the nano-cone array structure of sub-wavelength or adopt hard mask and impression materials at glass surface and etch the nano-cone array structure of sub-wavelength based on the nano impression of band shape soft mold and hard mask transfer etching technics.
Described nanocone is that circular cone or pyramid are tied or pyramid-like structure, and nanocone basal diameter is 100 ~ 300nm, and depth-to-width ratio is 3 ~ 12, and the distance between nanocone bottom center is 100 ~ 300nm.
Described band shape soft mold has the square or conical characteristic pattern of circle of array depression.
Described impression materials is ultraviolet photochemical polymer materials or sol-gel material or titanic oxide material or earth silicon material.
A manufacture method for antireflection and self-cleaning glass, it forms the nano-cone array structure of sub-wavelength at glass surface based on band shape soft mold nano-imprint process, comprise the steps:
Step (1): pre-treatment, deposits one or more layers hard mask layer at glass surface, forms glass substrate;
Step (2): liquid impression materials coating on a glass substrate;
Step (3): imprinting moulding:
(3-1) first, utilize impression mode by a glass substrate attached for the band shape soft mold pressure with circular or square recess feature, make the liquid impression materials extrusion packing be coated with on glass substrate in the recess feature of band shape soft mold;
(3-2) liquid impression materials is made to be filled in the recess feature of band shape soft mold completely, and guarantee that the impression materials on the band shape soft mold after filling completely and glass substrate remains bringing into conformal contact, utilize UV curing mode to solidify liquid impression materials, realize the complete curing molding of stamping structure;
(3-3) last, the feature structure of impression curing molding is separated with band shape soft mold, completes the demoulding;
Step (4): utilize etching technics to carry out coining pattern transfer, during etching, the etch rate of hard mask material is lower than glass substrate, to obtain the nano-cone array structure of sub-wavelength;
Step (5): aftertreatment.
The etching technics of described step (4) adopts reactive ion etching or sense coupling or wet etching.
In described step (4), the height of nanocone depends on material and the thickness of hard mask.
A manufacture method for antireflection and self-cleaning glass, it forms the nano-cone array structure of sub-wavelength at glass based on band shape soft mold nano-imprint process, comprise the steps:
Step (1): pre-treatment, increases the adhesion characteristics of glass substrate surface;
Step (2): liquid impression materials is coated on glass, described liquid impression materials is the coated material of glass substrate;
Step (3): imprinting moulding:
(3-1) first, utilize impression mode by a glass substrate attached for the band shape soft mold pressure with conical shaped depression shape feature, make the liquid impression materials extrusion packing be coated with on glass substrate in the feature pattern of depression;
(3-2) liquid impression materials is made to be filled in band shape soft mold completely, and guarantee that the liquid impression materials on the band shape soft mold after filling completely and glass remains bringing into conformal contact, utilize UV curing mode to solidify liquid impression materials, realize the complete curing molding of stamping structure;
(3-3) last, the feature structure of impression curing molding is separated with band shape soft mold, completes the demoulding;
Step (4): aftertreatment.
Beneficial effect of the present invention:
The present invention utilizes nano impression and etching to produce the nanocone of sub-wavelength at exposed glass substrate surface, or directly impresses out the nanocone of sub-wavelength at the liquid impression materials (coated material) of glass substrate surface.The nanocone depth-to-width ratio of sub-wavelength is larger, antireflection and self-cleaning performance better.
The present invention adopts the nano-imprint process based on band shape soft mold, and it has, and efficiency is high, production cost is low, coining pattern area large (realizing rigid substrate meter level scale nanometer graphical), good demolding performace, die life is long and easy to maintenance, coining pattern consistence is good and resolving power is high, for the good significant advantage of non-smooth glass substrate adaptability.Overcome that classic flat-plate type nano impression efficiency is low, imprint area is little, die life is short and difficult in maintenance and the defect of row graph cannot be realized.Overcome contour roll forming nano impression and impress efficiency low (ultra-violet curing linear contact lay needs length set time), the non-shortcoming for smooth glass substrate bringing into conformal contact ability for glass substrate (rigid substrate).The solution that manufacture for overlarge area antireflection and self-cleaning glass provides a kind of efficient, low cost mass to manufacture, can realize overlarge area antireflection and self-cleaning glass is efficient and low cost mass production.
Significant advantage of the present invention is:
(1) antireflective in wide band, large ranges of incidence angles is realized, there is within the scope of wide band good antireflective properties, because nanocone body structure provides the aspect ratio (height/diameter of nanocone) that strengthens photoabsorption optimum shape, it can all play a role to the antireflection of short wavelength light and the scattering of light of long wavelength simultaneously;
(2) higher antireflective property, shows as the reflection (when the characteristic dimension of optical element is much smaller than incident light wave, will only there is Zero-order diffractive ripple) or transmitted light that only there are zero level when light wave acts on sub-wavelength nanostructure;
(3) stable performance, anti-reflective effect is good, especially severe environment strong adaptability (is avoided causing due to the difference of shrinkage coefficient between multilayer film coming off, the defects such as surface mount anti-reflection film poor adhesive force, poor in timeliness), be specially adapted to by the larger visible ray of the such environmental effects such as temperature and humidity and infrared antireflective device;
(4) there is good antireflection and self-cleaning performance simultaneously;
(5) graded index can be realized;
(6) production cost is low;
(7) production efficiency is high, can realize continuous seepage;
(8) manufacture of overlarge area antireflection and self-cleaning glass can be realized.
Instant invention overcomes the deficiency of the method such as conventional multilayer plated film and surface mount anti-reflection film, provide a kind of antireflection and self-cleaning glass of high performance-price ratio, and provide a kind of production method of technical grade for the manufacture of overlarge area antireflection and self-cleaning glass.The present invention can be used for the field such as solar panel, glass curtain wall, windshield, optical element and instrument (lens, microscope, photographic camera, optical mirror slip etc.), flat pannel display (touch-screen, television screen, smart mobile phone screen etc.).Be particularly suitable for solar panel, glass curtain wall, large size high definition flat display field, and by fields such as the larger infrared eye of the such environmental effects such as temperature and humidity, high-efficiency solar photovoltaic battery, outdoor and portable displays.
Accompanying drawing explanation
Fig. 1 is the antireflection and the self-cleaning glass structural representation that the present invention is based on glass sheet surface nano patterning;
Fig. 2 is the antireflection and the self-cleaning glass structure fabrication process schema that the present invention is based on glass sheet surface nano patterning;
Fig. 3 is the antireflection and the self-cleaning glass structure manufacturing process schematic diagram that the present invention is based on glass sheet surface nano patterning;
Fig. 4 is the imprinting moulding structural representation based on band shape mould nano-imprinting device used;
Fig. 5 is the antireflection and the self-cleaning glass structural representation that the present invention is based on glass sheet surface coating nano patterning;
Fig. 6 is the antireflection and the self-cleaning glass structure fabrication process schema that the present invention is based on glass sheet surface coating nano patterning;
Fig. 7 is the antireflection and the self-cleaning glass structure manufacture schematic diagram that the present invention is based on glass sheet surface coating nano patterning;
Wherein 1. wafer-supporting platforms, 2. glass substrate, 3. liquid impression materials, 4. apparatus for coating, 5. eindruckwerk, 501. roller platens, 502. demoulding rollers, 503. feeding device I, 504. feeding device II, 6. be with shape soft mold, 7. ultra-violet curing device, 8. feature structure, 9. conformal roller.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further elaborated, should be noted that following explanation is only to explain the present invention, not limiting its content.
The present invention can utilize the imprinting apparatus shown in Fig. 4 to realize.It comprises wafer-supporting platform 1, and glass substrate 2 is placed in also synchronous operation with it on wafer-supporting platform 1; Liquid impression materials 3 is uniformly coated on glass substrate 2 by apparatus for coating 4; Be connected with feeding device I503, feeding device II504, roller platen 501 and demoulding roller 502 and auxiliary imprinting apparatus running roller separately with shape soft mold 6, band shape soft mold 6 pressure is attached on the liquid impression materials 3 of glass substrate 2 by roller platen 501; Consolidation zone between roller platen 501 and demoulding roller 502 arranges ultra-violet curing device 7, and is positioned at the top of auxiliary imprinting apparatus; Auxiliary imprinting apparatus comprises the conformal roller 9 that at least one impels band shape soft mold 6 and substrate bringing into conformal contact.
During use, glass substrate 2 is placed on wafer-supporting platform 1, on the glass substrate 2 processed, utilizes apparatus for coating 4 to be coated with impression materials 3 afterwards, impress.
Embodiment 1
The nanometer conical array array structure of sub-wavelength is formed in exposed glass sheet surface.
As shown in Figure 1, the nanometer conical array array structure of sub-wavelength is etched in exposed glass sheet surface, the shape of nanocone is conical, basal diameter 180nm, depth-to-width ratio is 4 (height of nanocone is 880nm), and the spacing (cycle) between nanocone bottom center is 220nm.
Concrete preparation process following (Fig. 2 ~ 3):
(1) pre-treatment
1. glass substrate 2 cleans, and use acetone, ethanol, deionized water ultrasonic cleaning sheet glass 5 minutes respectively, nitrogen dries up, and dries, as Fig. 3 a;
2. deposited hard mask layer, the silicon-dioxide that glass substrate 2 deposits 300nm as hard mask layer, as Fig. 3 b.
(2) liquid impression materials 3 is coated with
Adopting bar seam coating process to be coated with by uv curable polymers homogenize material is layered on silicon-dioxide, and thickness is 800nm.
(3) imprinting moulding
1. eindruckwerk 5 is exerted pressure to band shape soft mold 6 by roller platen 501, under the effect of online contact printing power by liquid for the ultra-violet curing of coating on glass substrate 2 impression materials 3 extrusion packing in the concave character of band shape soft mold 6;
2. feeding device I503 and feeding device II504 drives band shape soft mold 6 to move to demoulding roller 502 direction, wafer-supporting platform 1 carries sheet glass and the equidirectional motion of band shape soft mold 6 simultaneously, realize the liquid impression materials 3 of ultra-violet curing to the filling completely of band shape soft mold 6 concave character and uniform spreading by the conformal roller 9 of auxiliary imprinting apparatus, guarantee that filling rear band shape soft mold 6 completely remains good bringing into conformal contact with the liquid impression materials 3 of ultra-violet curing on sheet glass.And utilize ultra-violet curing device 7 to solidify the liquid impression materials 3 of liquid ultra-violet curing, realize the curing molding cmpletely of stamping structure;
3. utilize demoulding roller 502 feature structure 8 of impression curing molding and band shape soft mold 6 to be separated from each other, complete the demoulding.
As Fig. 3 c.
(4) Graphic transitions
1. adopt reactive ion etching process, remove the residual layer of coining pattern;
2. with the figure of impression for mask, adopt sense coupling technique to transfer on silicon oxide hard mask layer by the feature pattern be stamped on ultra-violet curing organic polymer material, as Fig. 3 d.
3. with the silicon oxide hard mask layer after transition diagram for mask, adopt sense coupling technique to etch nano-cone array structure at glass surface, as Fig. 3 e.Because the etch rate of hard mask layer is lower than sheet glass, therefore etch nanocone on the glass sheet, and along with the formation of nanocone, hard mask layer is removed simultaneously, the height of nanocone depends on material and the thickness of hard mask layer.
(5) aftertreatment
1. residual silicon-dioxide is removed;
2. clean glass, remove glass surface residue and dirt.
Feature pattern with shape soft mold 6 described in the present embodiment is circular pore structure.
Imprinting apparatus described in the present embodiment is 1MPa to roller platen applied pressure, and the translational speed of band shape soft mold 6 is 1m/min, and the translational speed of glass substrate is 1m/min.
Embodiment 2
The liquid impression materials coating of glass substrate directly impresses out the nanometer conical array array structure of sub-wavelength.
As shown in Figure 5, liquid impression materials coating is scribbled on sheet glass substrate 2 surface, and in coating, directly impress out the nanometer conical array array structure of sub-wavelength, the shape of figure is conical, basal diameter 200nm, the depth-to-width ratio of nanocone is 5 (height of nanocone is 1000nm), and the spacing (cycle) between nanocone bottom center is 260nm.
Coating described in the present embodiment is nm TiO 2-base ultra-violet curing transparent liquid impression materials (as added the impression materials that titanium dioxide nano-particle is formed in epoxy polymer matrix KATIONBONDOMVE110707).
Concrete steps following (Fig. 6 ~ 7):
(1) pre-treatment
1. glass substrate 2 cleans, and use acetone, ethanol, deionized water ultrasonic cleaning sheet glass 5 minutes respectively, nitrogen dries up, and dries;
2. paving silane coupling agent is coated with, use silane coupling agent is the bonding force in order to improve transparent polymer and glass substrate 2, its mechanism of action is that first coupling agent reacts with water and be hydrolyzed into silanol, hydrogen bond is formed with the hydroxyl of glass surface after silanol dehydrating condensation becomes oligopolymer, heat treated is then dewatered formation covalent linkage, it should be noted that Heating temperature can not be too high, in order to avoid destroy the organic group on Siliciumatom.Silane coupling agent is made into the dilute solution that mass concentration is 0.5 ~ 1%, is coated very thin one deck, thickness 200nm in clean by maxxaedium.
(2) liquid impression materials coating
Adopting roller coat coating process to be evenly coated with by nm TiO 2-base ultra-violet curing transparent liquid impression materials is layered on as coating on glass substrate 2, and thickness is 5 μm, as Fig. 7 b.
(3) imprinting moulding
1. by roller platen 501, band shape soft mold 6 is exerted pressure, under the effect of online contact printing power by liquid for the ultra-violet curing of coating on glass substrate 2 impression materials 3 extrusion packing in the concave character of band shape soft mold 6;
2. feeding device I503 and feeding device II504 drives band shape soft mold 6 to move to demoulding roller 502 direction, wafer-supporting platform 1 carries glass substrate 2 and the equidirectional motion of band shape soft mold 6 simultaneously, realize the liquid impression materials 3 of ultra-violet curing to the filling completely of band shape soft mold 6 concave character and uniform spreading by auxiliary imprinting apparatus conformal roller, guarantee that filling rear band shape soft mold 6 completely remains good bringing into conformal contact with the liquid impression materials 3 of ultra-violet curing on glass substrate 2.And utilize ultra-violet curing device 7 to solidify the liquid impression materials 3 of liquid ultra-violet curing, realize the curing molding cmpletely of stamping structure;
3. utilize demoulding roller 502 feature structure 8 of impression curing molding and band shape soft mold 6 to be separated from each other, complete the demoulding.
As Fig. 7 c.
(4) aftertreatment
Structure after impression carries out post curing treatment, guarantees to solidify completely.
Feature pattern with shape soft mold 6 described in the present embodiment is conical structure.
Imprinting apparatus described in the present embodiment is 1.3MPa to roller platen applied pressure, and the translational speed of band shape soft mold 6 is 1m/min, and the translational speed of glass substrate is 1m/min.
The present embodiment in order to improve glass substrate 2 and liquid state the liquid impression materials 3 of ultra-violet curing between adhesivity, also can adopt for glass substrate 2 and carry out surface treatment with the following method.First oxygen gas plasma surface treatment is carried out, processing parameter: 100w, 250mTorr, 10min; Heat deposition adhesion promotor Sliquest187 (GE) subsequently, processing parameter: 140 DEG C, 10 minutes.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that creative work can make still within protection scope of the present invention.
Claims (3)
1. an antireflection and self-cleaning glass, it is characterized in that, the impression materials of glass surface utilizes the nano-imprint process based on band shape soft mold form the nano-cone array structure of sub-wavelength or adopt hard mask and impression materials at glass surface and etch the nano-cone array structure of sub-wavelength based on the nano impression of band shape soft mold and hard mask transfer etching technics; Described nanocone is circular cone, and nanocone basal diameter is 100-300nm, depth-to-width ratio, and namely the height/diameter of nanocone is 4-12, and the distance between nanocone bottom center is 100-300nm; Described impression materials is ultraviolet photochemical polymer materials or sol-gel material or titanic oxide material or earth silicon material; Described band shape soft mold has the square or conical characteristic pattern of circle of array depression.
2. a manufacture method for antireflection according to claim 1 and self-cleaning glass, is characterized in that, it etches the nano-cone array structure of sub-wavelength based on band shape soft mold nano impression and hard mask transfer etching technics, comprises the steps:
Step (1): pre-treatment, deposits one or more layers hard mask layer at glass surface, forms glass substrate;
Step (2): liquid impression materials coating on a glass substrate;
Step (3): imprinting moulding:
(3-1) first, utilize impression mode by a glass substrate attached for the band shape soft mold pressure with circular or square recess feature, make the liquid impression materials extrusion packing be coated with on glass substrate in the recess feature of band shape soft mold;
(3-2) liquid impression materials is made to be filled in the recess feature of band shape soft mold completely, and guarantee that the impression materials on the band shape soft mold after filling completely and glass substrate remains bringing into conformal contact, utilize UV curing mode to solidify liquid impression materials, realize the complete curing molding of stamping structure;
(3-3) last, the feature structure of impression curing molding is separated with band shape soft mold, completes the demoulding;
Step (4): utilize etching technics to carry out coining pattern transfer, during etching, the etch rate of hard mask material is lower than glass substrate, to obtain the nano-cone array structure of sub-wavelength;
Step (5): aftertreatment;
The etching technics of described step (4) adopts reactive ion etching or sense coupling or wet etching;
In described step (4), the height of nanocone depends on material and the thickness of hard mask.
3. a manufacture method for antireflection according to claim 1 and self-cleaning glass, is characterized in that, it forms the nano-cone array structure of sub-wavelength at glass based on band shape soft mold nano-imprint process, comprise the steps:
Step (1): pre-treatment, increases the adhesion characteristics of glass substrate surface;
Step (2): liquid impression materials is coated on glass, described liquid impression materials is the coated material of glass substrate;
Step (3): imprinting moulding:
(3-1) first, utilize impression mode by a glass substrate attached for the band shape soft mold pressure with conical shaped depression shape feature, make the liquid impression materials extrusion packing be coated with on glass substrate in the feature pattern of depression;
(3-2) liquid impression materials is made to be filled in band shape soft mold completely, and guarantee that the liquid impression materials on the band shape soft mold after filling completely and glass remains bringing into conformal contact, utilize UV curing mode to solidify liquid impression materials, realize the complete curing molding of stamping structure;
(3-3) last, the feature structure of impression curing molding is separated with band shape soft mold, completes the demoulding;
Step (4): aftertreatment.
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| TWI610804B (en) * | 2016-05-23 | 2018-01-11 | 國立成功大學 | Energy-saving Glass and Method of Manufacturing the Same |
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