CN102998723A - Antireflection optical assembly and manufacturing method thereof - Google Patents
Antireflection optical assembly and manufacturing method thereof Download PDFInfo
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- CN102998723A CN102998723A CN2012104997706A CN201210499770A CN102998723A CN 102998723 A CN102998723 A CN 102998723A CN 2012104997706 A CN2012104997706 A CN 2012104997706A CN 201210499770 A CN201210499770 A CN 201210499770A CN 102998723 A CN102998723 A CN 102998723A
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Abstract
Provided are an antireflection optical assembly and a manufacturing method thereof. The antireflection optical assembly comprises a substrate, an antireflection layer located on the surface of the substrate and a covering layer located on the surface of the antireflection layer, wherein the antireflection layer comprises a zinc oxide nanorod array composed of a plurality of zinc oxide nanorods, and the covering layer is made of one or more of silicon oxide, titanium oxide, aluminum oxide and zirconium oxide. The manufacturing method comprises providing the substrate, enabling the antireflection layer with a moth eye structure to be formed on the surface of the substrate, and enabling the covering layer to be formed on the surface of the antireflection layer, wherein the antireflection layer comprises a protrusion array composed of a plurality of protrusions, and the covering layer is made of one or more of silicon oxide, titanium oxide, aluminum oxide and zirconium oxide.
Description
Technical field
The present invention relates to technical field of nano material, relate in particular to a kind of anti-reflection optical module and manufacture method.
Background technology
Light is usually understood some and is changed direction of propagation and return in the original medium when propagating on the interphase of different medium, this is called as reflection of light.Usually, the difference of refractive index is larger between the different medium, and light will be stronger in the reflection at this interphase place.In the fields such as photovoltaic device, display, how to reduce reflection of light is the focus of research always.
The compound eye of moth can be counted as the array structure that is formed by hexagonal nano structure projection ordered arrangement.This array is considered to the homogeneity hyaline layer of anterior corneal surface, and each nanostructured projection is equivalent to an antireflection unit.Such structure makes it seem unusually black so that the compound eye of moth has low reflective.Therefore, even moth also is difficult for being discovered in night flying.Such effect is called as moth eye effect.Compare with the conventional monolayers porous membrane structure, wider based on the spectral range that the antireflection layer of moth eye effect adapts to, incident angle is larger, and has super water-wet behavior, can realize automatically cleaning.
Below in conjunction with the different optical model of moth ocular structure, the principle of moth ocular structure antireflection effect is described.
With reference to figure 1, show a kind of equivalent schematic of moth ocular structure model.According to diffraction theory, when the surface of moth ocular structure 1 has the structural change of projection (the small stair difference in height in the moth ocular structure 1 approach or less than optical wavelength time), the structural change of this projection will cause the microvariations of Refractive Index of Material, can form the trend that increases successively to moth ocular structure 1 refractive index n 1, n2, n3, n4 from air, thereby reduce reflection of light.
With reference to figure 2, show the equivalent schematic of another kind of moth ocular structure model.When bump sizes further reduces, the density of projection further increases, and its structure is in general just more and more close to the continuous variation inclined-plane of moth ocular structure 2.This will cause in the refractive index of moth ocular structure 2 and be continuous variation along depth direction from n1 to n4, sharply change the reflex that causes thereby further reduce refractive index.
More technology about the moth ocular structure can the application reference publication No. be the Chinese patent application of CN102395905A.
Based on described moth eye effect, developed multiple bionics optics material, to play the effect that reduces the light reflection.With reference to shown in Figure 3, a kind of anti-reflection optical module can comprise in the prior art:
Substrate of glass 3;
Be positioned at the antireflection layer on substrate of glass 3 surfaces, described antireflection layer comprises the nanometic zinc oxide rod array that is comprised of a plurality of zinc oxide nano rods 4, and as shown in the figure, the height of these nanometer rods is different, thereby forms the antireflection layer of moth ocular structure.
But because the specific activity of zinc paste is larger, easily and acidic materials or alkaline matter carry out chemical reaction, and physical strength is low, thus the less stable of described antireflection layer finally causes the serviceable life of antireflection layer shorter.
Similarly, when antireflection layer adopts other material, also may there be the problems referred to above.
Summary of the invention
Therefore, need a kind of optical module and manufacture method thereof, can improve the stability of antireflection layer.In addition, in the stability that improves antireflection layer, it also will be favourable not affecting its anti-reflective effect.
According to an aspect of the present invention, provide a kind of anti-reflection optical module, having comprised:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer comprises the nanometic zinc oxide rod array that is comprised of a plurality of zinc oxide nano rods; And
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
Basic thought is that to increase material by the surface at nanometic zinc oxide rod array be one or more overlayer in monox, titanium dioxide, aluminium oxide and the zirconia; can play the effect of protection antireflection layer; avoid the direct and antireflection layer generation chemical reaction of acidic materials or alkaline matter; and can improve the anti-wear performance of antireflection layer; the final stability that improves antireflection layer, the serviceable life of prolongation anti-reflection optical module.In addition, described overlayer does not affect the super water-wet behavior of anti-reflection optics assembly surface, thereby can realize the self-cleaning function of anti-reflection optical module, and so that the anti-fog effect of anti-reflection optics assembly surface is remarkable.
In an example, described overlayer covers the top of described a plurality of zinc oxide nano rods, thereby has the space between described overlayer and two adjacent zinc oxide nano rods.Owing to have the space between overlayer and two adjacent zinc oxide nano rods, therefore described overlayer meeting is so that the variations in refractive index of anti-reflection optics assembly surface is abundanter, thereby improved the anti-reflection effect of antireflection layer.
According to another aspect of the present invention, provide a kind of anti-reflection optical module, having comprised:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer has the moth ocular structure, and described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections;
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
Basic thought is that to increase material by the antireflection layer surface at the moth ocular structure be one or more overlayer in monox, titanium dioxide, aluminium oxide and the zirconia; can play the effect of protection antireflection layer; avoid the direct and antireflection layer generation chemical reaction of acidic materials or alkaline matter; and can improve the anti-wear performance of antireflection layer; the final stability that improves antireflection layer, the serviceable life of prolongation anti-reflection optical module.In addition, described overlayer does not affect the super water-wet behavior of anti-reflection optics assembly surface, thereby can realize the self-cleaning function of anti-reflection optical module, and so that the anti-fog effect of anti-reflection optics assembly surface is remarkable.
In an example, described anti-reflection optical module also comprises: the low surface energy coat that is positioned at described cover surface.Owing to form low surface energy coat at described overlayer, thereby so that the surface of anti-reflection optical module hydrophilicly becomes super-hydrophobicly by super, keeping to realize antifreeze function under the constant prerequisite of self-cleaning function.
In an example, the material of described substrate is glass, and described antireflection layer is nanometic zinc oxide rod array, and described tectal material is monox, and can greatly reduce the production cost of anti-reflection optical module this moment.
In an example, described overlayer covers the top of described a plurality of projections, thereby has the space between described overlayer and two adjacent projections.Owing to have the space between overlayer and two adjacent projections, therefore described overlayer meeting is so that the variations in refractive index of anti-reflection optics assembly surface is abundanter, thereby improved the anti-reflection effect of antireflection layer.
According to a further aspect of the invention, provide a kind of manufacture method of anti-reflection optical module, having comprised:
Substrate is provided;
Form the antireflection layer with moth ocular structure at described substrate surface, described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections;
Surface at described antireflection layer forms overlayer, and described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
Basic thought is that to form material by the antireflection layer surface at the moth ocular structure be one or more overlayer in monox, titanium dioxide, aluminium oxide and the zirconia; can play the effect of protection antireflection layer; avoid the direct and antireflection layer generation chemical reaction of acidic materials or alkaline matter; and can improve the anti-wear performance of antireflection layer; the final stability that improves antireflection layer, the serviceable life of prolongation anti-reflection optical module.In addition, described overlayer does not affect the super water-wet behavior of anti-reflection optics assembly surface, thereby can realize the self-cleaning function of anti-reflection optical module, and so that the anti-fog effect of anti-reflection optics assembly surface is remarkable.
In an example, the manufacture method of described anti-reflection optical module also comprises: form low surface energy coat in described cover surface.Owing to form low surface energy coat at described overlayer, thereby so that the surface of anti-reflection optical module hydrophilicly becomes super-hydrophobicly by super, keeping to realize antifreeze function under the constant prerequisite of self-cleaning function.
Description of drawings
Fig. 1 is the structural representation of a kind of moth ocular structure in the prior art;
Fig. 2 is the structural representation of another kind of moth ocular structure in the prior art;
Fig. 3 is the structural representation of a kind of anti-reflection optical module in the prior art;
Fig. 4 is the schematic flow sheet of the manufacture method of anti-reflection optical module in one embodiment of the invention;
Fig. 5 is an exemplary structural representation behind the formation antireflection layer among Fig. 4;
Fig. 6 is an exemplary schematic flow sheet that forms antireflection layer among Fig. 4;
Fig. 7 is an exemplary structural representation behind the formation overlayer among Fig. 4;
Fig. 8 is another exemplary structural representation behind the formation overlayer among Fig. 4;
Fig. 9 is the schematic flow sheet of the manufacture method of anti-reflection optical module in another embodiment of the present invention;
Figure 10 is an exemplary schematic flow sheet that forms low surface energy coat among Fig. 9;
Figure 11 is the transmittance synoptic diagram of optical module under different wave length of different structure in the embodiment of the invention.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing the specific embodiment of the present invention is described in detail.
Set forth in the following description a lot of details so that fully understand the present invention, implement but the present invention can also adopt other to be different from alternate manner described here, so the present invention has not been subjected to the restriction of following public specific embodiment.
Hereinafter, be the demonstration purpose, product embodiments reference method embodiment describes.Yet, should be appreciated that the realization of product and method among the present invention is independent mutually.That is to say that disclosed product embodiments can prepare according to additive method, disclosed embodiment of the method is not limited only to realize product embodiments.
Employed moth ocular structure is by seamlessly arranging the relief pattern that is less than or equal to light wavelength (as: being less than or equal to 400nm) gap on the surface of carrying out the article that antireflection processes in the disclosure, thereby make the variation of borderline refractive index on external world's (as: air) and film surface as the continuous structure in simulation ground, can irrespectively make with refractive index interfaces roughly all transmissions of light, the lip-deep light reflection of these article is roughly eliminated.
Be elaborated below in conjunction with accompanying drawing.
With reference to shown in Figure 4, present embodiment one embodiment provides a kind of manufacture method of anti-reflection optical module, comprising:
Step S11 provides substrate;
Step S12 forms the antireflection layer with moth ocular structure at described substrate surface;
Step S13 forms overlayer on the surface of described antireflection layer.
Described overlayer both can protect antireflection layer not to be subjected to the chemical corrosion of the materials such as extraneous soda acid, can protect again antireflection layer not to be subjected to extraneous physical hazard, thereby improve the stability of antireflection layer, had prolonged the service time of antireflection layer.
At first execution in step S11 provides substrate.
The material of described substrate can be the transparent materials such as glass or plastics, also can be the opaque materials such as metal or pottery.
Present embodiment does not limit concrete shape, size and the thickness of substrate.
In order to guarantee the cleanliness of substrate, present embodiment can adopt the mixed solution of acetone, isopropyl acetone and deionized water that Ultrasonic Cleaning is carried out in described substrate, to remove the impurity of substrate surface, guarantee to obtain clean substrate, do not make the carrying out of described impurity effect subsequent step, its detailed process is known for those skilled in the art, does not repeat them here.
Then, present embodiment can adopt hydrofluorite (HF) or nitric acid (HNO
3) solution carries out roughening and process.Described hydrofluorite or salpeter solution can react with substrate, thereby so that substrate surface is more coarse.Process by described roughening, can increase the wettability of substrate, increase fastness and the homogeneity of follow-up rete in substrate surface formation.
Particularly, described substrate directly can be immersed in hydrofluorite or the salpeter solution in this example.Wherein, the weight percentage ranges of described hydrofluorite or nitric acid can be 5wt% ~ 20wt%; The time range that roughening is processed can be 30 minutes ~ 120 minutes; The temperature range that roughening is processed can be 20 ℃ ~ 80 ℃.
In addition, after carrying out the roughening processing, can also adopt the described substrate of washed with de-ionized water, to remove the residual acid solution of described substrate surface.
Follow execution in step S12, form the antireflection layer of moth ocular structure at substrate surface.
The material of described antireflection layer can be for zinc paste, silicon, monox, titanium dioxide, silicon nitride, tantalum oxide, zirconia, aluminium oxide, indium oxide, tin oxide, gallium oxide, tin-doped indium oxide, fluoridize tin-doped indium oxide, mix one or more the combination in any in fluorine indium oxide, Al-Doped ZnO, gallium-doped zinc oxide, zinc sulphide, zinc selenide and the magnesium fluoride.
The thickness range of described antireflection layer can be 100nm ~ 2000nm, such as 100nm, 500nm, 1000nm or 2000nm etc.
Described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections, and the shape of described projection can comprise: one or more in taper, cylindrical, prismatic, spherical, semisphere and the curved surface column.
Be the situation of uniform cross section cylindricality for this projection, for array of protrusions that these a plurality of projections are formed have the moth ocular structure, the height of these a plurality of projections is different.
Be unequal section cylindricality, taper, sphere, hemispheric situation for this projection, the height of each described projection can be identical, also can be different.For the projection of highly identical unequal section, because this protruding cross section is with height change, the refractive index in the reflection horizon that is comprised of array of protrusions also changes in short transverse, thereby this reflection horizon has the moth ocular structure.
Need to prove that the height of described projection is identical, and to refer to the height of projection roughly the same, for example, the difference in height between the projection is in 5% scope.
Described antireflection layer specifically can adopt at least a method in chemical vapor deposition, spin coating, sprinkling, wet chemical method, chemical solution glue gel, chemical liquid deposition, photoengraving, template, physical vapour deposition (PVD), evaporation or the sputter mode to form.
With reference to shown in Figure 5, the material of substrate described in the present embodiment 11 is glass, the material of described antireflection layer is zinc paste, described protruding 12 be shaped as is cylindrical, be that described antireflection layer is nanometic zinc oxide rod array, and the height of each projection 12 is different, thereby can further improve anti-reflective effect.Particularly, with reference to shown in Figure 6, the step that forms described reflection horizon in the present embodiment can comprise:
Step S221 is dissolved in the ethanolic solution to major general's zinc salts of organic acid, forms seed-solution;
Step S222 is formed on substrate surface with described seed-solution;
Step S223 carries out heat treated to described substrate, forms zinc oxide crystal seed at described substrate surface;
Step S224 mixes inorganic zinc salt and alkaline solution, forms growth solution;
Step S225 is placed on described substrate in the described growth solution, forms the nano-array rod of zinc paste on described zinc oxide crystal seed surface.
At first, configuration seed-solution.
In dehydration acetate zinc and the zinc propionate one or both can be dissolved in the ethanolic solution in the present embodiment, to form seed-solution.
Particularly, the volumetric molar concentration scope of zinc salts of organic acid can be 2 mM/ls ~ 10 mol/L in the described seed-solution, as: 2 mM/ls, 10 mM/ls, 500 mM/ls, 3 mol/L, 7 mol/L or 10 mol/L.
In other embodiments of the invention, when being dissolved in zinc salts of organic acid in the ethanolic solution, monoethanolamine also can also be dissolved in the ethanol, namely comprise monoethanolamine in the seed-solution, thereby can catalysis generate ZnO.
Then, by spin coating, sprinkling or infiltration described seed-solution is formed on substrate surface, it is known for those skilled in the art, does not repeat them here.
Then, carry out heat treated.
The temperature range of heat treated described in the present embodiment can be 300 ℃ ~ 400 ℃, as: 300 ℃, 350 ℃ or 400 ℃; Time range can be 30 minutes ~ 60 minutes, as: 30 minutes, 45 minutes or 60 minutes.
By described heat treated, zinc salts of organic acid will thermal decomposition form ZnO, thereby just can form zinc oxide crystal seed at described substrate surface.
Zinc oxide crystal seed described in the present embodiment can comprise 1 layer ~ 5 layers zinc oxide nano-particle.
Then, configuration growth solution.
Described inorganic zinc salt can be one or more the combination in any in zinc nitrate hexahydrate, six water zinc sulphates and the six water zinc chloride; Described alkaline solution can be one or more the combination in any in hexamethylene tetramine, hydrogen-oxygen potassium and the NaOH; The volume mol ratio of described inorganic zinc salt and described alkaline solution can be 0.9 ~ 1.1.
Present embodiment can mix zinc nitrate hexahydrate and urotropine equal-volume molar weight.
Then, described substrate is placed in the described growth solution, forms the nanometer stick array of zinc paste on described zinc oxide crystal seed surface.
Need to prove, in other embodiments of the invention, can also pass through chemical deposition, hydro-thermal method, solvent-thermal method, electrochemical method or template, so that described growth solution forms the nanometer stick array of zinc paste on described zinc oxide crystal seed surface.
The time range that substrate described in the present embodiment is placed in the described growth solution can be 120 minutes ~ 300 minutes, as: 120 minutes, 200 minutes or 300 minutes; Temperature range can be 80 ℃ ~ 95 ℃, as: 80 ℃, 90 ℃ or 95 ℃.
Described substrate is placed on the thickness of the Time dependent antireflection layer in the described growth solution, and the time is longer, and thickness is larger.
The solubility inorganic zinc salt generates the nanometer stick array of zinc paste in the present embodiment under the alkaline solution environment, and oriented growth under the inducing of zinc oxide crystal seed forms described antireflection layer.
Need to prove that present embodiment can according to concrete needs, form described antireflection layer on all or part of surface of substrate.
Then execution in step S13 forms overlayer on the surface of described antireflection layer.
Described tectal activity of materials should be lower, and physical strength is higher.Particularly, described tectal material can be in monox, titanium dioxide, aluminium oxide and the zirconia one or more.
Described tectal thickness range can not be too little, otherwise can not protect well antireflection layer; Described tectal thickness range also need not be too large, otherwise can improve production cost, and may affect the anti-reflection effect of antireflection layer.Particularly, described tectal thickness range can be 5nm ~ 200nm, as: 5nm, 50nm, 100nm or 200nm.
In an object lesson; with reference to shown in Figure 7; described overlayer 13a covers described a plurality of top of protruding 12; thereby there is space 14 between described overlayer 13a and two adjacent projections 12; though this moment, described overlayer 13a did not cover all surfaces of projection 12; but described protruding 12 surface does not directly expose outside, and therefore described overlayer 13a still can play the effect in protection reflection horizon.Particularly, the top of the projection 12 that described overlayer 13a covers can refer to 10%, 20%, 40% or 50% etc. of whole height of projection, thus the variable size in space 14.
In another object lesson; with reference to shown in Figure 8; described overlayer 13b covers described protruding 12 all surfaces, and covers the upper surface of substrate 11 between two adjacent projections 12, thereby described overlayer 13b can protect the reflection horizon not to be subjected to extraneous infringement well.
Described overlayer can adopt lift film, at least a method in spin coating or the spray pattern forms.
Tectal material described in the present embodiment is monox, adopts to lift the mode of filming and form described tectal step and can comprise: the substrate that will comprise described antireflection layer is placed in the silica sol, after 5 minutes ~ 50 minutes, takes out described substrate.
Described silica sol is comprised of silicon oxide particle and water, and it is a kind of nano dispersion fluid, has again the characteristic of common sol.
The particle diameter of silicon oxide particle can not be too large in the described silica sol, otherwise silicon oxide particle can't be filled the space between adjacent two projections, so the particle diameter of silicon oxide particle should be less than described tectal thickness; The particle diameter of silicon oxide particle can not be too little in the described silica sol, otherwise can increase the number of times that lifts coating process, reduces production efficiency.Described in the present embodiment in the silica sol particle size range of silicon oxide particle can be 5nm ~ 50nm, such as 5nm, 20nm, 35nm or 50nm.
The mass percent of silicon oxide particle can not be too large in the described silica sol, otherwise the thickness of the antireflection layer that forms can be too large; The mass percent of silicon oxide particle can not be too little in the described silica sol, otherwise can increase the number of times that lifts coating process, reduces production efficiency.The mass percent of silicon oxide particle described in the present embodiment can be 0.01% ~ 5%, as: 0.01%, 0.5%, 2% or 5%.
For described silicon oxide particle can be adhered on the described antireflection layer better, by the pH value of control silica sol, can make antireflection layer and silicon oxide particle in silica sol, present different electrically.In addition, zinc oxide material is very sensitive to pH value, and when the pH value of solution was improper, meeting was so that antireflection layer is dissolved falls.The pH value of silica sol described in the present embodiment can be 5 ~ 9, as: 5,7 or 9, so that the antireflection layer of zinc oxide material is electronegative in this silica sol, and silicon oxide particle positively charged in silica sol, thereby inhale mutually principle according to the charges of different polarity, can guarantee that silicon oxide particle stably is formed on the described antireflection layer.
Present embodiment can carry out annealing in process after forming described overlayer, temperature range can be 300 ℃ ~ 600 ℃, as: 300 ℃, 400 ℃, 500 ℃ or 600 ℃; Time range can be 120 minutes ~ 720 minutes, as: 120 minutes, 400 minutes or 720 minutes.By the annealing in process of this moment, can promote overlayer dry, and can strengthen the intensity of anti-reflection optical module.
Need to prove that in other embodiments of the invention, in order to simplify step, can form under antireflection layer and the tectal prerequisite at substrate surface guaranteeing, described cleaning treatment, roughening process or step corresponding to annealing in process all can be omitted.
Increase overlayer by the antireflection layer surface at the moth ocular structure in the present embodiment; can play the effect of protection antireflection layer; avoid the direct and antireflection layer generation chemical reaction of acidic materials or alkaline matter; and can improve the anti-wear performance of antireflection layer; the final stability that improves antireflection layer, the serviceable life of prolongation anti-reflection optical module.
In addition, described overlayer is so that the variations in refractive index of anti-reflection optics assembly surface is abundanter, thereby improved the anti-reflection effect of antireflection layer.
Further, described overlayer does not affect the super water-wet behavior of anti-reflection optics assembly surface, thereby can realize the self-cleaning function of anti-reflection optical module, and so that the anti-fog effect of anti-reflection optics assembly surface is remarkable.
Further, the material of substrate is glass in the present embodiment, and antireflection layer is nanometic zinc oxide rod array, tectal material is monox, because above-mentioned material is all very cheap, and manufacturing process is simple, thereby can greatly reduce the production cost of anti-reflection optical module.
With reference to shown in Figure 9, a kind of manufacture method of anti-reflection optical module is provided among another embodiment of present embodiment, comprising:
Step S21 provides substrate;
Step S22 forms the antireflection layer with moth ocular structure at described substrate surface;
Step S23 forms overlayer on the surface of described antireflection layer;
Step S24 forms low surface energy coat in described cover surface.
Step S21, step S22 are identical with step S13 with above-mentioned steps S11, step S12 respectively with step S23 in the present embodiment, do not repeat them here.
After forming overlayer, then execution in step S24 forms low surface energy coat.
The material of described low surface energy coat can be one or more the combination in any in methoxy silane, alkyl silane, fluorine containing silane or the grafted silicone chain compound.
Described low surface energy coat also can adopt at least a method in chemical vapor deposition, spin coating, sprinkling, wet chemical method, chemical solution glue gel, chemical liquid deposition, photoengraving, template, physical vapour deposition (PVD), evaporation or the sputter mode to form.
When carbochain is too short in the low-surface-energy material, will cause surface energy too high, not have hydrophobic effect; The link fracture then occurs when carbochain is long easily, less stable.Select cetyl trimethoxy silane (Hexadecyltrimethoxysilane, HDTMS) as low-surface-energy material in the present embodiment, the carbon chain lengths of HDTMS is moderate, thereby both can play hydrophobic effect, and stability is also relatively good.
With reference to shown in Figure 10, the step that forms low surface energy coat in described cover surface can comprise:
Step S241 provides the cetyl trimethoxy silane;
Step S242 adds ethanol and forms solution in the cetyl trimethoxy silane;
Step S243 carries out acidification to described solution;
Step S244 carries out stir process to the solution after the acidification;
Step S245, the mode by infiltration, spin coating or sprinkling is formed on described cover surface with described solution.
At first, providing chemical structural formula is CH
3(CH
2)
15Si (OCH
3)
3HDTMS.
Then, the inventor studies and finds that HDTMS is soluble in ethanol, therefore adds ethanol in HDTMS, thereby can obtain comprising the solution of HDTMS.Particularly, the mass percent scope of cetyl trimethoxy silane can be 3%～5% in the described solution.
Then, described solution is carried out acidification, so that HDTMS is hydrolyzed, and generate the reactive group hydroxyl.Particularly, in described solution, add at least a in acetic acid, hydrochloric acid or the nitric acid, until the pH value of solution is positioned between 4.5 ~ 5.5, as: pH value is 4.5,5.0 or 5.5.
Then, the solution after the acidification is carried out stir process, so that the HDTMS hydrolysis is abundant and even.Particularly, the solution after the acidification is put into stirring apparatus, this solution is carried out stirring more than 60 minutes.
Then, treat that mentioned solution preparation is finished after, just it can be formed on described cover surface, with as low surface energy coat.Particularly, can by in infiltration, spin coating or the spray pattern any, described solution be formed on described cover surface.
When adopting pattern of invasion that described solution is formed on described cover surface, described substrate is placed in the described solution, more abundant in order to guarantee reaction, can be 30 minutes ~ 60 minutes standing time, as: 30 minutes, 40 minutes, 50 minutes or 60 minutes.This operation can directly be carried out at normal temperatures, need not other devices, and is simple to operate, and can guarantee that low surface energy coat is very even in the distribution of cover surface.
When adopting spin coating or spray pattern that described solution is formed on described cover surface, required time is shorter, and efficient is higher, also can guarantee the homogeneity that low surface energy coat distributes in cover surface simultaneously.
So far, formed low surface energy coat in cover surface.The thickness of described low surface energy coat is the molecule rank, is specifically as follows 10nm ~ 500nm, as: 10nm, 50nm, 100nm, 250nm or 500nm.
Further, after cover surface forms low surface energy coat, can also at room temperature described low surface energy coat be dried, then be cured processing.Particularly, the time range that described curing is processed can be 30 minutes ~ 60 minutes, as: 30 minutes, 40 minutes, 50 minutes or 60 minutes; Temperature range can be 100 ℃ ~ 150 ℃, as: 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃.
Process by described curing, can increase low surface energy coat in the set of cover surface, prevent coming off of low surface energy coat.
In the present embodiment by forming low surface energy coat in cover surface, can make surface that antireflection learns assembly by super hydrophilic become super-hydrophobic, thereby keeping can realizing better antifreezing effect under the constant prerequisite of self-cleaning function.
Although low surface energy coat is directly exposed in the external environment in the present embodiment; and the corrosion resistivity of low surface energy coat and wearing quality are all relatively good; but because the thinner thickness of low surface energy coat; if there is not tectal protection; acidic materials or alkaline matter etc. still can penetrate in the antireflection layer by low surface energy coat; thereby affect the stability of antireflection layer; shorten its serviceable life; therefore overlayer described in the present embodiment still can protect antireflection layer not to be subjected to extraneous infringement well, and can further improve the anti-reflection effect of antireflection layer.
Correspondingly, present embodiment one embodiment provides a kind of anti-reflection optical module, comprising:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer has the moth ocular structure, and described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections;
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
Wherein, described tectal thickness range can be 5nm ~ 200nm.
Wherein, the material of described substrate can be glass, metal, pottery or plastics.When the material of substrate was the transparent materials such as glass or plastics, described antireflection layer can also play anti-reflection effect.
Wherein, the material of described antireflection layer can be for zinc paste, silicon, monox, titanium dioxide, silicon nitride, tantalum oxide, zirconia, aluminium oxide, indium oxide, tin oxide, gallium oxide, tin-doped indium oxide, fluoridize tin-doped indium oxide, mix one or more the combination in any in fluorine indium oxide, Al-Doped ZnO, gallium-doped zinc oxide, zinc sulphide, zinc selenide and the magnesium fluoride.
Wherein, the thickness range of described antireflection layer can be 100nm ~ 2000nm.
Wherein, the shape of described projection comprises: one or more in taper, cylindrical, prismatic, spherical, semisphere and the curved surface column.
Described overlayer can cover the surface (comprising upper surface and side surface) of described projection fully, also can only cover the top of described a plurality of projections, thereby have the space between described overlayer and two adjacent projections.
Further, the anti-reflection optical module can also comprise in the present embodiment: be positioned at the low surface energy coat of described cover surface, so that the surface of anti-reflection optical module becomes hydrophobicity from water wettability, thereby realize antifreeze effect.
Wherein, the material of described low surface energy coat can be one or more the combination in any in methoxy silane, alkyl silane, fluorine containing silane and the grafted silicone chain compound.
Wherein, the thickness range of described low surface energy coat can be 10nm ~ 500nm.
Preferably, the material of described substrate is glass, and described antireflection layer is nanometic zinc oxide rod array, and described tectal material is monox, thereby can reduce production costs.
The anti-reflection optical module can adopt method manufacturing shown in Figure 9 in the present embodiment, does not repeat them here.
In the present embodiment owing to increased overlayer on the antireflection layer surface, thereby improved the stability of antireflection layer, and prolonged its serviceable life.
Another embodiment provides a kind of anti-reflection optical module, comprising:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer comprises the nanometic zinc oxide rod array that is comprised of a plurality of zinc oxide nano rods; And
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
In an example, described tectal material is monox.
In an example, described tectal thickness range is 5nm-200nm.
Wherein, the height of a plurality of zinc oxide nano rods of described nanometic zinc oxide rod array can be identical, also can be different.Preferably, the height of a plurality of zinc oxide nano rods of described nanometic zinc oxide rod array is different, thereby described antireflection layer can be brought into play better according to moth ocular structure principle the effect of anti-reflection.
Wherein, described overlayer can cover the surface (comprising upper surface and side surface) of described zinc oxide nano rod fully; Also can only cover the top of described a plurality of zinc oxide nano rods, thereby there is the space between described overlayer and two adjacent zinc oxide nano rods, therefore described overlayer meeting is so that the variations in refractive index of anti-reflection optics assembly surface is abundanter, thereby improved the anti-reflection effect of antireflection layer.
Owing to tectal existence, can play the effect of protection antireflection layer in the above-mentioned anti-reflection optical module.
In addition, described overlayer can also improve the anti-reflection effect of antireflection layer.With reference to shown in Figure 11, horizontal ordinate represents wavelength, and unit is nm; Ordinate represents the transmittance of optical module, and unit is %.The transmittance of optical module under different wave length that curve 5 expressions wherein only are made of substrate, curve 6 expression is only by substrate be positioned at the transmittance of optical module under different wave length that suprabasil antireflection layer consists of, curve 7 expressions are successively by substrate, antireflection layer and thickness are the transmittance of optical module under different wave length that the overlayer of H1 consists of, curve 8 expressions are successively by substrate, antireflection layer and thickness are the transmittance of optical module under different wave length that the overlayer of H2 consists of, curve 9 expressions are successively by substrate, antireflection layer and thickness are the transmittance of optical module under different wave length that the overlayer of H3 consists of, wherein, H1＜H2＜H3.
Can sufficient proof by comparison curves 5 ~ curve 9: after the surface at antireflection layer forms overlayer, can improve the anti-reflection effect of described optical module; Under the prerequisite of thickness in the 5nm-200nm scope of ensuring coverage layer, along with the increase of cover thickness, the anti-reflection effect of described optical module can further improve.
Although the present invention discloses as above with preferred embodiment, yet is not to limit the present invention.Any those of ordinary skill in the art, do not breaking away from the technical solution of the present invention scope situation, all can utilize method and the technology contents of above-mentioned announcement that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical solution of the present invention according to any simple modification, equivalent variations and the modification that technical spirit of the present invention is done above embodiment, all still belongs in the scope of technical solution of the present invention protection.
Claims (24)
1. an anti-reflection optical module is characterized in that, comprising:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer comprises the nanometic zinc oxide rod array that is comprised of a plurality of zinc oxide nano rods; And
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
2. anti-reflection optical module as claimed in claim 1 is characterized in that, described tectal material is monox.
3. anti-reflection optical module as claimed in claim 1 is characterized in that, described tectal thickness range is 5nm-200nm.
4. anti-reflection optical module as claimed in claim 1 is characterized in that, the height of a plurality of zinc oxide nano rods of described nanometic zinc oxide rod array is different, thereby described antireflection layer has the moth ocular structure.
5. anti-reflection optical module as claimed in claim 1 is characterized in that, described overlayer covers the top of described a plurality of zinc oxide nano rods, thereby has the space between described overlayer and two adjacent zinc oxide nano rods.
6. an anti-reflection optical module is characterized in that, comprising:
Substrate;
Be positioned at the antireflection layer of described substrate surface, described antireflection layer has the moth ocular structure, and described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections;
Be positioned at the overlayer on described antireflection layer surface, described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
7. anti-reflection optical module as claimed in claim 6 is characterized in that, described tectal thickness range is 5nm ~ 200nm.
8. anti-reflection optical module as claimed in claim 6 is characterized in that, the material of described substrate is glass, metal, pottery or plastics.
9. anti-reflection optical module as claimed in claim 6, it is characterized in that the material of described antireflection layer is zinc paste, silicon, monox, titanium dioxide, silicon nitride, tantalum oxide, zirconia, aluminium oxide, indium oxide, tin oxide, gallium oxide, tin-doped indium oxide, fluoridize tin-doped indium oxide, mix one or more the combination in any in fluorine indium oxide, Al-Doped ZnO, gallium-doped zinc oxide, zinc sulphide, zinc selenide and the magnesium fluoride.
10. anti-reflection optical module as claimed in claim 6 is characterized in that, the thickness range of described antireflection layer is 100nm ~ 2000nm.
11. anti-reflection optical module as claimed in claim 6 is characterized in that, also comprises: the low surface energy coat that is positioned at described cover surface.
12. anti-reflection optical module as claimed in claim 11 is characterized in that, the material of described low surface energy coat is one or more the combination in any in methoxy silane, alkyl silane, fluorine containing silane and the grafted silicone chain compound.
13. such as claim 11 or 12 described anti-reflection optical modules, it is characterized in that the thickness range of described low surface energy coat is 10nm ~ 500nm.
14. anti-reflection optical module as claimed in claim 6 is characterized in that, the shape of described projection comprises: one or more in taper, cylindrical, prismatic, spherical, semisphere and the curved surface column.
15. anti-reflection optical module as claimed in claim 14 is characterized in that described overlayer covers the top of described a plurality of projections, thereby has the space between described overlayer and two adjacent projections.
16. anti-reflection optical module as claimed in claim 6 is characterized in that, the material of described substrate is glass, and described antireflection layer is nanometic zinc oxide rod array, and described tectal material is monox.
17. the manufacture method of an anti-reflection optical module is characterized in that, comprising:
Substrate is provided;
Form the antireflection layer with moth ocular structure at described substrate surface, described antireflection layer comprises the array of protrusions that is comprised of a plurality of projections;
Surface at described antireflection layer forms overlayer, and described tectal material is one or more in monox, titanium dioxide, aluminium oxide and the zirconia.
18. the manufacture method of anti-reflection optical module as claimed in claim 17 is characterized in that, described antireflection layer is nanometic zinc oxide rod array; The step that forms described antireflection layer comprises:
Zinc salts of organic acid is dissolved in the ethanolic solution, forms seed-solution;
Described seed-solution is formed on substrate surface;
Heat treated is carried out in described substrate, form zinc oxide crystal seed at described substrate surface;
Inorganic zinc salt and alkaline solution are mixed, form growth solution;
Described substrate is placed in the described growth solution, forms nanometic zinc oxide rod array on described zinc oxide crystal seed surface.
19. the manufacture method of anti-reflection optical module as claimed in claim 17 is characterized in that, described overlayer adopt lift film, at least a method in spin coating or the spray pattern forms.
20. the manufacture method of anti-reflection optical module as claimed in claim 17 is characterized in that, described tectal material is monox; Forming described tectal step comprises: the substrate that will comprise described antireflection layer is placed in the silica sol, after 5 minutes ~ 50 minutes, takes out described substrate.
21. the manufacture method of anti-reflection optical module as claimed in claim 20 is characterized in that, the particle size range of silicon oxide particle is 5nm ~ 50nm in the described silica sol, and the mass percent of silicon oxide particle is 0.01% ~ 5%, and the pH value of silica sol is 5 ~ 9.
22. the manufacture method of anti-reflection optical module as claimed in claim 17 is characterized in that, after forming described overlayer, also comprise: carry out annealing in process, temperature range is 300 ℃ ~ 600 ℃, and time range is 120 minutes ~ 720 minutes.
23. the manufacture method of anti-reflection optical module as claimed in claim 17 is characterized in that, also comprises: form low surface energy coat in described cover surface.
24. the manufacture method of anti-reflection optical module as claimed in claim 23 is characterized in that, the material of described low surface energy coat is the cetyl trimethoxy silane; The step that forms described low surface energy coat comprises:
The cetyl trimethoxy silane is provided;
In the cetyl trimethoxy silane, add ethanol and form solution;
Described solution is carried out acidification;
Solution after the acidification is carried out stir process;
Mode by infiltration, spin coating or sprinkling is formed on described cover surface with described solution.
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