CN104846336A - Anti-reflective micro-nano structure of sapphire surface and preparation method thereof - Google Patents
Anti-reflective micro-nano structure of sapphire surface and preparation method thereof Download PDFInfo
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Abstract
The invention provides an anti-reflective micro-nano structure of sapphire surface and a preparation method thereof. The method comprises the following steps: preparing a layer of metal aluminium membrane on surface of the sapphire; performing twice anodization on the metal aluminium membrane to form an ordered porous alumina film with uniform surface; and performing a two-step heat treatment on the porous alumina film to form the sapphire with surface having the poriform micro-nano structure. The preparation method has the advantages of simple process and can obviously reduce the preparation cost; the prepared sapphire has the micro-nano structure on the surface, has obvious anti-reflective anti-reflection effect on visible light or middle-infrared band, and self cleaning property for the surface is better.
Description
Technical field
The present invention relates to optical window field, especially a kind of sapphire surface antireflection micro-nano structure and preparation method thereof.
Background technology
Sapphire, also known as alumina single crystal, there is the over-all propertieies such as excellent machinery, physics and chemistry, as large in hardness, stable chemical nature, good wave transmission rate in the wide wavelength band of ultraviolet-visible light-medium-wave infrared, thus can be used for preparing various optics, as: optical detection window, display screen and touch panel etc.But, compared to current opticglass, surface light reflection loss (double-sided reflecting rate R=14.3%) that sapphire causes it larger due to the larger specific refractory power of its material itself (1.77@550nm), transmitance, less than 86.0%, limits sapphire and applies widely.More seriously, the Service Environment of infrared acquisition optical window more and more severe (as high-speed and high-temperature), now the transmittance of the candidate material such as sapphire reduces with the rising of envrionment temperature; In addition, along with angle of light degree increases, transmitance sharply declines.Antireflection sub-wavelength micro-nano structure is prepared at sapphire surface, the reflection of light can be reduced, improve transmittance, there is the characteristic such as wide visual field and wide band high transmission, many deficiencies of traditional anti-reflective film layer can be overcome: the problems such as erosion as not good, easy in rete adhesion property and diffusion.Meanwhile, due to the existence of surperficial sub-wavelength structure, sapphire surface pattern will be changed, and then the wettability of sapphire material can be improved, thus be expected to realize its self-cleaning effect.
At present, the general method adopting etching, at sapphire substrate surface preparation antireflection micro-nano structure; Concrete lithographic method can be divided into wet etching and dry etching.
Wet etching utilizes suitable chemical reagent first to be decomposed container portion not covered by photoresist, then forms the compound of solubility to reach the object of removal.As utilized SiO
2graphical film, as mask, adopts H
2sO
4+ H
3pO
4mixing solutions wet etching Sapphire Substrate, by Graphic transitions in Sapphire Substrate; Recycle the SiO of rare HF acid solution etching away remnants
2film.This lithographic technique, therefore can by the control of the choosing of chemical reagent, proportioning and temperature to reach suitable etch rate and good etching selection ratio mainly by the chemical reaction of etching liquid and wafer material.The advantage of wet etching is that program is single, and equipment is simple, and cost is low, and output is high, and has good etching selection ratio; But wet etching is generally isotropic simultaneously, while litho pattern is transferred on wafer, etching also towards laterally carrying out, can cause aliasing, even making live width inconsistent like this.In addition, the potential safety hazard that the Working environment of high-temperature strong acid causes, limits the application popularization of this technology.
Dry etching many employings reactive ion etching (RIE) and inductively coupled plasma etching (ICP) method.The high energy ion that reactive ion etching uses, plasma damage can be produced to substrate material, prepared device performance is caused to be degenerated, thus be necessary to find a kind of alternative high density plasma etch system in conjunction with high quality and low etch damage feature, i.e. inductively coupled plasma etching.It has plurality of advantages: as etch rate is relatively high, operating air pressure is lower, and etching parameters easily controls.But in general, dry etching is easy to sapphire surface, particularly mesa edge position, causes certain pollution and damage.The more important thing is, because sapphire hardness is comparatively large, for etching sapphire ICP etching machine in test, compared to general etching machine costly; Also need to prepare etch mask simultaneously, test overall cost higher.
Summary of the invention
In order to solve above-mentioned prior art Problems existing, one of them object of the present invention is to provide a kind ofly does not damage that sapphire substrate, preparation technology are simple, the preparation method of the sapphire surface antireflection micro-nano structure of low cost.
Embodiment provided by the invention is as follows:
1, a kind of preparation method of sapphire surface antireflection micro-nano structure is provided, comprises:
Splash-proofing sputtering metal aluminium film on sapphire substrate; Wherein, described aluminium film, thickness is 50 ~ 1000nm; Fig. 2 for institute's embodiment prepare sapphire surface micro-nano structure process evolution SEM typical case pattern.Surface topography test result shows, in order to realize the antireflection micro-nano structure for different wave length preferably at sapphire surface, be necessary the aluminium film preparing different thickness, preferably 50 ~ 1000nm, general infrared wavelength antireflection micro-nano structure requires that aluminium film is relatively thick.
2, by described sapphire surface metallic aluminium film, the ordered porous aluminum oxide film of surface uniform is formed through twice anodic oxidation.Anodic oxidation can occur under numerous conditions; But adopt twice anonizing, be more conducive to the uniform sequential degree improving cavernous structure.
Anodic oxidation should select the low pH value electrolytic solution such as oxalic acid, to be conducive to the cavernous structure preparing small diameter; Lower anodizing temperature (-5 ~ 15 DEG C), can ensure the uniform sequential degree of cavernous structure; Suitable anodic oxidation voltage (30 ~ 60V), can avoid the less and excessive cavernous structure out-of-shape caused respectively of voltage and destroy the shortcoming of poroid structural integrity; And increase anodizing time (5 ~ 30min), be conducive to improving anodic oxidation degree and increasing the cavernous structure degree of depth.In addition, change pore-enlargement (20 ~ 90min) can realize the control to cavernous structure occupy-place ratio.Wherein preferred two step anodization step comprise:
First described aluminium film is carried out twice anodic oxidation in the oxalic acid of 0.2 ~ 0.5mol/L, the wherein oxalic acid of preferred 0.3mol/L, anodizing temperature is-5 ~ 15 DEG C, and anodic oxidation voltage is 30 ~ 60V, anodizing time is 5 ~ 30min; In the phosphoric acid of 3 ~ 8wt.%, carry out reaming more subsequently, wherein the phosphoric acid of preferred 5wt.%, pore-enlargement is 20 ~ 90min, thus forms the surperficial aluminum oxide film had compared with even porous structure.Wherein the implication of wt.% is mass percent.
3, by porous alumina polycrystal film orderly for described surface uniform, through double annealing thermal treatment, thus the poroid antireflection micro-nano structure of sapphire surface is formed.When preparing sapphire surface micro-nano structure, adopt double annealing thermal treatment important in inhibiting.Annealing thermal treatment can occur under numerous conditions, but contriver finds in practice, notice that the selection of following parameter will be conducive to improving the quality of sapphire surface micro-nano structure: be necessary that antianode is oxidized the cavernous structure obtained and adopts two-step thermal processing, that is: first low-temperature heat treatment high-temperature heat treatment again.
Low-temperature heat treatment can make remaining aluminium film fully oxidized; Wherein temperature is higher, and the time longer (400 ~ 600 DEG C, 2 ~ 24h), degree of oxidation is more abundant, but melts to prevent aluminium film no more than 600 DEG C.High-temperature heat treatment (800 ~ 1000 DEG C, insulation 1 ~ 6h) aluminum oxide polycrystal film can be made fully to change aluminium oxide single crystal film into, wherein temperature is higher, time is longer, react more thorough, the aluminium oxide single crystal film quality obtained is higher, and surface Raman peak shape is more close to sapphire itself (as shown in Figure 3); But simultaneous temperature unsuitable too high (>1100 DEG C), in order to avoid destroy the integrity of hole microstructure.Wherein preferred double annealing heat treatment step comprises:
First carry out low-temperature heat treatment, under 400 ~ 600 DEG C of conditions be incubated 2 ~ 24h, by fully oxidized for Al film remaining for anodic oxidation reactions be aluminum oxide polycrystal film;
Carry out high-temperature heat treatment again, under 800 ~ 1000 DEG C of conditions, be incubated 1 ~ 3h, thus the poroid aluminum oxide polycrystal film in surface that will obtain, be fully converted into aluminium oxide single crystal film.
Another object of the present invention is to provide a kind of sapphire surface antireflection micro-nano structure, and described sapphire adopts above-mentioned method to prepare.
Further, described sapphire has even cavernous structure, and the distance between its adjacent holes is 80 ~ 160nm.Further, pore size is 30 ~ 100nm.Further, the degree of depth in hole is 50 ~ 1000nm.
After Fig. 4 (a) and Fig. 4 (b) is through process optimization respectively, the sapphire surface antireflection micro-nano structure prepared by embodiment 8 and 14.Can find out that surperficial poroid micro-nano structure is preserved comparatively good, all substantially comparatively in order evenly, wherein owing to only changing anodizing time when anodic oxidation, so both pore sizes are about 60nm, pitch of holes is about 100nm; And corresponding hole depth is respectively H=650nm and 86nm.
Fig. 5 is embodiment 1, sapphire surface micro-nano structure infrared light transmission rate prepared by example 7, example 8 and example 9 compares; Wherein different embodiment only changes the pore-enlargement (respectively corresponding 40min, 30min, 50min and two-sided repetitive operation) in anode oxidation process, surface hole defect occupy-place ratios corresponding different respectively, that is: F=0.55, F=0.5, F=0.6 and F=0.6 (two-sided).Can find out, corresponding medium-wave infrared average transmittance reaches 88.7% respectively, and 86.2%, 91.2% and 92.4%; Compared to sapphire itself (85.5%), along with the increase of surface hole defect occupy-place ratio improves within the scope of this, all there is raising in various degree.Wherein, example 8 and the sapphire surface antireflection micro-nano structure prepared by example 9, improve 6.7% and 8.0% respectively, reaches in the anti-reflection effect of the effective antireflection of infrared band.
Fig. 6 compares for sapphire surface micro-nano structure (as shown in Figure 4) the visible ray wave transmission rate with different hole depth after process optimization prepared by embodiment 8 and 14.Can find out, hole depth can have influence on antireflection antireflective effect.And for the sapphire surface micro-nano structure prepared by embodiment 14, compared to sapphire visible ray (400 ~ 800nm) average transmittance (85.8%), its transmittance reaches 96.8%, improves 12.8%, achieves more significant antireflective effect.
Fig. 7 is the hydrophilic wetting angle test result with the sapphire surface micro-nano structure (as shown in Figure 4) of different hole depth after process optimization prepared by embodiment 8 and 14.Can find out, compared to the wetting angle (61.4 °) of sapphire with water itself, prepared antireflection micro-nano structure, all effectively can reduce wetting angle (being only 14.8 ° and 15.2 °).Wherein embodiment 8, due to larger hole depth, contact surface area is larger; Under similarity condition, the liquid such as water are more easily sprawled at sapphire micro-nano structure surface, thus can be air-dry sooner while dedusting, reach the better effect of automatically cleaning.Beneficial effect of the present invention:
The preparation method of sapphire surface antireflection micro-nano structure of the present invention, be different from and at present usual adopted directly wet etching or dry etching carried out to Sapphire Substrate both at home and abroad, but first adopt twice anonizing at sapphire surface preparation uniform cavernous structure comparatively in order, by double annealing process, aluminum oxide film is oxidized to the sapphire that surface has vesicular structure again, obtains sapphire surface micro-nano structure with this.Preparation technology of the present invention is simple, compared with dry etching Sapphire Substrate, prevents the pollution and damage that cause sapphire substrate surface, particularly mesa edge position; Compared with wet etching Sapphire Substrate, overcome the problem that aliasing that isotropic etching causes even makes live width distortion.
Meanwhile, adopt sapphire surface micro-nano structure prepared by this process parameters range, more regular, there is the effects such as the anti-reflection and hydrophilic automatically cleaning of obvious antireflection.
Accompanying drawing explanation
Fig. 1 is the technological process schematic diagram that the present invention prepares sapphire surface antireflection micro-nano structure;
Fig. 2 is the process evolution typical case SEM figure that sapphire surface aluminium film prepares antireflection micro-nano structure in succession after twice anodic oxidation and double annealing process: the orderly cavernous structure in surface prepared after the anodic oxidation of (a) aluminium film, porous surface aluminum oxide polycrystal film prepared after (b) low-temperature heat treatment, the orderly poroid micro-nano structure of sapphire surface prepared after (c) high-temperature heat treatment;
Fig. 3 is the Raman spectrum comparison diagram of prepared sapphire surface micro-nano structure and sapphire crystal;
Fig. 4 is that the sapphire surface micro-nano structure AFM with different hole depth schemes: (a) be the macroscopic void degree of depth (650nm) comparatively, and (b) be the small holes degree of depth (86nm) comparatively;
Fig. 5 is the infrared transmission spectra figure of the sapphire surface micro-nano structure with different hole occupy-place ratio;
Fig. 6 is the visible transmission spectra figure of the sapphire surface micro-nano structure with different hole depth;
Fig. 7 is the wetting angle test pattern of the sapphire surface micro-nano structure with different hole depth: (a) sapphire, and (b) be the macroscopic void degree of depth (650nm) comparatively, and (c) be the small holes degree of depth (86nm) comparatively.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described.
In order to embodiments of the invention will be solved technical problem, technical scheme and advantage clearly, be described in detail below in conjunction with the accompanying drawings and the specific embodiments.
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment 1
Steps A: prepare layer of metal aluminium film at sapphire surface: adopt the method for magnetron sputtering to sputter at sapphire surface the aluminium film that a layer thickness is about 1 μm;
Step B: the aluminium film anodic oxygen of sapphire surface is changed into surface and has uniform sequential cavernous aluminum oxide film, anodic oxidation is carried out in the oxalic acid electrolytic solution of 0.3mol/L, and oxidizing temperature is 0 DEG C, and oxidation voltage is 40V; First time anodic oxidation, chemistry is wherein generally divided into melt film, second time anodic oxidation and reaming procedure.Anodizing time is 30min for the first time; Chemistry melts film and carry out 10min in the phosphoric acid of the 6wt.% of 60 DEG C and the chromic acid mixture of 1.8wt.%; Second time oxidization time is equally also 30min; Reaming in the phosphoric acid solution of 5wt.%, pore-enlargement is 40min.
Step C: low-temperature heat treatment: the sapphire surface obtained by step B has the sample of even cavernous structure, put into alumina crucible, carry out 450 DEG C of anneal of 24 hours in the lehr, thus remaining aluminium film after the reaction of step B Anodic Oxidation is converted into aluminum oxide polycrystal film.
Step D: high-temperature heat treatment: on the basis of completing steps C, carry out 1000 DEG C of thermal treatments of 3 hours, to realize solid state reaction iso-epitaxy, make it be converted into the aluminium oxide single crystal film of cavernous structure completely, thus complete the preparation of sapphire surface antireflection micro-nano structure.
Embodiment 2 and example 1 unlike, changing step B is straight reaming after 1 anodic oxidation, and other step remains unchanged.
Embodiment 3 and example 1 unlike, the anodizing temperature only changing step B is 15 DEG C, and other step remains unchanged.
Embodiment 4 and example 1 unlike, the anodic oxidation voltage only changing step B is 30V, and other step remains unchanged.
Embodiment 5 and example 1 unlike, the anodic oxidation voltage only changing step B is 60V, and other step remains unchanged.
Embodiment 6 and example 1 unlike, the anodizing time only changing step B is 5.0min, and other step remains unchanged.
Embodiment 7 and example 1 unlike, the pore-enlargement only changing step B is 30min, and other step remains unchanged.
Embodiment 8 and example 1 unlike, the pore-enlargement only changing step B is 50min, and other step remains unchanged.
Embodiment 9 and example 8 unlike, at sapphire backsides, then repeat the step of an embodiment 8.
Embodiment 10 and example 1 unlike, the thermal treatment temp only changing step C is 550 DEG C, and other step remains unchanged.
Embodiment 11 and example 8 unlike, the thermal treatment temp only changing step D is 1000 DEG C, and other step remains unchanged.
Embodiment 12 and example 8 unlike, the thermal treatment temp only changing step D is 1100 DEG C, and other step remains unchanged.
Embodiment 13 and example 8 unlike, the heat treatment time only changing step D is 6h, and other step remains unchanged.
Embodiment 14
Steps A: prepare layer of metal aluminium film at sapphire surface: adopt the method for magnetron sputtering to sputter at sapphire surface the aluminium film that a layer thickness is about 100nm;
Step B: the aluminium film anodic oxygen of sapphire surface is changed into the aluminum oxide film that surface has uniform sequential vesicular structure, its Anodic Oxidation carries out in the oxalic acid electrolytic solution of 0.3mol/L, oxidizing temperature is 0 DEG C, oxidation voltage is 40V, and specifically can be divided into first time anodic oxidation, chemistry and melt film, second time anodic oxidation and reaming procedure.Anodizing time is 8min for the first time; Chemistry melts film and refers to carry out 5min in the phosphoric acid of 6wt.% of 60 DEG C and the chromic acid mixture of 1.8wt.%; Second time oxidization time is equally also 8min; Reaming in the phosphoric acid solution of 5wt.%, pore-enlargement is 50min.
Step C: low-temperature heat treatment: the sapphire surface obtained by step B has the sample of even cavernous structure, put into alumina crucible, carry out 450 DEG C of anneal of 5 hours in the lehr, thus remaining aluminium film after the reaction of step B Anodic Oxidation is converted into polycrystal alumina film.
Step D: high-temperature heat treatment: the 1000 DEG C of thermal treatments carrying out 1 hour on the basis of completing steps C, realize solid state reaction iso-epitaxy, make it be converted into the aluminium oxide single crystal film of cavernous structure completely, complete the preparation of sapphire surface antireflection micro-nano structure.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. a preparation method for sapphire surface antireflection micro-nano structure, is characterized in that, comprising:
(1) splash-proofing sputtering metal aluminium film on sapphire substrate;
(2) described sapphire surface metallic aluminium film is formed the ordered porous aluminum oxide polycrystal film of surface uniform through twice anodic oxidation;
(3) by aluminum oxide polycrystal film ordered porous for described surface uniform through double annealing thermal treatment, thus form sapphire surface poroid antireflection micro-nano structure.
2. preparation method according to claim 1, is characterized in that: the described aluminium film thickness of step (1) is 50 ~ 1000 nm.
3. according to preparation method according to claim 1 or claim 2, it is characterized in that: step (2) is described through twice anodic oxidation, comprising:
First described aluminium film is carried out twice anodic oxidation in the oxalic acid of 0.2 ~ 0.5 mol/L, anodizing temperature is-5 ~ 15 DEG C, anodic oxidation voltage is 30 ~ 60 V, anodizing time is 5 ~ 40 min, in the phosphoric acid of 3 ~ 8 wt.%, carry out reaming more subsequently, pore-enlargement is 20 ~ 90 min.
4. according to preparation method according to claim 1 or claim 2, it is characterized in that: the double annealing thermal treatment described in step (3), comprising:
First carry out low-temperature heat treatment, namely 400 ~ 600 DEG C time be incubated 2 ~ 24 h, by fully oxidized for aluminium film remaining for anodic oxidation reactions be aluminum oxide polycrystal film; Then, carry out high-temperature heat treatment, namely 800 ~ 1000 DEG C time, be incubated 1 ~ 6 h, thus the poroid aluminum oxide polycrystal film in surface that will obtain, be fully converted into aluminium oxide single crystal film.
5. preparation method according to claim 3, is characterized in that: the double annealing thermal treatment described in step (3), comprising:
First carry out low-temperature heat treatment, namely 400 ~ 600 DEG C time be incubated 2 ~ 24 h, by fully oxidized for aluminium film remaining for anodic oxidation reactions be aluminum oxide polycrystal film; Then, carry out high-temperature heat treatment, namely 800 ~ 1000 DEG C time, be incubated 1 ~ 6 h, thus the poroid aluminum oxide polycrystal film in surface that will obtain, be fully converted into aluminium oxide single crystal film.
6. a sapphire surface antireflection micro-nano structure, is characterized in that: adopt the method described in claim 1 ~ 5 to prepare.
7. sapphire surface antireflection micro-nano structure according to claim 6, is characterized in that, adjacent two distance between borehole of described even cavernous structure are 80 ~ 160 nm.
8. according to claim 6 or sapphire surface antireflection micro-nano structure according to claim 7, it is characterized in that, the pore size of described even cavernous structure is 30 ~ 100 nm.
9. according to claim 6 or sapphire surface antireflection micro-nano structure according to claim 7, it is characterized in that, the hole depth of described cavernous structure is 50 ~ 1000 nm.
10. sapphire surface antireflection micro-nano structure according to claim 8, is characterized in that, the hole depth of described cavernous structure is 50 ~ 1000 nm.
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