CN103337575A - Efficient and low-cost preparing method for large-area graphical sapphire substrate - Google Patents
Efficient and low-cost preparing method for large-area graphical sapphire substrate Download PDFInfo
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- CN103337575A CN103337575A CN2013102723180A CN201310272318A CN103337575A CN 103337575 A CN103337575 A CN 103337575A CN 2013102723180 A CN2013102723180 A CN 2013102723180A CN 201310272318 A CN201310272318 A CN 201310272318A CN 103337575 A CN103337575 A CN 103337575A
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Abstract
The invention provides an efficient and low-cost preparing method for a large-area graphical sapphire substrate, which includes the following steps: step A, coating PDMS (polydimethylsiloxane) diluted by methylbenzene in a grating structured graph hard template in a spinning manner; step B, coating a PDMS prepolymer with the PDMS diluted by methylbenzene; step C, demoulding, and obtaining a PDMS soft embossing template; step D, performing metallic aluminium film magnetron sputtering to one surface of a sapphire substrate; step E, demoulding, and obtaining an ultraviolet curing glue graph; step F, taking the graphic ultraviolet curing glue on the metallic aluminium film as a mask; step G, performing low-temperature thermal treatment, and completely oxidizing the graphic metallic aluminium film to form a graphic polycrystal Al2O3 film; step H, performing high-temperature thermal treatment to the obtained graphic polycrystal Al2O3 film, and obtaining the graphical sapphire substrate. The graphical sapphire substrate for epitaxial growth of nitride, obtained through adopting the method, has the advantages that the process is simple and feasible, the production efficiency is high, the cost is low and the area is big.
Description
Technical field
The present invention relates to a kind of preparation method of graphic sapphire substrate, especially relate to the preparation method of a kind of high efficiency, low cost, large-area graphic sapphire substrate for nitride place epitaxial growth.
Background technology
Highlighted high power nitride light-emitting diode (LED) is paid attention to deeply in recent years, and it is widely used in traffic lights, LCD backlight, solid-state illumination, full color display etc.These commercial products require LED having good performance aspect brightness and the luminous efficiency.Sapphire has chemistry and advantage such as physical property is stable, light transmission is good, cost is suitable, so extensively is used to the nitride epitaxial substrate.But because the Sapphire Substrate of nitride epitaxial film and bottom exists lattice constant mismatch and the coefficient of thermal expansion mismatch of greatest differences, so utilize the nitride epitaxial film of beam epitaxy (MBE) the homepitaxy growth of hydride gas-phase epitaxy (HVPE), metal organic chemical vapor deposition (MOCVD), branch, can produce high line dislocation density at the nitride epitaxial film, this high line dislocation density will influence optics and the electrology characteristic of epitaxial film, cause the reliability of device and internal quantum efficiency to reduce.Adopt the Sapphire Substrate that the sapphire graphical substrate technology can be alleviated owing to nitride epitaxial film and bottom to have the lattice constant mismatch of greatest differences and the stress that coefficient of thermal expansion mismatch causes, make stress obtain effective relaxation, can effectively reduce in the nitride epitaxial film line dislocation density.The graphic sapphire substrate is different from common plain film Sapphire Substrate.It is the fluctuating figure of fabrication cycle on the smooth sapphire substrate of extension level.The graphic sapphire substrate is mainly used on the extension chip of semiconductor indigo plant, green, white light LEDs, can increase substantially led chip brightness, increases substantially power and the radiating efficiency of chip, is just becoming the main flow substrate of semiconductor lighting industry.Sapphire Substrate is carried out reasonably graphical preliminary treatment, realize its laterally overgrown, and then reduce it and expand to defective in the Multiple Quantum Well grown layer, thereby improve the luminous efficiency of LED device, improve the bright dipping mode simultaneously, be the inexorable trend of the development of high-brightness LED field and research, important theory and real value are arranged.
At present, generally adopt the method for etching sapphire substrate to prepare the sapphire graphical substrate, etching can be divided into wet etching and dry etching.
Wet etching is to prepare one deck mask layer at sapphire substrate earlier, etches away the part mask layer as required, and the wafer that the chemical reagent that recycling is suitable will not covered by mask layer earlier partly decomposes, and forms the compound of solubility then to reach the purpose of removal.Therefore this lithographic technique mainly is the chemical reaction by etching liquid and wafer material, can reach suitable etch rate and good etching selection ratio by the choosing of chemical reagent, proportioning and temperature controlling.The advantage of wet etching is that program is single, and equipment is simple, and cost is low, the production efficiency height, and have good etching selection ratio.But wet etching generally is isotropic, and when transferring to litho pattern on the wafer, etching is not only vertically carried out, also can be towards laterally carrying out.Can make aliasing like this, even make the live width distortion.
That what adopt is dry etching technology is more for the etching of sapphire graphical substrate in the world, but because high rigidity and the anti-strong acid characteristic of sapphire substrate cause it to be faced with cutting often in element manufacturing, difficulties such as polishing and device isolation, therefore progressively adopt ion beam etching (IBE), laser assistant chemical corrosion (LAE), ion injects chemical corrosion and inductively coupled plasma technology such as (ICP) replaces Machining Technology, wherein the ICP dry etching technology has with it and can control plasma density and ion bombardment energy respectively, advantage such as Automatic Network Matching when being suitable for glow discharge and a large amount of the employing.But dry etching is easily to the sapphire substrate surface, and particularly certain pollution and damage are caused in the mesa edge position, are unfavorable for the further raising of epitaxial loayer crystal mass.
Because the intrinsic optical characteristics of projection optical system, how to utilize existing technology and equipment to carry out the selection of resolution and these two contradiction parameters of depth of focus, become the subject matter that optical lithography techniques faces, and cause that problems such as new light sources, photoresist, mask, technology, lens material and design need to solve.More than ten years in past, effort aspect shortening exposure wavelength, increase optical system numerical aperture, adding phase shifting mask off-axis illumination, proximity correction etc. and strengthen the photoetching resolution technology, is all to obtain good achievement aspect raising resolution and the increasing depth of focus two.But because the contradiction between resolving power and the depth of focus makes photoetching technique have the limit.Photoetching based on particle focusing, no matter be ion beam lithography or electron beam lithography, although have sufficiently high resolution, and by the travelling workpiece platform, can obtain relatively large exposure visual field, but film speed has limited application in manufacturing process low-costly and in high volume slowly.
Summary of the invention
In order to solve above technical problem, the invention provides the preparation method of a kind of high efficiency of avoiding aliasing and not damaging sapphire substrate, low cost, large-area graphs Sapphire Substrate, comprise following several steps:
Steps A: the PDMS of spin coating toluene (toluene) dilution on optical grating construction figure hard template;
Step B: apply the PDMS prepolymer at the PDMS of dilution with toluene, the PDMS plate of 80 μ m to 120 μ m is pressed in PDMS prepolymer surface, then be heating and curing;
Step C: the demoulding obtains the soft impression block of PDMS;
Step D: magnetron sputtering aluminium film on a face of sapphire substrate, then apply ultra-violet curing glue at aluminium film, oven dry adopts the soft impression block of PDMS that ultra-violet curing glue is carried out the soft impression of ultraviolet nanometer then;
Step e: the demoulding obtains the ultra-violet curing glue pattern;
Step F: be mask with graphical ultra-violet curing glue on the aluminium film, adopt the reactive ion etching aluminium film and remove photoresist, obtain the graphical aluminium film of aluminium film optical grating construction at sapphire substrate;
Step G: carry out Low Temperature Heat Treatment, make graphical aluminium film fully be oxidized into graphical polymorph A l
2O
3Film;
Step H: the graphical polymorph A l that will obtain
2O
3Film carries out high-temperature heat treatment, makes graphical polymorph A l
2O
3Film is converted into graphical monocrystalline Al fully
2O
3Film namely obtains the graphic sapphire substrate.
Wherein, PDMS (polydimethylsiloxane) is the english abbreviation of dimethyl silicone polymer.100um
The present invention adopts above technical scheme, and its advantage is, adopts the soft stamping technique of ultraviolet nanometer,
Compare with hot press printing technology, the ultraviolet nanometer stamping technique has a lot of outstanding features and advantage.For example: at room temperature can impress, not need heating-cooling procedure, thereby reduce the thermal mismatching between template and the substrate, the size drift of generation; The production technology period ratio is shorter, and ultra-violet curing time length depends primarily on photoresist to the sensitivity of ultraviolet light, has saved heating-cooling time in hot padding; The coefficient of viscosity of ultra-violet curing photoresist is very little, so it is very low to impress required pressure, and the cull layer behind the impression is very thin; Because the ultraviolet nanometer pressuring template is transparent, realize the aligning (overlay) of interlayer easily.Because the ultraviolet nanometer stamping technique can be realized the quick copy nano-scale pattern at normal temperatures, and template is transparent can fine solution semiconductor fabrication in the alignment issues of interlayer, it is a kind of graph copying technology that has very much development prospect, be subjected to paying close attention to widely, become the focus of domestic and international correlation technique research.
Preferably, the thickness of described aluminium film is 150nm～200nm.
Preferably, the PDMS mass concentration of the dilution with toluene in the described steps A is 60%wt.
Preferably, the PDMS prepolymer is the PDMS prepolymer among the described step B: curing agent=1:10 preparation.
Preferably, the impression block among the described step D adopts the soft impression block of PDMS.
Preferably, the stamping technique among the described step D adopts the soft stamping technique of ultraviolet nanometer.
Wherein, the soft stamping technique of ultraviolet nanometer, be to adopt the template that has nano graph to prepare the soft impression block of PDMS, the PDMS soft template impresses at ultra-violet curing glue, nano graph on the PDMS soft template is transferred on the ultra-violet curing glue of substrate surface, adopt etching technics again, the figure on the ultra-violet curing glue is transferred to on-chip technical process.PDMS is a kind of good elastomer, fits well with substrate surface, can carry out contact printing at plane surface not; Can easily peel off from substrate behind the impression, not destroy the figure that copies; The PDMS chemical property is stable, and has very low surface free energy (21.6 * 10-3Jm
-2), be difficult for being stained with sticking or chemical reaction with the surface of the material that is used for the making figure; PDMS material homogeneous, isotropism, light transmission are good, and ultraviolet light (325nm) transmitance of the soft impression block of PDMS that lmm is thick can reach～and 90%, therefore can see through the PDMS template, the photosensitive polymer performed polymer is carried out crosslinking curing.PDMS is durable in use, and the PDMS soft template can under normal circumstances be reused 50-100 time, satisfies industrial needs.
The advantage of the soft impression of ultraviolet nanometer: the damage of having avoided direct hard impression that template and substrate are caused; Avoided the rigidity impression block can't be accurately and the contacted shortcoming of substrate; And the PDMS material is that a kind of light transmission is good, thermoplastic.In sum, the soft stamping technique of ultraviolet nanometer has production efficiency height, low, the simple technological process and other advantages of cost, is the strong instrument of device of making nanostructure, is one of the most promising photoetching technique of future generation.
Preferably, described step D medium ultraviolet is solidified glue employing AMONIL-MMS4 ultra-violet curing glue.
Preferably, the thickness of described step D medium ultraviolet solidified glue film is 150nm～250nm.
Preferably, the temperature of Low Temperature Heat Treatment is 400 ℃～600 ℃ among the described step G.
Preferably, the temperature of high-temperature heat treatment is 950 ℃～1250 ℃ among the described step H.
The inventive method compares with wet etching sapphire graphical substrate, overcome the aliasing that isotropic etching causes even the problem that makes the live width distortion; Compare with dry etching sapphire graphical substrate, overcome the Sapphire Substrate surface, the particularly pollution and the damage that cause of mesa edge position; Compare with ion beam lithography or electron beam lithography, the ultraviolet nanometer impression has production efficiency height, low, the simple technological process and other advantages of cost, is the strong instrument of device of making nanostructure.
The invention has the beneficial effects as follows: the preparation method of graphic sapphire substrate of the present invention, be different from present both at home and abroad common adopt Sapphire Substrate is directly carried out dry etching or wet etching, but adopt the soft impression of ultraviolet nanometer and reactive ion etching earlier, form graphical aluminium film at sapphire substrate, make the aluminium film carry out solid phase reaction by heat treated mode of two steps then, the final aluminium oxide single crystal film that generates, thereby can obtain the optimum graphic sapphire substrate that is used for nitride epitaxial growth, simple for process, the production efficiency height, cost is low, and area is big.
Description of drawings
Fig. 1 is the technical process schematic diagram that the present invention prepares the graphic sapphire substrate.
Fig. 2 is the SEM figure of raster graphic structure PDMS soft template among the present invention.
Fig. 3 is the SEM figure of raster graphic structure AMONIL-MMS4 ultra-violet curing glue among the present invention.
Fig. 4 is the SEM figure of the graphic sapphire substrate that obtains through 450 ℃ of 24 hours, 1000 ℃ 24 hours solid phase reactions of the graphical aluminium film of optical grating construction.
Fig. 5 is the SEM figure of the graphic sapphire substrate that obtains through 500 ℃ of 24 hours, 1200 ℃ 24 hours solid phase reactions of the graphical aluminium film of optical grating construction.
Fig. 6 is the XRD-Φ scanning result of graphic sapphire substrate (11-23).
Fig. 7 is the XRD-ω/2 θ scanning results of graphic sapphire substrate (0006).
Fig. 8 is the XRD-ω/2 θ scanning results of not patterned sapphire substrate (0006).
Embodiment
Below in conjunction with accompanying drawing, more excellent embodiment of the present invention is described in further detail:
As shown in Figure 1, the preparation process of graphic sapphire substrate of the present invention specifically comprises the following steps:
Step S1: adopt dilution with toluene PDMS, mass concentration is 60%wt, stir, pour injector for medical purpose into, the PDMS that diluted is injected the hard template of optical grating construction figure, and cover whole raster graphic stay in place form surface, and then carry out whirl coating at sol evenning machine, the main effect of whirl coating is that the PDMS that will dilute carries out attenuate and homogenizing.
Step S2: with the PDMS prepolymer: curing agent=1:10 preparation PDMS prepolymer, stir, be coated on the PDMS that mass concentration is 60%wt, then thick elasticity PDMS plate is pressed on the PDMS prepolymer, template is placed on the hot plate, hot plate temperature arranges 90 ℃, solidifies 2-3h, naturally cooling.
Step S3: with tweezers the template of optical grating construction figure is peeled off, thereby obtain ultraviolet nanometer impression PDMS soft template.As shown in Figure 2, be the SEM figure of the raster graphic structure PDMS soft template that obtains.
Step S4: adopting magnetron sputtering technique magnetron sputtering thickness on a face of sapphire substrate is the aluminium film of 150nm～200nm, then applying thickness at aluminium film is 200nm ultra-violet curing glued membrane, oven dry, utilize the PDMS soft template to carry out the ultraviolet nanometer impression then, ultra-violet curing glue can be selected AMONIL-MMS4 ultra-violet curing glue for use.
Step S5: with tweezers the PDMS soft template is peeled off, thereby obtain graphical ultra-violet curing glue.
Step S6: be mask with graphical ultra-violet curing glue on the aluminium film, adopt the reactive ion etching aluminium film and remove photoresist, obtain the graphical aluminium film of aluminium film optical grating construction at sapphire substrate.
Step S7: under 400 ℃～600 ℃, carry out Low Temperature Heat Treatment, make graphical aluminium film fully be oxidized into graphical polymorph A l
2O
3Film.
Step S8: then place and carry out high-temperature heat treatment realization solid phase reaction homoepitaxy under 950 ℃～1250 ℃, make graphical polymorph A l
2O
3Film is converted into graphical monocrystalline Al fully
2O
3Film obtains being applicable to the graphic sapphire substrate of nitride epitaxial growth.
Embodiment 1
The method of carrying out is for the preparation of the graphic sapphire substrate of nitride epitaxial growth in the following order:
(1), the template evaporation FDTS release agent of optical grating construction figure at first, then adopt toluene (toluene) dilution PDMS, concentration is 60%wt, stirs, and pours injector for medical purpose into, the PDMS that will dilute then injects the template of optical grating construction figure, and cover whole raster graphic stay in place form surface, then carry out whirl coating at sol evenning machine: first low speed 900 rpm, the even glue 6s of rotation, again during high speed 3000rpm, the even glue 20s of rotation.
(2), with the PDMS prepolymer: curing agent=1:10 preparation PDMS prepolymer, stir, be coated on the PDMS that mass fraction is 60%wt, then the PDMS plate with 80 μ m to 120 μ m is pressed on the PDMS prepolymer, template is placed on the hot plate, and hot plate temperature is set to 90 ℃, solidifies 2-3 h, naturally cooling, wherein hot plate is a kind of equipment of drying glue.
(3), with tweezers the template of optical grating construction figure is peeled off, thereby obtain ultraviolet nanometer impression PDMS soft template, as shown in Figure 2, be the SEM figure of the graphical PDMS soft template of optical grating construction that obtains, raster size is 540nm, and grating space is 240nm.
(4), splash-proofing sputtering metal aluminium film: adopt magnetically controlled DC sputtering technology about 150nm aluminium film of magnetron sputtering on face of sapphire substrate.
(5), ultraviolet nanometer impression: in step (4) sputter spin coating AMONIL-MMS4 ultra-violet curing glue on the Sapphire Substrate aluminium film of aluminium film, thickness is 200nm, whirl coating rotating speed 3500 r/min, 110 ℃ of oven dry 2min; PDMS soft template evaporation FDTS release agent, then in EVG620 ultraviolet nanometer Embosser, utilize the PDMS soft template that AMONIL-MMS4 ultra-violet curing glue is carried out the ultraviolet nanometer impression, under 500mbar pressure, AMONIL-MMS4 photoresist ultra-violet curing time 120s.
(6), with tweezers the PDMS soft template is peeled off, thus obtain graphical ultra-violet curing glue.As shown in Figure 3, be the SEM figure of the graphical ultra-violet curing glue of optical grating construction that obtains.
(7), reactive ion etching aluminium film and removing photoresist: be mask with graphical photoresist on the splash-proofing sputtering metal aluminium film of step (6), adopt the reactive ion etching aluminium film, RF power is 600W, and Dc bias-200V, cavity pressure are 7mT, BCl
3Flow be 100sccm, Cl
2Flow be 25sccm, etch period is 90s.The employing reactive ion etching is removed photoresist, and RF power is 50W, and cavity pressure is 100mT, O
2Flow be 200sccm, etch period is 120s, and photoresist is removed fully, obtains the graphical aluminium film of optical grating construction.
(8), Low Temperature Heat Treatment: the sample with the graphical aluminium film of optical grating construction of step (7) is put into alumina crucible, in annealing furnace, carry out 450 ℃ of processing in 24 hours and make aluminium film fully be oxidized into polymorph A l
2O
3Film.
(9), high-temperature heat treatment: carry out 1000 ℃ of heat treatments in 24 hours on the basis of completing steps (8), realize solid phase reaction homoepitaxy, make graphical polymorph A l
2O
3Film is converted into graphical monocrystalline Al fully
2O
3Film is finished the preparation for the graphic sapphire substrate of nitride epitaxial growth.As shown in Figure 4, be the SEM figure of the soft coining pattern aluminium film of ultraviolet nanometer through the graphic sapphire substrate of 450 ℃ of 24 hours and the preparations of 1000 ℃ of 24 hours solid phase reactions, as can be seen from the figure figure complete display, raster width is 240nm, grating space is 540nm.
Embodiment 2
The method of carrying out is for the preparation of the graphic sapphire substrate of nitride epitaxial growth in the following order:
(1), the template evaporation FDTS release agent of optical grating construction figure at first, then adopt dilution with toluene PDMS, mass concentration is 60%wt, stirs, and pours injector for medical purpose into, the PDMS that will dilute then injects the template of optical grating construction figure, and cover whole raster graphic stay in place form surface, and then carry out whirl coating at sol evenning machine: under low speed 900 rpm, the even glue 6s of rotation, under the high speed 3000rpm, the even glue 20s of rotation.
(2), with the PDMS prepolymer: curing agent=1:10 prepares the PDMS prepolymer, stirs, and is coated on the PDMS of 60%wt, then thick elasticity PDMS plate is pressed on the PDMS prepolymer, template is placed on the hot plate, hot plate temperature arranges 90 ℃, solidify 2-3 h, naturally cooling.
(3), with tweezers the template of optical grating construction figure is peeled off, thus obtain ultraviolet nanometer impression PDMS soft template, raster size 540nm, grating space 240nm.As shown in Figure 2, be the SEM figure of the graphical PDMS soft template of optical grating construction that obtains.
(4), splash-proofing sputtering metal aluminium film: adopt magnetically controlled DC sputtering technology about 150nm aluminium film of magnetron sputtering on face of sapphire substrate.
(5), ultraviolet nanometer impression: in step (4) sputter spin coating AMONIL-MMS4 ultra-violet curing glue on the Sapphire Substrate aluminium film of aluminium film, thickness is about 200nm, whirl coating rotating speed 3500 r/min, 110 ℃ of oven dry 2min; PDMS soft template evaporation FDTS release agent, then in EVG620 ultraviolet nanometer Embosser, utilize the PDMS soft template that AMONIL-MMS4 ultra-violet curing glue is carried out the ultraviolet nanometer impression, under 500mbar pressure, AMONIL-MMS4 photoresist ultra-violet curing time 120s.
(6), with tweezers the PDMS soft template is peeled off, thereby obtain graphical ultra-violet curing glue, as shown in Figure 3, be the SEM figure of the graphical ultra-violet curing glue of optical grating construction that obtains.
(7), reactive ion etching aluminium film and removing photoresist: be mask with graphical photoresist on the splash-proofing sputtering metal aluminium film of step (6), adopt the reactive ion etching aluminium film, RF power is 600W, and Dc bias-200V, cavity pressure are 7mT, BCl
3Flow be 100sccm, Cl
2Flow be 25sccm, etch period is 90s.The employing reactive ion etching is removed photoresist, and RF power is 50W, and cavity pressure is 100mT, O
2Flow be 200sccm, etch period is 120s, and photoresist is removed fully, obtains the graphical aluminium film of optical grating construction.
(8), Low Temperature Heat Treatment: the sample with graphical aluminium film of step (7) is put into alumina crucible, in annealing furnace, carry out 500 ℃ of processing in 24 hours and make aluminium film fully be oxidized into polymorph A l
2O
3Film.
(9), high-temperature heat treatment: carry out 1200 ℃ of heat treatments in 24 hours on the basis of completing steps (8), realize solid phase reaction homoepitaxy, make graphical polymorph A l
2O
3Film is converted into graphical monocrystalline Al fully
2O
3Film is finished the preparation for the graphic sapphire substrate of nitride epitaxial growth.As shown in Figure 5, be for the SEM figure of the soft coining pattern aluminium film of ultraviolet nanometer through the graphic sapphire substrate of 450 ℃ of 24 hours and the preparations of 1200 ℃ of 24 hours solid phase reactions, can see that from Fig. 5 figure is clear.
Embodiment 3
The crystal structure test
Use the high-resolution X-ray diffractometer that the graphic sapphire substrate of preparation is carried out the crystal structure test.Fig. 6 is the scanning result of graphic sapphire substrate (11-23), and Fig. 7 is the XRD-ω/2 θ scanning results of graphic sapphire substrate (0006), and the result shows FWHM=0.0101 ° of the diffraction maximum halfwidth of graphic sapphire substrate (0006).Fig. 8 is the XRD-ω/2 θ scanning results of not patterned sapphire substrate (0006), and the result shows FWHM=0.0133 ° of the diffraction maximum halfwidth of graphic sapphire substrate (0006) not.The XRD-Φ scanning result of the graphic sapphire substrate (11-23) of Fig. 6 (11-23) with crystal face included angle=61.2 of (0006) °, makes sample do 0～360 ° of scanning around surface normal n.6 equally spaced diffraction maximums have appearred in Fig. 6, differ 60 ° between the adjacent diffraction maximum, show that the graphic sapphire substrate is hexagonal crystal system, and it is consistent with substrate orientation, and the graphic sapphire substrate more not graphic sapphire substrate crystalline quality improve, thereby realized graphic sapphire substrate for the preparation of nitride epitaxial growth.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention does, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. the preparation method of a high efficiency, low cost, large-area graphs Sapphire Substrate is characterized in that, comprises following several steps:
Steps A: the PDMS of spin coating dilution with toluene on optical grating construction figure hard template;
Step B: apply the PDMS prepolymer at the PDMS of dilution with toluene, the PDMS plate of 80 μ m to 120 μ m is pressed in PDMS prepolymer surface, then be heating and curing;
Step C: the demoulding obtains the soft impression block of PDMS;
Step D: magnetron sputtering aluminium film on a face of sapphire substrate, then apply ultra-violet curing glue at aluminium film, oven dry adopts the soft impression block of PDMS that ultra-violet curing glue is carried out the soft impression of ultraviolet nanometer then;
Step e: the demoulding obtains the ultra-violet curing glue pattern;
Step F: be mask with graphical ultra-violet curing glue on the aluminium film, adopt the reactive ion etching aluminium film and remove photoresist, obtain the graphical aluminium film of aluminium film optical grating construction at sapphire substrate;
Step G: carry out Low Temperature Heat Treatment, make graphical aluminium film fully be oxidized into graphical polymorph A l
2O
3Film;
Step H: the graphical polymorph A l that will obtain
2O
3Film carries out high-temperature heat treatment, makes graphical polymorph A l
2O
3Film is converted into graphical monocrystalline Al fully
2O
3Film namely obtains the graphic sapphire substrate.
2.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the thickness of described aluminium film is 150nm～200nm.
3.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the PDMS mass concentration of the dilution with toluene in the described steps A is 60%wt.
4.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the PDMS prepolymer is the PDMS prepolymer among the described step B: curing agent=1:10 preparation.
5.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the impression block among the described step D is selected the soft impression block of PDMS for use.
6.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the stamping technique among the described step D is selected the soft stamping technique of ultraviolet nanometer for use.
7.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, described step D medium ultraviolet is solidified glue and adopted AMONIL-MMS4 ultra-violet curing glue.
8.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the thickness of described step D medium ultraviolet solidified glue film is 150nm～250nm.
9.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the temperature of Low Temperature Heat Treatment is 400 ℃～600 ℃ among the described step G.
10.
.The preparation method of high efficiency as claimed in claim 1, low cost, large-area graphs Sapphire Substrate is characterized in that, the temperature of high-temperature heat treatment is 950 ℃～1250 ℃ among the described step H.
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| CN104846336A (en) * | 2015-03-20 | 2015-08-19 | 哈尔滨工业大学深圳研究生院 | Anti-reflective micro-nano structure of sapphire surface and preparation method thereof |
| CN105926014A (en) * | 2016-05-05 | 2016-09-07 | 中国科学院上海高等研究院 | Preparation method of large-area highly-ordered porous oxide films based on nano soft embossing |
| CN107203014A (en) * | 2017-06-01 | 2017-09-26 | 武汉华星光电技术有限公司 | A kind of preparation method, antireflection substrate and the electronic product of moth eye micro-structural |
| CN107817547A (en) * | 2017-12-08 | 2018-03-20 | 深圳市华星光电技术有限公司 | The manufacture method of grating |
| CN108801512A (en) * | 2018-05-03 | 2018-11-13 | 五邑大学 | A kind of nano-hemisphere pressure sensor and preparation method thereof |
| CN110095441A (en) * | 2019-04-19 | 2019-08-06 | 中国科学院苏州生物医学工程技术研究所 | A kind of fluorescence nano scale member and its preparation and application |
| CN113451519A (en) * | 2020-07-13 | 2021-09-28 | 河南大学 | Quantum dot light-emitting diode device and preparation method thereof |
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| CN104846336A (en) * | 2015-03-20 | 2015-08-19 | 哈尔滨工业大学深圳研究生院 | Anti-reflective micro-nano structure of sapphire surface and preparation method thereof |
| CN104846336B (en) * | 2015-03-20 | 2017-05-24 | 哈尔滨工业大学深圳研究生院 | Anti-reflective micro-nano structure of sapphire surface and preparation method thereof |
| CN105926014A (en) * | 2016-05-05 | 2016-09-07 | 中国科学院上海高等研究院 | Preparation method of large-area highly-ordered porous oxide films based on nano soft embossing |
| CN107203014A (en) * | 2017-06-01 | 2017-09-26 | 武汉华星光电技术有限公司 | A kind of preparation method, antireflection substrate and the electronic product of moth eye micro-structural |
| WO2018218720A1 (en) * | 2017-06-01 | 2018-12-06 | 武汉华星光电技术有限公司 | Preparation method for moth eye microstructure, anti-reflection substrate and electronic product |
| US10634822B2 (en) | 2017-06-01 | 2020-04-28 | Wuhan China Star Optoelectronics Technology Co., Ltd. | Method of manufacturing a moth eye mircostructure, an antireflective substrate and an electronic product |
| CN107817547A (en) * | 2017-12-08 | 2018-03-20 | 深圳市华星光电技术有限公司 | The manufacture method of grating |
| CN108801512A (en) * | 2018-05-03 | 2018-11-13 | 五邑大学 | A kind of nano-hemisphere pressure sensor and preparation method thereof |
| CN110095441A (en) * | 2019-04-19 | 2019-08-06 | 中国科学院苏州生物医学工程技术研究所 | A kind of fluorescence nano scale member and its preparation and application |
| CN110095441B (en) * | 2019-04-19 | 2021-12-10 | 中国科学院苏州生物医学工程技术研究所 | Fluorescent nanometer scale component and preparation and application thereof |
| CN113451519A (en) * | 2020-07-13 | 2021-09-28 | 河南大学 | Quantum dot light-emitting diode device and preparation method thereof |
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