CN103117339A - Patterned sapphire substrate production method based on composite soft template nanometer stamping technique - Google Patents
Patterned sapphire substrate production method based on composite soft template nanometer stamping technique Download PDFInfo
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 150000001875 compounds Chemical class 0.000 claims description 22
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- 230000001070 adhesive effect Effects 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000059 patterning Methods 0.000 claims description 6
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- 238000005260 corrosion Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 4
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 4
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- YXJYBPXSEKMEEJ-UHFFFAOYSA-N phosphoric acid;sulfuric acid Chemical compound OP(O)(O)=O.OS(O)(=O)=O YXJYBPXSEKMEEJ-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention provides a patterned sapphire substrate production method based on a composite soft template nanometer stamping technique. The patterned sapphire substrate production method includes steps: (1) a silica layer is deposited on a sapphire substrate to serve as a wet etching mask; (2) an ultraviolet light polymerization glue layer is coated on the silica layer in spinning mode, and the structure is shifted to a glue layer in a composite soft template nanometer stamping method; (3) a residual layer is removed in an inductively coupled plasma (ICP) etching method to expose the silica surface, etching is continued, and the structure is shifted to the silica layer; and (4) the silica layer serves as the mask, sapphire is subjected to wet etching by aid of sulfuric acid and phosphoric acid mixed liquor, and finally the silica layer is removed by aid of hydrofluoric acid to obtain a patterned sapphire substrate. The patterned sapphire substrate production method has the advantages that the composite soft template nanometer stamping technique is adopted, and small-scale patterns can be produced with low cost and large area compared with the traditional photoetching method; and the problems that the etching mask is irregular and sapphire dry etching is high in cost are solved, and luminous efficiency of light-emitting diodes (LEDs) is improved.
Description
Technical field
The present invention relates to the preparation method of patterned substrate, relate in particular to a kind of method for preparing patterned sapphire substrate based on compound soft template nanometer embossing.
Background technology
LED has the advantages such as volume is little, efficient is high, the life-span is long, has been widely used in now field, the especially efficient LEDs such as traffic signals and outdoor demonstration and has been applied to realize prospect on semiconductor solid lighting attracted greatly people's attention.But, the application of LED device also needs further to improve its internal quantum efficiency and external quantum efficiency.
The limiting factor of LED internal quantum efficiency is mainly lattice mismatch and the thermal stress mismatch between Sapphire Substrate and extension GaN layer, this causes the GaN layer of extension to have a large amount of defective dislocations, the non-radiative compound internal quantum efficiency that not only reduces LED of fault light in place, and light has also reduced the useful life of LED in the non-radiative compound heat release of inside.And that the influencing factor of external quantum efficiency is mainly refringence between GaN layer and air is larger, causes light that a large amount of total reflections can occur when the smooth flat outgoing, only has the light of 4% left and right to emit, and has greatly limited the efficient that light extracts.
In order to address the above problem, introduced the method for patterned sapphire substrate.Utilize the method, the laterally overgrown technology in conjunction with MOCVD has reduced epitaxial loayer stress, and during growing GaN, a large amount of dislocations can terminate in the underlay pattern zone, has reduced the defect concentration of LED inside; And the existence of area of the pattern increased the effusion angle of GaN and sapphire contact-making surface light, makes originally the light that is limited in LED inside by total reflection also can go out to shoot out, thereby improved simultaneously interior quantum and external quantum efficiency.
Present stage, the preparation patterned sapphire substrate adopts conventional photoetching method mostly, a kind of method of utilizing the standby patterned sapphire substrate of optical graving is disclosed in CN102694090A, but the standby minor cycle structure of optical graving needs comparatively expensive instrument and equipment, do not meet the production requirement of low-cost large-area, other methods such as PS nanosphere, the self assembly of Ni cluster, anodic oxidation aluminium formwork, all degree of order of control structure comparatively accurately.Aspect the corrosion of Sapphire Substrate, although dry etching can be controlled shape comparatively accurately, because sapphire hardness is large, dry etching requires high to apparatus and process, and cost is also corresponding higher.And studies show that, reduce the cycle of patterning, the depth-to-width ratio that improves pattern all can be conducive to the raising of LED luminous intensity.Therefore, the patterned sapphire substrate of low-cost large-area ground preparation minor cycle, high-aspect-ratio how is to need at present a difficult problem solving.
Nano impression as a kind of manufacturing process of preparation minor cycle structure of high rate/low cost production, is the Superior selection of preparation patterned substrate.Nano impression is the working mechanism of physical contact formula, and seek template has reasonable applying degree with substrate, and Sapphire Substrate surface undulation degree is larger, if hard template just need to apply larger pressure, easily causes the damage of template or substrate.The soft template of PDMS is due to its pliability, can with substrate on glue-line form good flexible contact, but its maximum shortcoming is exactly that deformation easily occurs, and is difficult to realize the preparation of high-resolution, high-fidelity, affects productivity ratio.
Summary of the invention
The object of the present invention is to provide a kind of can be with the low cost preparation method than the patterned sapphire substrate of minor cycle, high-aspect-ratio.The compound soft template elastic bearing layer that the present invention adopts is PDMS, can be without template and substrate surface are fitted tightly, the stamping structure layer is ultra-thin highly cross-linked ultraviolet photocureable material, make template that certain mechanical strength be arranged, be highly suitable for the impression block of the larger Sapphire Substrate of waviness.
The object of the present invention is achieved like this:
Prepare the method for patterned sapphire substrate based on compound soft template nanometer embossing, comprise the steps:
(1) deposition one deck wet etching mask layer on Sapphire Substrate, thickness is at 50nm～200nm;
(2) spin coating one deck ultraviolet cured adhesive on the wet etching mask layer then with the soft template applying ultraviolet cured adhesive of patterning, and is placed in N
2Under atmosphere, exposure made adhesive curing in 10 minutes, and the design transfer of soft template to ultraviolet cured adhesive, is sloughed soft template, the glue-line that obtains solidifying;
(3) the etching glue-line exposes the wet etching mask layer, and continues the etch mask layer to exposing Sapphire Substrate;
(4) structure that step (3) is obtained is placed in the mixed solution of sulfuric acid and phosphoric acid, 250 ℃～300 ℃ lower wet etchings 15 minutes～30 minutes, take out Sapphire Substrate, remove mask layer with hydrofluoric acid, and obtain the Sapphire Substrate of patterning after cleaning respectively with acetone, ethanol and deionized water.
The pattern for preparing on Sapphire Substrate through above-mentioned steps is the array of circular apertures of square structure, and the diameter of circular hole is 0.2 ~ 2 μ m, and the cycle is 0.5 ~ 5 μ m, and the degree of depth is 0.2 ~ 2 μ m.
Wherein, the wet etching mask layer of step (1) is selected the corrosion material of energy withstand high temperatures sulfuric acid phosphoric acid mixed liquor, as silicon dioxide, silicon nitride etc., should adopt PECVD to grow to obtain the high rete of compactness when thinner thickness.
In step (2), the elastic bearing layer of soft template is PDMS, can be without template and substrate surface be fitted tightly, and its stamping structure layer is ultra-thin highly cross-linked ultraviolet photocureable material, makes template that certain mechanical strength be arranged.
The etching of step (3) adopts the method for ICP dry etching, and wherein the etching of remaining glue-line is taken O
2Gas, the etching of mask layer adopts CHF
3And CHF
4Gas.
In the mixed solution of step (4), the phosphoric acid volume ratio of sulfuric acid is at 2:1～5:1, and corrosion rate is 30～40nm/min.
The patterned substrate of utilizing microscope and SEM to observe the said method preparation, compound soft template nano-imprinting method need not complicated instrument and equipment, just can with structural integrity from template transfer to the ultraviolet light polymerization glue-line, facilitate the carrying out of next step.Silicon dioxide structure pattern and the project organization scale error of utilizing the ICP dry etching to obtain are little, and etch rate can accurately be controlled.Follow-up wet etching Sapphire Substrate speed is comparatively stable, can access the pattern of design object.
The present invention is based on compound soft template nanometer embossing, completed the transfer for the first time of pattern, under the prerequisite that keeps precision, compare photoetching method and greatly reduce process costs, following adopted inductively coupled plasma (ICP) lithographic method obtains the silicon dioxide structure pattern of rule, recycling sulfuric acid phosphoric acid wet etching carries out last figure transfer and prepares patterned sapphire substrate, solve the irregular and high problem of dry etching sapphire cost of etching mask, improved the light extraction efficiency of LED.
Description of drawings
Fig. 1 is at sapphire surface deposition wet etching mask layer schematic diagram;
Fig. 2 is at silica surface spin coating ultraviolet cured adhesive schematic diagram;
Fig. 3 is the compound soft template of fitting, and carries out ultraviolet light curing nano impression schematic diagram;
Fig. 4 sloughs structural adhesive layer schematic diagram after compound soft template;
Fig. 5 is ICP etching remnant layer schematic diagram;
Fig. 6 is ICP etching silicon dioxide layer schematic diagram;
Fig. 7 is that ICP removes remaining glue-line schematic diagram;
Fig. 8 is wet etching Sapphire Substrate schematic diagram;
Fig. 9 is the patterned sapphire substrate schematic diagram that obtains;
Figure 10 is the patterned sapphire substrate of microscopic examination preparation;
Figure 11 is the patterned sapphire substrate that SEM characterizes preparation, and the illustration in the upper right corner is amplification profile.
Embodiment
Below be described in detail the present invention is based on the method that compound soft template nanometer embossing prepares patterned sapphire substrate.The pattern that the present embodiment prepares on Sapphire Substrate is 1 μ m diameter circular hole, and array is the square structure in 3 μ m cycles, and the degree of depth is about 0.45 μ m.
(1) at the surperficial silicon dioxide 2 with PECVD method growth one deck 60nm thickness of 2 inches Sapphire Substrate 1, as the mask layer of wet etching;
(2) coupling processing is carried out on silicon dioxide 2 surfaces, to strengthen the surface energy of silica surface.At silica surface spin coating one deck ultraviolet light polymerization glue-line 3, thickness is about 200nm with sol evenning machine;
(3) compound soft template 4 is fitted on glue-line, that 3 μ m periodic arrays are 1 square μ m diameter cylinder on template, be highly 150nm, the elastic bearing layer of soft template is PDMS, the stamping structure layer is ultra-thin highly cross-linked ultraviolet photocureable material, composition can be the polysiloxanes of acrylic ester grafted polysiloxanes, epoxide group grafting, the polysiloxanes of vinyl ethers grafting, (referring to patent CN101477304A).Due to capillarity, thereby the structure that ultraviolet light polymerization glue-line 3 will infiltrate on compound soft template forms its antistructure.Be placed on N
2Under atmosphere, exposure made ultraviolet light polymerization in 10 minutes;
(4) slough compound soft template 4, glue-line 3 structures that obtain solidifying;
(5) the whole etching glue-line 3 of ICP dry etching, to remove remnant layer, etching gas is O
2
(6) take glue-line 3 as mask, 2 layers of ICP etching silicon dioxides, etching gas are CHF
3And CF
4, in order to guarantee carrying out smoothly of wet etching, the bottom of pore structure must assurance have etched into and has exposed the Sapphire Substrate surface, therefore generally will cross a little to carve and process;
(7) ICP etching glue-line 3 masks prevent that remaining glue-line 3 is carbonized when wet etching, etching gas is O
2
(8) take silicon dioxide layer 2 as mask, utilize sulfuric acid and phosphoric acid mixed liquor wet etching Sapphire Substrate 1, both volume ratio is 3:1, corrosion temperature is about 260 ℃, etching time approximately 20 minutes, due to sapphire crystal structure, surface observation is with triangular in shape;
(9) hydrofluoric acid dips Sapphire Substrate 1 is approximately 15 minutes, to remove 2 layers of silicon dioxide;
(10) utilize acetone, ethanol, the deionized water patterned sapphire substrate 1 approximately 10 minutes of ultrasonic cleaning preparation respectively, technique is completed.
The patterned sapphire substrate figure Circularhole diameter for preparing by said method is 1 μ m, and pitch of holes is 3 μ m, is square structure and arranges, and the degree of depth is about 0.45 μ m, and patterning is substantially undistorted.The present invention utilizes compound soft template nanometer embossing, dry etching, wet etching technology to combine, and has successfully prepared the patterned sapphire substrate than small scale, compares with traditional handicraft, greatly reduces production cost.
Above-described embodiment is exemplary illustration principle of the present invention and effect only, and unrestricted the present invention, within the innovation and creation that any unsubstantiality that does not exceed in connotation scope of the present invention is replaced or revised all fall into protection range of the present invention.
Claims (7)
1. prepare the method for patterned sapphire substrate based on compound soft template nanometer embossing, it is characterized in that: comprise the steps:
(1) deposition one deck wet etching mask layer on Sapphire Substrate, thickness is at 50nm～200nm;
(2) spin coating one deck ultraviolet cured adhesive on the wet etching mask layer then with the soft template applying ultraviolet cured adhesive of patterning, and is placed in N
2Under atmosphere, exposure made adhesive curing in 10 minutes, and the design transfer of soft template to ultraviolet cured adhesive, is sloughed soft template, the glue-line that obtains solidifying;
(3) the etching glue-line exposes the wet etching mask layer, and continues the etch mask layer to exposing Sapphire Substrate;
(4) structure that step (3) is obtained is placed in the mixed solution of sulfuric acid and phosphoric acid, 250 ℃～300 ℃ lower wet etchings 15 minutes～30 minutes, take out Sapphire Substrate, remove mask layer with hydrofluoric acid, and obtain the Sapphire Substrate of patterning after cleaning respectively with acetone, ethanol and deionized water.
2. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 1, it is characterized in that: the pattern for preparing on Sapphire Substrate is the array of circular apertures of square structure, the diameter of circular hole is 0.2～2 μ m, cycle is 0.5～5 μ m, and the degree of depth is 0.2～2 μ m.
3. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 1, it is characterized in that: the wet etching mask layer in described step (1) is earth silicon material.
4. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 3, is characterized in that: the method growth rete of the deposition using plasma enhancing chemical vapour deposition (CVD) in described step (1).
5. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 1, it is characterized in that: in described step (2), the elastic bearing layer of soft template is dimethyl silicone polymer, and its stamping structure layer is ultra-thin highly cross-linked ultraviolet photocureable material.
6. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 1, it is characterized in that: the etching in described step (3) adopts the method for inductively coupled plasma dry etching, and the etching of its mesoglea is taken O
2Gas, the etching of mask layer adopts CHF
3And CHF
4Gas.
7. the method for preparing patterned sapphire substrate based on compound soft template nanometer embossing according to claim 1, it is characterized in that: the sulfuric acid in described step (4) and the volume ratio of phosphoric acid are 2:1～5:1, and corrosion rate is 30～40nm/min.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103995435A (en) * | 2014-05-22 | 2014-08-20 | 西安交通大学 | Nano patterning sapphire substrate and preparation method thereof |
| CN104659166A (en) * | 2015-02-11 | 2015-05-27 | 山东浪潮华光光电子股份有限公司 | Wet-oxygen oxidation method of GaAs-based light emitting diode |
| CN106350783A (en) * | 2016-08-31 | 2017-01-25 | 北京大学 | Method for preparing low-dislocation-density AlGaN film based on MOCVD (metal organic chemical vapor deposition) lateral epitaxy and AlGaN film |
| CN107092162A (en) * | 2016-02-17 | 2017-08-25 | 苏州光舵微纳科技股份有限公司 | A kind of preparation method of nano-imprinting composite template |
| CN108241185A (en) * | 2016-12-26 | 2018-07-03 | 苏州纳邦光电技术有限公司 | Micro nano structure optical element and preparation method and application |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103995435B (en) * | 2014-05-22 | 2017-06-06 | 西安交通大学 | Nano-patterning Sapphire Substrate and preparation method thereof |
| CN103995435A (en) * | 2014-05-22 | 2014-08-20 | 西安交通大学 | Nano patterning sapphire substrate and preparation method thereof |
| CN104659166A (en) * | 2015-02-11 | 2015-05-27 | 山东浪潮华光光电子股份有限公司 | Wet-oxygen oxidation method of GaAs-based light emitting diode |
| CN108463744A (en) * | 2015-12-31 | 2018-08-28 | 沙特基础工业全球技术公司 | Multi-functional classifying nano and lenticule for the extraction efficiency for improving OLED illuminations |
| CN107092162A (en) * | 2016-02-17 | 2017-08-25 | 苏州光舵微纳科技股份有限公司 | A kind of preparation method of nano-imprinting composite template |
| CN106350783A (en) * | 2016-08-31 | 2017-01-25 | 北京大学 | Method for preparing low-dislocation-density AlGaN film based on MOCVD (metal organic chemical vapor deposition) lateral epitaxy and AlGaN film |
| CN106350783B (en) * | 2016-08-31 | 2019-01-15 | 北京大学 | A kind of method and AlGaN film preparing low-dislocation-density AlGaN film based on MOCVD epitaxial lateral overgrowth |
| CN108241185A (en) * | 2016-12-26 | 2018-07-03 | 苏州纳邦光电技术有限公司 | Micro nano structure optical element and preparation method and application |
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