CN103311097A - Method for manufacturing micro-nano graph on sapphire substrate - Google Patents
Method for manufacturing micro-nano graph on sapphire substrate Download PDFInfo
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- CN103311097A CN103311097A CN2013101964936A CN201310196493A CN103311097A CN 103311097 A CN103311097 A CN 103311097A CN 2013101964936 A CN2013101964936 A CN 2013101964936A CN 201310196493 A CN201310196493 A CN 201310196493A CN 103311097 A CN103311097 A CN 103311097A
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Abstract
A method for manufacturing a micro-nano graph on a sapphire substrate comprises the steps of S1, manufacturing a monocrystal film on the sapphire substrate; S2, rotationally coating a layer of photoresist on the monocrystal film; S3, preparing a sequentially arrayed micro-nano ball monolayer film on the photoresist; S4, carrying out exposure on the photoresist by a photoetching machine by the light condensing function of micro-nano balls; S5, removing the micro-nano ball monolayer film and developing the sequentially arrayed photoresist micro-nano hole array; S6, transferring the micro-nano hole array onto the monocrystal film by a dry etching method to form the monocrystal film micro-nano hole array on the monocrystal film; S7, taking the monocrystal film micro-nano hole array as a mask for wet etching the sapphire substrate, thus obtaining sequential micro-nano graph array on the sapphire substrate; and S8, finishing the manufacturing after the monocrystal film mask is removed.
Description
Technical field
The invention belongs to technical field of semiconductors, particularly relate to a kind of method at the micro-nano figure of Sapphire Substrate preparation.
Background technology
At present, the nitride compound semiconductor of III-V family has widely application such as gallium nitride (GaN), aluminium nitride (AlN), indium nitride (InN), aluminium gallium nitride alloy (AlGaN), indium gallium nitride (InGaN), aluminum indium nitride (AlInN), aluminum indium gallium nitride (AlInGaN) etc. in fields such as UV/blue/green light LED, laser, photo-detector, solar cell and power electronic devices.Sapphire Substrate becomes the substrate of the extensive use of nitride epitaxial growth with its low cost.But because heteroepitaxy, Sapphire Substrate and nitride epitaxial layer exist larger lattice adaptive adaptive with thermal expansion, therefore higher stress and higher dislocation density in nitride epitaxial layer greatly reduce the crystal mass of epitaxial material, and then reduce device performance.And extensive use micron graph substrate has improved quality of materials by reducing stress and the dislocation density in the epitaxial loayer at present, has improved simultaneously light extraction efficiency.
And compare with traditional micron graph substrate, the stress of micro-nano graph substrate in can more effective alleviation epitaxial loayer, the dislocation density in the more effective reduction epitaxial loayer, thus improve crystal mass and the device performance of material.But the precision of normal optical lithography is difficult to reach nano level precision usually at the 2-5 micron.And the technology such as the electron beam exposure of the micro/nano level precision of commonly using at present, nano impression need expensive equipment and higher cost.Therefore the development process process simple, low-cost, be convenient to large-area manufacturing, size controlled, be easy to realize that orderly patterned nano graph substrate manufacturing technology is very important.
Summary of the invention
The object of the invention is to, a kind of method at the micro-nano figure of Sapphire Substrate preparation is provided, have technical process simple, low-cost, be convenient to large-area manufacturing, size controlled, be easy to realize in order patterned micro-nano graph substrate manufacturing technology.Be used for improving the crystal mass of nitride epitaxial material and the optical efficiency of its device.
For reaching above purpose, the invention provides a kind of method at the micro-nano figure of Sapphire Substrate preparation, may further comprise the steps:
Step 1: at Sapphire Substrate preparation one monocrystal thin films;
Step 2: spin coating one deck photoresist on monocrystal thin films;
Step 3: at the micro-nano ball monofilm of photoresist preparation one ordered arrangement;
Step 4: utilize the optically focused effect of micro-nano ball, by mask aligner photoresist is exposed;
Step 5: remove the micro-nano ball monofilm, and the photoresist micro-nano hole array of the ordered arrangement that develops;
Step 6: by dry etching the micro-nano hole array is transferred on the monocrystal thin films, formed monocrystal thin films micro-nano hole array at monocrystal thin films;
Step 7: utilize monocrystal thin films micro-nano hole array as mask, the wet etching Sapphire Substrate, thus obtain orderly micro-nano graphic array in Sapphire Substrate;
Step 8: after removing the monocrystal thin films mask, finish preparation.
The invention has the beneficial effects as follows: a kind of method at the micro-nano figure of Sapphire Substrate preparation is provided, can reduce dislocation density in the nitride epitaxial layer with the micro-nano graphical sapphire substrate of the method preparation, improve the crystal mass of nitride epitaxial layer, improve the optical efficiency of nitride photoelectric device, thereby improve the performance of nitride photoelectric device (comprising nitride based light-emitting diode, laser, solar cell and detector etc.).
Description of drawings
In order to further specify content of the present invention, be described in detail below in conjunction with accompanying drawing, embodiment and embodiment, wherein:
Fig. 1 is preparation flow figure of the present invention;
Fig. 2-Fig. 6 is the structure chart of preparation process of the present invention.
Embodiment
Please refer to Fig. 1, and in conjunction with consulting Fig. 2 to shown in Figure 6, the invention provides a kind of method at the micro-nano figure of Sapphire Substrate preparation, may further comprise the steps:
Step 1: at a Sapphire Substrate 1 preparation one monocrystal thin films 2, this Sapphire Substrate 1 is the plane sapphire substrate, and size is not limit, and shape is not limit; The material of described monocrystal thin films 2 be in silicon dioxide, silicon nitride or the carborundum a kind of, two or more, can be one deck, two-layer or multilayer, its thickness is 10nm-10000nm, its preferred thickness is 100nm-500nm, and its preparation method can strengthen the preparation methods such as vapour deposition, electron beam evaporation or magnetron sputtering by using plasma.
Step 2: spin coating one deck photoresist 3 on monocrystal thin films 2, described photoresist 3 is positive photoresist, and its thickness is 100nm-5000nm, and preferred thickness is 200nm-2000nm; The thickness of photoresist can be controlled by the rotating speed of selecting photoresist or adjusting glue spreader; Select the rotating speed of rarer photoresist or increase glue spreader, can reduce the thickness of photoresist; This step need to be carried out can not causing under the lightstruck environment photoresist, such as between gold-tinted, between photoetching, darkroom etc.
Step 3: at the micro-nano ball monofilm 4 of photoresist 3 preparations one ordered arrangement, obtain structure as shown in Figure 2, described ordered arrangement is relatively orderly or local order or complete ordering, can allow local unordered, the material of described micro-nano ball monofilm 4 is silicon dioxide, the micron ball of the organic or inorganic compositions such as polystyrene or poly-methylpropanoic acid methyl esters, and be that the light of 200nm-500nm has certain permeability to wavelength, the diameter of its micro-nano ball is 100nm-5000nm, the preferred diameter of its micro-nano ball is 300nm-2000nm, its preparation method can be spin-coating method, LB embrane method etc. can be prepared the method for micro-nano ball monofilm, this step need to be carried out can not causing under the lightstruck environment photoresist, such as between gold-tinted, between photoetching, darkroom etc.
Step 4: utilize the optically focused effect of micro-nano ball, by mask aligner photoresist 3 is exposed, the used wave-length coverage of described exposure is 200nm-500nm, and its optimal wavelength is 365nm or 405nm, and the time for exposure is 1s-100s; The concrete time needs to determine according to the size of the figure of the used wavelength of used exposure, light intensity, photoresist, developer solution and required acquisition; Can improve the exposure quality by selecting highly sensitive photoresist; This step need to be carried out can not causing under the lightstruck environment photoresist, such as between gold-tinted, between photoetching, darkroom etc.
Step 5: remove micro-nano ball monofilm 4, and the photoresist micro-nano hole array 31 of the ordered arrangement that develops, obtain structure as shown in Figure 3, developing time needs to determine according to the size of the figure of used conditions of exposure, photoresist, developer solution and required acquisition; Can be by selecting to improve with the dilute strength of the developer solution of photoresist coupling and developer solution the systematicness of development quality and figure; This step need to be carried out can not causing under the lightstruck environment photoresist, such as between gold-tinted, between photoetching, darkroom etc.
Step 6: photoresist is carried out with behind hot plate or the baking oven post bake, by dry etching micro-nano hole array 31 is transferred on the monocrystal thin films 2, and after utilizing acetone or stripper cleaning to remove photoresist micro-nano hole array 31, form monocrystal thin films micro-nano hole array 21 at monocrystal thin films 2, obtain structure as shown in Figure 4, the method of described dry etching monocrystal thin films 2 is ICP or RIE etching, also can adopt the method corrosion monocrystal thin films 2 of wet etching; When adopting dry etching or wet etching certain over etching or excessive erosion need be arranged, to guarantee that monocrystal thin films 2 forms monocrystal thin films micro-nano hole array 21 and penetrates fully.
Step 7: utilize monocrystal thin films micro-nano hole array 21 as mask, wet etching Sapphire Substrate 1, thus obtain orderly micro-nano graphic array in Sapphire Substrate 1, obtain structure as shown in Figure 5; The corrosive liquid of described wet etching Sapphire Substrate 1 is the mixed liquor of sulfuric acid and phosphoric acid, and its volume proportion is: 1: 10-10: 1, and the optimum ratio scope is 1: 5-5: 1, more preferably ratio range is 2: 1-4: 1; The corrosion temperature scope is 100 ℃-400 ℃, and preferred range is 250 ℃-350 ℃; Etching time is 1-60 minute, and the concrete time needs to determine according to the proportioning of corrosive liquid and the size of temperature and required acquisition figure.
Step 8: after removing monocrystal thin films 2 masks, the method of described removal monocrystal thin films 2 is put into hydrofluoric acid solution until the mask of monocrystal thin films 2 is completely removed for the Sapphire Substrate 1 after will corroding, immerse again soaking and washing in the sulfuric acid solution, rinse well with deionized water again, obtain structure as shown in Figure 6 after nitrogen dries up, finish preparation.
The figure of the micro-nano graphic array on the wherein said Sapphire Substrate 1 is conical hole, triangular pyramidal hole, square conical pit, five limit conical pits, hexagonal pyramidal hole or polygon conical pit.
The micro-nano graphical sapphire substrate of the method preparation of the micro-nano figure of preparation can be used for the epitaxial growth of the nitride material of III-V family on the above-mentioned Sapphire Substrate, can reduce the dislocation density in the nitride epitaxial layer, improve the crystal mass of nitride epitaxial layer, improve the optical efficiency of nitride photoelectric device, thereby improve the performance of nitride photoelectric device (comprising nitride based light-emitting diode, laser, solar cell and detector etc.).
The above; only be the embodiment among the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with the people of this technology in the disclosed technical scope of the present invention; the conversion that can expect easily or replacement all should be encompassed in of the present invention comprising within the scope.Therefore, protection scope of the present invention should be as the criterion with the protection range of claims.
Claims (10)
1. method at the micro-nano figure of Sapphire Substrate preparation may further comprise the steps:
Step 1: at Sapphire Substrate preparation one monocrystal thin films;
Step 2: spin coating one deck photoresist on monocrystal thin films;
Step 3: at the micro-nano ball monofilm of photoresist preparation one ordered arrangement;
Step 4: utilize the optically focused effect of micro-nano ball, by mask aligner photoresist is exposed;
Step 5: remove the micro-nano ball monofilm, and the photoresist micro-nano hole array of the ordered arrangement that develops;
Step 6: by dry etching the micro-nano hole array is transferred on the monocrystal thin films, formed monocrystal thin films micro-nano hole array at monocrystal thin films;
Step 7: utilize monocrystal thin films micro-nano hole array as mask, the wet etching Sapphire Substrate, thus obtain orderly micro-nano graphic array in Sapphire Substrate;
Step 8: after removing the monocrystal thin films mask, finish preparation.
2. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein Sapphire Substrate is the plane sapphire substrate.
3. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein the material of monocrystal thin films is silicon dioxide, silicon nitride or carborundum, its thickness is 10nm-10000nm.
4. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein photoresist is positive photoresist, its thickness is 100nm-5000nm.
5. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein the material of micro-nano ball monofilm is silicon dioxide, polystyrene or poly-methylpropanoic acid methyl esters, the diameter of micro-nano ball is 100nm-5000nm.
6. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, the used wave-length coverage of wherein exposing is 200nm-500nm.
7. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein the method for dry etching monocrystal thin films is ICP or RIE etching.
8. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein the corrosive liquid of wet etching Sapphire Substrate is the mixed liquor of sulfuric acid and phosphoric acid, its volume proportion is: 1: 10-10: 1, and the corrosion temperature scope is 100 ℃-400 ℃, etching time is 1-60 minute.
9. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein remove the method for monocrystal thin films and put into hydrofluoric acid solution until the mask of monocrystal thin films is completely removed for the Sapphire Substrate after will corroding, immerse in the sulfuric acid solution again and soak, rinse well with deionized water again.
10. the method at the micro-nano figure of Sapphire Substrate preparation according to claim 1, wherein the figure of the micro-nano graphic array on the Sapphire Substrate be that cheat or polygon conical pit in conical hole, triangular pyramidal hole, square conical pit, five limit conical pits, hexagonal pyramidal.
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Cited By (12)
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CN103545173A (en) * | 2013-10-28 | 2014-01-29 | 中国科学院半导体研究所 | Manufacturing method for sapphire template with large-area nanometer patterns |
CN103904175A (en) * | 2014-04-18 | 2014-07-02 | 中国科学院半导体研究所 | Method for manufacturing photonic crystal light-emitting diode of waveguiding structures |
CN103943736A (en) * | 2014-04-24 | 2014-07-23 | 西安神光安瑞光电科技有限公司 | Method for manufacturing pyramid graphic substrate for improving luminance of epitaxial wafer |
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CN104174999B (en) * | 2014-08-13 | 2016-09-21 | 清华大学 | Utilize the method that two-step method prepares surface micro-nano graph |
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CN104355287A (en) * | 2014-11-18 | 2015-02-18 | 中国科学院半导体研究所 | Manufacturing method of multifunctional combined nanometer pattern |
CN104355287B (en) * | 2014-11-18 | 2016-08-24 | 中国科学院半导体研究所 | A kind of multifunctional combination type nano graph preparation method |
CN105177718A (en) * | 2015-06-24 | 2015-12-23 | 哈尔滨工业大学 | Six-edge pyramid graphical sapphire preparation method |
CN105177718B (en) * | 2015-06-24 | 2018-07-03 | 哈尔滨工业大学 | The preparation method of six corner cone graphic sapphires |
CN107346797A (en) * | 2016-05-06 | 2017-11-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Sapphire Substrate nano-pore preparation method |
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