CN104241465A - Nano coarsening composite graphical sapphire substrate and manufacturing method - Google Patents
Nano coarsening composite graphical sapphire substrate and manufacturing method Download PDFInfo
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- CN104241465A CN104241465A CN201410486688.9A CN201410486688A CN104241465A CN 104241465 A CN104241465 A CN 104241465A CN 201410486688 A CN201410486688 A CN 201410486688A CN 104241465 A CN104241465 A CN 104241465A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
Provided are a nano coarsening composite graphical sapphire substrate and a manufacturing method thereof. The sapphire substrate is provided with a composite graphic formed by combining micron dimension graphics with nano dimension graphics, and the nano dimension graphics are arranged on the micron dimension graphics. The manufacturing method includes the steps that (1) the micron dimension graphics are manufactured on the sapphire substrate; (2) a silicon dioxide film is deposited on the micron dimension graphics; (3) a silver film is further deposited on the silicon dioxide film; (4) the silver film is agglomerated into silver nanoparticles; (5) silver nanoparticle graphics are transferred onto the silicon dioxide film; (6) the silver nanoparticles are corroded; (7) the nano dimension graphics are manufactured on the sapphire micron graphics; (8) a silicon dioxide mask layer is removed in a corroded mode; (9) the substrate is cleaned. Nano coarsening is carried out on the micron dimension graphics, the light propagation direction can be changed more efficiently, the light escape probability is increased, and the light extraction efficiency and light output power of a GaN-based LED of the sapphire substrate are improved.
Description
Technical field
The present invention relates to Sapphire Substrate of a kind of nanometer alligatoring compound pattern for epitaxial growth GaN crystal and preparation method thereof, belong to semiconductor crystal preparing technical field.
Background technology
GaN has the characteristics such as wide direct band gap, high electron saturation velocities, high breakdown electric field and high heat conductance, has very large application potential at photoelectron and microelectronic.GaN and other III group nitride (InN, AlN) can form ternary or quaternary solid solution, and its energy gap is from 0.7eV to 6.28eV, and emission wavelength, from infrared adjustable to ultraviolet, obtains extensive use at blue green light and ultraviolet band opto-electronic device.
Owing to lacking large scale GaN substrate, current GaN film is generally grown by heteroepitaxy on the substrates such as sapphire, carborundum and silicon.Sapphire is due to low price, and transparency is high, chemical stability and Heat stability is good, is the most frequently used substrate of current commercialization GaN base LED.
The lattice mismatch about 16% of GaN film and Sapphire Substrate, therefore the GaN film of Sapphire Substrate Epitaxial growth has higher dislocation density.The refractive index of GaN about 2.4 in addition, much larger than the refractive index of air, therefore total reflection effect can reduce the light extraction efficiency of LED.
Prepare the figure of nanometer or micron dimension on a sapphire substrate, can make GaN that horizontal extension occurs, improve the crystal mass of GaN film.Figure can change the direction of propagation of light in addition, suppresses total reflection effect, improves the light extraction efficiency of GaN base LED.
Chinese patent literature CN102064088B disclosed " a kind of dry etching and wet etching are mixed with the method for sapphire pattern substrate ", make mask by silicon dioxide or silicon nitride, first utilize ICP dry etching silicon dioxide or silicon nitride mask, the triangle of formation rule and ring-shaped figure, then adopt the mixed solution wet etching sapphire of sulfuric acid and phosphoric acid, prepare sapphire pattern substrate.The CN102184842B disclosed method of graphic sapphire " a kind of wet etching combine with dry etching " deposits layer of silicon dioxide film on a sapphire substrate; Utilize photoetching technique on described silicon dioxide film, prepare the photoresist mask of band figure; Litho pattern is etched on silicon dioxide film; With patterned silicon dioxide film for mask, adopt wet etching in conjunction with the method for short time dry etching, by pattern etching in Sapphire Substrate; Wet etching removes silicon dioxide film, and Sapphire Substrate is cleaned up, and completes the preparation of graphical sapphire substrate.
CN102881791A disclosed " a kind of sapphire LED graph substrate and preparation method thereof ", deposit DBR on a sapphire substrate in advance, then inductively coupled plasma (ICP) dry etching technology is adopted to prepare figure, finally obtain the Sapphire Substrate with graphical DBR, be actually the novel graphic substrate depositing DBR reflector on a sapphire substrate in advance.
CN102790150A disclosed " manufacture method of the bowl-shape sapphire pattern substrate of a kind of nanometer ", it is cvd silicon dioxide film on cesium chloride nano island, cesium chloride nano island is removed afterwards by ultrasonic method, silicon dioxide becomes etch mask, adopts the preparation of ICP technology to have the Sapphire Substrate of the bowl-shape figure of nanometer.
Graphical sapphire substrate in above-mentioned document all just has the figure of single micron dimension, and its structure as shown in Figure 1, is prepare micron dimension figure 2 in Sapphire Substrate 1.The light that GaN base LED active area sends reflects through the figure of micron-scale, the direction of propagation can be changed, increase escape probability, but still have very most of light to be limited in GaN film and Sapphire Substrate inside because of total reflection effect, cause optical output power on the low side.
Summary of the invention
The present invention is directed to the problem lower at the light extraction efficiency of the GaN base LED prepared with it (light-emitting diode) that existing graphical sapphire substrate exists, a kind of Sapphire Substrate that can obtain the nanometer alligatoring compound pattern of high light extraction efficiency GaN base LED is provided, a kind of preparation method of this graphical sapphire substrate is provided simultaneously.
The Sapphire Substrate of nanometer alligatoring compound pattern of the present invention, it has the compound pattern that micron dimension figure and nanometer scale figure combine, micron dimension figure arranges nanometer scale figure.
Described micron dimension figure is the hemisphere of micron dimension, round platform, circular cone, pyramid or terrace with edge.The height of described micron dimension figure is 1 μm-10 μm, basal diameter (basal diameter of pyramid and terrace with edge is its most long-diagonal) 2 μm-20 μm.
Described nanometer scale figure is pyramid, terrace with edge, hemisphere or other any irregular figure.The height of described nanometer scale figure is 10nm-500nm, and bottom width is 1nm-500nm.
The preparation method of the Sapphire Substrate of above-mentioned nanometer alligatoring compound pattern, prepares micron dimension figure first on a sapphire substrate, and then prepare nanometer scale figure on micron dimension figure; Specifically comprise the following steps:
(1) figure of micron dimension is prepared on a sapphire substrate;
This micron dimension figure is the hemisphere of micron dimension, round platform, circular cone, pyramid or terrace with edge, and the height of micron dimension figure is 1 μm-10 μm, basal diameter (basal diameter of pyramid and terrace with edge, i.e. its most long-diagonal) 2 μm-20 μm.
(2) figure of the micron dimension formed in step (1) deposits the silica membrane of a layer thickness 200nm-1000nm;
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 50nm-500nm again;
(4) annealed in air or oxygen by the substrate that step (3) is formed, annealing temperature 300-900 DEG C, 30 seconds-1000 seconds time, makes Ag films be agglomerated into silver nano-grain, and the figure that silver nano-grain is formed is silver nano-grain figure;
The Ag films of different-thickness, coordinates and controls annealing temperature and annealing time, and can to form pyramid, terrace with edge, hemisphere or other any irregular height be 10nm-500nm and bottom width is the silver nano-grain figure of 1nm-500nm.
(5) by silver nano-grain Graphic transitions on silica membrane, silica membrane forms nano graph;
By the method for existing conventional ICP dry etching or wet etching.ICP dry etch step: load in ICP etching apparatus by the Sapphire Substrate with silver nano-grain figure, setting ICP etching apparatus technological parameter, transfers to photoetching offset plate figure in Sapphire Substrate.Wet etching method step, has the Sapphire Substrate of silver nano-grain figure with acid solution corrosion, by its Graphic transitions in Sapphire Substrate, rinsing dries.
(6) corrosive liquid is adopted to be eroded by silver nano-grain;
Corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:3-3:1, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:10-1:0.2;
(7) on sapphire micron figure, nanometer scale figure is prepared;
(8) corrosive liquid erosion removal earth silicon mask layer is adopted;
Corrosive liquid is the mixed solution of hydrofluoric acid and water or the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of hydrofluoric acid and water is 2:9-4:3, and the volume ratio of ammoniacal liquor, hydrogen peroxide and water is 1:1:2;
(9) adopt acetone, ethanol and deionized water to clean step (8) gained substrate respectively, finally obtain the Sapphire Substrate with micron and nano combined figure.
The present invention prepares the compound pattern of micron dimension figure and nanometer scale figure on a sapphire substrate, nanometer alligatoring is carried out to the figure of micron-scale, can the direction of propagation of more effective change light, improve the probability of light effusion, increase light extraction efficiency and the optical output power of Sapphire Substrate GaN base LED.
Accompanying drawing explanation
Fig. 1 is the generalized section of Conventional patterning Sapphire Substrate.
Fig. 2 is the generalized section with the Sapphire Substrate of nanometer alligatoring compound pattern of the present invention.
Fig. 3 is the enlarged local section schematic diagram of Sapphire Substrate prepared by the present invention.
In figure: 1, Sapphire Substrate; 2, micron dimension figure; 3, compound pattern; 4, nanometer scale figure.
Embodiment
As shown in Figure 2, the Sapphire Substrate 1 of nanometer alligatoring compound pattern of the present invention has the compound pattern that micron dimension figure 2 and nanometer scale figure combine, micron dimension figure 2 arranges nanometer scale figure, forms the micron figure 3 with nanometer alligatoring.The preparation method of the Sapphire Substrate of nanometer alligatoring compound pattern of the present invention can be undertaken by described in following examples.
Embodiment 1
(1) in Sapphire Substrate 1, micron dimension figure 2 is prepared.
The ICP of existing routine or wet etching method is adopted (to deposit layer of silicon dioxide mask on a sapphire substrate; Mask layer is coated with last layer photoresist, utilizes ICP equipment etching mask layer, form mask pattern; With sulfuric acid and phosphoric acid mixed solution wet etching sapphire.)。Micron dimension figure can be hemisphere, pyramid or terrace with edge, and the height of figure is 1 μm, and basal diameter is 2 μm (basal diameter of pyramid and terrace with edge, i.e. its most long-diagonals).
(2) substrate is cleaned, then the silica membrane of deposit thickness 200nm on micron dimension figure 1.
(3) substrate is cleaned, then the Ag films of deposit thickness 50nm on silica membrane, anneal in atmosphere, temperature 300 degree, 1000 seconds time, Ag films is reunited in silver nano-grain, the irregular silver nano-grain figure of the figure that silver nano-grain is formed to be height be 10nm, bottom width 500nm.
(4) by the ICP dry etching figure transfer method of existing routine by nano particle Graphic transitions on silica membrane, etching gas is sulphur hexafluoride.
(5) erosion removal silver nano-grain, corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:3, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:5;
(6) adopt the ICP dry etching Sapphire Substrate of existing routine, micron figure carries out nanometer alligatoring, obtains nanometer scale figure 4.
(7) substrate described in step (6) is put into mixed solution (volume ratio of hydrofluoric acid and water is 1:1) the erosion removal silicon dioxide etch mask of hydrofluoric acid and water, acetone, ethanol and deionized water is adopted to clean gained substrate respectively, obtain the Sapphire Substrate with compound pattern 3 (micron dimension figure 2 having nanometer scale figure 4), as shown in figure Fig. 2 and Fig. 3.
Embodiment 2
(1) identical with the step (1) of embodiment 1.
(2) substrate is cleaned, then the silica membrane of deposit thickness 1000nm on micron dimension figure 1.
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 500nm again; Anneal in oxygen, temperature 900 degree, time 30s, makes Ag films reunite in nano particle, the irregular silver nano-grain figure that the figure that silver nano-grain is formed is is highly 30nm, bottom width is 200nm.
(4) by wet etching graph transfer method by nano particle Graphic transitions on silica membrane, specifically adopt the aqueous solution of hydrofluoric acid (volume ratio of hydrofluoric acid and water is 1:5) by nano particle Graphic transitions on silica membrane.
(5) erosion removal silver nano-grain, corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 2:3, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:10.
(6) adopt the mixed solution (volume ratio of sulfuric acid and phosphoric acid is 1:1) of sulfuric acid and phosphoric acid to corrode Sapphire Substrate, micron figure carries out nanometer alligatoring, obtains nanometer scale figure 4.
(7) be 4:9 with step (7) in embodiment 1 unlike the volume ratio of hydrofluoric acid and water.
Embodiment 3
(1) identical with the step (1) of embodiment 1.
(2) figure of the micron dimension formed in step (1) deposits the silica membrane of a layer thickness 500nm;
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 300nm again; Anneal in atmosphere, temperature 700 degree, time 200s, makes Ag films reunite in nano particle, the irregular silver nano-grain figure that the figure that silver nano-grain is formed is is highly 155nm, bottom width is 20nm.
(4) identical with the process of step (4) in embodiment (1).
(5) erosion removal silver nano-grain, corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 3:1, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:0.2.
(6) identical with the process of step (6) in embodiment (1).
(7) substrate described in (6) is put into mixed solution (volume ratio of ammoniacal liquor, hydrogen peroxide and water is 1:1:2) the erosion removal silicon dioxide etch mask of ammoniacal liquor, hydrogen peroxide and water, adopt acetone, ethanol and deionized water to clean gained substrate respectively, obtain the Sapphire Substrate with nanometer alligatoring compound pattern.
Embodiment 4
(1) identical with the step (1) of embodiment 1.
(2) figure of the micron dimension formed in step (1) deposits the silica membrane of a layer thickness 400nm;
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 200nm again; Anneal in oxygen, temperature 500 degree, time 500s, makes Ag films reunite in nano particle, the irregular silver nano-grain figure that the figure that silver nano-grain is formed is is highly 200nm, bottom width is 1nm.
(4) identical with the process of step (4) in embodiment (2).
(5) erosion removal silver nano-grain, corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:2, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:7.
(6) identical with the process of step (6) in embodiment (1).
(7) be 2:3 with step (7) in embodiment 1 unlike the volume ratio of hydrofluoric acid and water.
Embodiment 5
(1) identical with the step (1) of embodiment 1.
(2) figure of the micron dimension formed in step (1) deposits the silica membrane of a layer thickness 800nm;
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 400nm again; Anneal in atmosphere, temperature 400 degree, time 700s, makes Ag films reunite in nano particle, the irregular silver nano-grain figure that the figure that silver nano-grain is formed is is highly 500nm, bottom width is 70nm.
(4) identical with the process of step (4) in embodiment (1).
(5) erosion removal silver nano-grain, corrosive liquid is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, and the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:1, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:1.
(6) identical with the process of step (6) in embodiment 2.
(7) be 4:3 with step (7) in embodiment 1 unlike the volume ratio of hydrofluoric acid and water.
Claims (8)
1. a Sapphire Substrate for nanometer alligatoring compound pattern, is characterized in that, this Sapphire Substrate has the compound pattern that micron dimension figure and nanometer scale figure combine, micron dimension figure arranges nanometer scale figure.
2. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 1, is characterized in that, described micron dimension figure is the hemisphere of micron dimension, round platform, circular cone, pyramid or terrace with edge.
3. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 1, is characterized in that, the height of described micron dimension figure is 1 μm-10 μm, basal diameter 2 μm-20 μm.
4. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 1, is characterized in that, described nanometer scale figure is pyramid, terrace with edge, hemisphere or other any irregular figure.
5. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 1, is characterized in that, the height of described nanometer scale figure is 10nm-500nm, and bottom width is 1nm-500nm.
6. a preparation method for the Sapphire Substrate of nanometer alligatoring compound pattern described in claim 1, is characterized in that, comprise the following steps:
(1) figure of micron dimension is prepared on a sapphire substrate;
(2) figure of the micron dimension formed in step (1) deposits the silica membrane of a layer thickness 200nm-1000nm;
(3) on the silica membrane of step (2), deposit the Ag films of a layer thickness 50nm-500nm again;
(4) annealed in air or oxygen by the substrate that step (3) is formed, annealing temperature 300-900 DEG C, 30 seconds-1000 seconds time, makes Ag films be agglomerated into silver nano-grain, and the figure that silver nano-grain is formed is silver nano-grain figure;
(5) by silver nano-grain Graphic transitions on silica membrane, silica membrane forms nano graph;
(6) corrosive liquid is adopted to be eroded by silver nano-grain;
(7) on sapphire micron figure, nanometer scale figure is prepared;
(8) corrosive liquid is adopted to remove earth silicon mask layer;
(9) adopt acetone, ethanol and deionized water to clean step (8) gained substrate respectively, finally obtain the Sapphire Substrate with micron and nano combined figure.
7. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 6, it is characterized in that, corrosive liquid in described step (6) is the mixed solution of ammoniacal liquor, hydrogen peroxide and water, the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:3-3:1, and the mixed liquor of ammoniacal liquor and hydrogen peroxide and the volume ratio of water are 1:10-1:0.2.
8. the Sapphire Substrate of nanometer alligatoring compound pattern according to claim 6, it is characterized in that, corrosive liquid corrosive liquid in described step (8) is the mixed solution of hydrofluoric acid and water or the mixed solution of ammoniacal liquor, hydrogen peroxide and water, the volume ratio of hydrofluoric acid and water is 2:9-4:3, and the volume ratio of ammoniacal liquor, hydrogen peroxide and water is 1:1:2.
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| CN105742440A (en) * | 2014-12-30 | 2016-07-06 | 嘉德晶光电股份有限公司 | Patterned structural substrate and optoelectronic semiconductor element |
| CN106025030A (en) * | 2016-08-08 | 2016-10-12 | 泉州市三星消防设备有限公司 | Method for preparing patterned substrate with double-hierarchy layer |
| CN106449921A (en) * | 2015-08-12 | 2017-02-22 | 固美实国际股份有限公司 | Patterned substrate for light emitting diodes |
| CN106469769A (en) * | 2015-08-17 | 2017-03-01 | 南通同方半导体有限公司 | A kind of micro-nano graph Sapphire Substrate and preparation method thereof |
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| CN106449921B (en) * | 2015-08-12 | 2018-12-28 | 固美实国际股份有限公司 | Patterned substrate for light emitting diodes |
| CN106449921A (en) * | 2015-08-12 | 2017-02-22 | 固美实国际股份有限公司 | Patterned substrate for light emitting diodes |
| CN106469769A (en) * | 2015-08-17 | 2017-03-01 | 南通同方半导体有限公司 | A kind of micro-nano graph Sapphire Substrate and preparation method thereof |
| CN106025030B (en) * | 2016-08-08 | 2018-10-23 | 泉州市三星消防设备有限公司 | It is a kind of that there is pair preparation method of the patterned substrate of classes' figure layer |
| CN106025030A (en) * | 2016-08-08 | 2016-10-12 | 泉州市三星消防设备有限公司 | Method for preparing patterned substrate with double-hierarchy layer |
| CN107123705A (en) * | 2017-03-17 | 2017-09-01 | 华灿光电（浙江）有限公司 | A kind of preparation method of light emitting diode |
| CN107123705B (en) * | 2017-03-17 | 2019-06-11 | 华灿光电（浙江）有限公司 | A kind of preparation method of light emitting diode |
| CN106960897A (en) * | 2017-04-18 | 2017-07-18 | 仇凯弘 | A kind of preparation method of compound pattern substrate |
| CN108807609A (en) * | 2018-05-03 | 2018-11-13 | 五邑大学 | The preparation method of the patterned substrate LED of metal nanoparticle modification |
| CN108807609B (en) * | 2018-05-03 | 2020-07-14 | 五邑大学 | Preparation method of metal nanoparticle modified patterned substrate L ED |
| CN115020563A (en) * | 2022-06-01 | 2022-09-06 | 淮安澳洋顺昌光电技术有限公司 | Preparation method of graphic substrate with micro-nano structure and epitaxial structure |
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