CN107634126A - A kind of vertical stratification deep ultraviolet LED complex function P-type electrode and preparation method - Google Patents

A kind of vertical stratification deep ultraviolet LED complex function P-type electrode and preparation method Download PDF

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CN107634126A
CN107634126A CN201710818900.0A CN201710818900A CN107634126A CN 107634126 A CN107634126 A CN 107634126A CN 201710818900 A CN201710818900 A CN 201710818900A CN 107634126 A CN107634126 A CN 107634126A
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layer
preparation
type electrode
deep ultraviolet
complex function
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CN107634126B (en
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李虞锋
云峰
张维涵
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Xian Jiaotong University
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Abstract

The invention discloses a kind of vertical stratification deep ultraviolet LED complex function P-type electrode and preparation method, the preparation method comprises the following steps:Adhesive layer, mirror layer are sequentially prepared by electron beam evaporation or magnetron sputtering on the P faces of the AlGaN base deep ultraviolet epitaxial wafers of cleaning, 3 d function pattern mask is prepared by photoetching, nano impression or nanosphere mask means, three-dimensional complex functional layer is prepared again, and packed layer, separation layer and electrode layer are finally sequentially prepared after cleaning.Complex function P-type electrode prepared by the present invention is used for vertical stratification and inverted structure AlGaN level deep ultraviolet LED, can provide efficient deep ultraviolet band light reflectivity, epitaxial layer can be provided in laser lift-off and support and realize the lossless release of stress.

Description

A kind of vertical stratification deep ultraviolet LED complex function P-type electrode and preparation method
Technical field
The invention belongs to field of photoelectric technology, and in particular to a kind of vertical stratification deep ultraviolet LED complex function P-type electrode And preparation method.
Background technology
AlGaN base deep ultraviolet light sources are in optical storage, chemical analysis, biotechnology, medical sterilization, photoetching, polymer solidify, Many fields such as non line of sight communication have broad application prospects.Compared with GaN base blue light emitting device more ripe at present, The luminous efficiency of the shorter deep-UV light-emitting device of wavelength and power output are much lower at present.Because epitaxial quality is poor, mixes The problems such as miscellaneous efficiency is low, so as to cause, electrical pumping is difficult, lights weaker, carrier congestion and generates heat serious.
Current more research institution has all used inverted structure to prepare AlGaN base deep ultraviolet chips, although light extraction makes moderate progress, But electric current jam still be present.Can be efficiently against light extraction, current spread using vertical stratification the problem of, but it is blue The laser lift-off of jewel substrate/AlN epitaxial layers is a problem:Traditional deep ultraviolet LED electrode, can not be provided in laser lift-off Enough supports, so as to cause epitaxial layer to be ruptured when peeling off;And the reflective mirror electrode system of GaN base blue-ray LED is used, electrode Material has higher absorption to DUV.
Therefore, can be in depth for vertical stratification, inverted structure AlGaN base deep ultraviolet LED, it is necessary to a kind of novel electrode Ultraviolet band provides effective light reflection, while can provide enough stress supports for epitaxial layer in laser lift-off.
The content of the invention
The invention aims to solve above-mentioned technical problem, there is provided a kind of vertical stratification deep ultraviolet LED's is compound Function P-type electrode and preparation method.
To reach above-mentioned purpose, the present invention, which adopts the following technical scheme that, to be achieved:
A kind of preparation method of vertical stratification deep ultraviolet LED complex function P-type electrode, comprises the following steps:
The first step, AlGaN base deep ultraviolet LED epitaxial structures are grown on a sapphire substrate, carried out after growth in situ Carrier activation is realized in annealing;
Second step, the AlGaN base deep ultraviolet LEDs H that will have been grown2SO4With H2O2Mixed solution heating, with After rinse, dry up;
3rd step, the epitaxial wafer P-type layer surface after the cleaning that second step obtains, is splashed by electron beam evaporation platform or magnetic control Penetrate platform and prepare complex function P-type electrode first layer:Adhesive layer;
4th step, in the bonding layer surface that the 3rd step obtains, prepared by electron beam evaporation platform or magnetic control platform compound The function P-type electrode second layer:Mirror layer;
5th step, on the mirror layer surface that the 4th step obtains, three are prepared by photoetching, nano impression or nanosphere mask Functional graphic is tieed up, complex function P-type electrode third layer is prepared by electron beam evaporation platform or magnetic control platform:Three-dimensional complex function Layer;
6th step, in the gap for the three-dimensional complex functional layer that the 5th step obtains, splashed by electron beam evaporation platform or magnetic control Penetrate platform and prepare the 4th layer of complex function P-type electrode:Packed layer;
7th step, in the filling layer surface that the 6th step obtains, prepared by electron beam evaporation platform or magnetic control platform compound Function P-type electrode layer 5:Separation layer;
8th step, in the insulation surface that the 7th step obtains, prepared by electron beam evaporation platform or magnetic control platform compound Function P-type electrode layer 6:Electrode layer.
Of the invention further improve is, in second step, the AlGaN base deep ultraviolet LED matter that will grow Amount percent concentration is 98%H2SO4It is 30%H with mass percent concentration2O2By volume 3:1 mixed solution is heated to 120 DEG C are soaked 20 minutes, then use deionized water rinsing 10 minutes, are finally dried up with nitrogen.
Of the invention further improve is that in the 3rd step, bondline thickness is 0.1nm to 20nm, by nickel, titanium, aluminium, A kind of metal composition in silver, gold, chromium, platinum and palladium.
Of the invention further improve is that in the 4th step, mirror layer thickness is 0nm to 100nm, by nickel, titanium, aluminium, A kind of metal composition in silver, gold, chromium, platinum and palladium, and it is different with the adhesion-layer materials in the 3rd step.
Further improve of the invention is that in the 5th step, three-dimensional complex functional layer thickness is 0.1nm to 2000nm, by A kind of metal composition in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium.
Of the invention further improve is that in the 6th step, packed layer thickness is 0.1nm to 2000nm, by nickel, titanium, aluminium, A kind of metal composition in silver, gold, chromium, platinum and palladium, and it is different with the three-dimensional complex function layer material in the 5th step.
Of the invention further improve is that in the 7th step, separation layer thickness is 1nm to 500nm, by nickel, titanium, aluminium, silver, A kind of metal composition in gold, chromium, platinum and palladium.
Of the invention further improve is that in the 8th step, electrode layers thickness is 10nm to 2000nm, by nickel, titanium, aluminium, A kind of metal composition in silver, gold, chromium, platinum and palladium, and it is different with the insolated layer materials in the 7th step.
Of the invention further improve be, the 3-D graphic in three-dimensional complex functional layer be grid-type raceway groove, tapered raceway groove, In cylinder, pyramid and prism one in or it is several, be highly 1nm to 2 μm, width is 20nm to 500 μm, and round diameter is 20nm to 500 μm, dutycycle 1:0.05 to 1:Between 50, the dutycycle is the width of figure and adjacent two at sustained height The ratio of spacing between figure corresponding points.
A kind of vertical stratification deep ultraviolet LED complex function P-type electrode, is made using above-mentioned preparation method.
The present invention is prepared for complex function P-type electrode in AlGaN base deep ultraviolet LEDs, wherein introducing has The three-dimensional complex functional layer of 3-D graphic feature.Compared with prior art, beneficial effects of the present invention are as follows:Patterned electrode Higher deep ultraviolet band light reflectivity can be ensured, by the control of size, shape to micro-nano graph, and to electrode The selection of material, screening of the mirror layer to reflection wavelength and reflectivity can be effectively realized using forbidden photon band effect.Together When, preferably bonding and supporting role can be provided extension using three-dimensional structure, compared to the reflective mirror of conventional multilayer structure Electrode, the present invention are more beneficial for reducing laser lift-off threshold energy density, reduce core in vertical stratification deep ultraviolet LED techniques The impact stress that piece is subject to, improve laser lift-off yield.
Brief description of the drawings
Fig. 1 is a kind of vertical stratification deep ultraviolet LED complex function P-type electrode schematic diagram of the present invention.
Fig. 2 a are three-dimensional complex functional layer in the inventive method:The side view of grid-type raceway groove.
Fig. 2 b are three-dimensional complex functional layer in the inventive method:The top view of grid-type raceway groove.
Fig. 3 a are three-dimensional complex functional layer in the inventive method:The side view of tapered raceway groove.
Fig. 3 b are three-dimensional complex functional layer in the inventive method:The top view of tapered raceway groove.
Fig. 4 a are three-dimensional complex functional layer in the inventive method:The side view of cylinder.
Fig. 4 b are three-dimensional complex functional layer in the inventive method:The top view of cylinder.
Fig. 5 a are three-dimensional complex functional layer in the inventive method:The side view of pyramid.
Fig. 5 b are three-dimensional complex functional layer in the inventive method:The top view of pyramid.
Fig. 6 a are three-dimensional complex functional layer in the inventive method:The side view of prism
Fig. 6 b are three-dimensional complex functional layer in the inventive method:The top view of prism.
In figure:1 is AlGaN base deep ultraviolet LEDs, and P is face-up;2-7 is complex function P-type electrode, wherein:2 are Adhesive layer;3 be mirror layer;4 be three-dimensional complex functional layer;5 be packed layer;6 be separation layer;7 be electrode layer.
Embodiment
In order that the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with specific embodiment, and join According to accompanying drawing, the present invention is described in further detail.
As shown in Figure 1, Figure 2 a, Fig. 2 b, Fig. 3 a, Fig. 3 b, Fig. 4 a, Fig. 4 b, Fig. 5 a, Fig. 5 b, shown in Fig. 6 a and Fig. 6 b, the present invention carries A kind of preparation method of the vertical stratification deep ultraviolet LED supplied complex function P-type electrode, comprises the following steps:
The first step, AlGaN base deep ultraviolet LED epitaxial structures are grown on a sapphire substrate, carried out after growth in situ Carrier activation is realized in annealing;
Second step, the AlGaN base deep ultraviolets LED 1 grown is used into H2SO4With H2O2Mixed solution heating, with After rinse, dry up;
3rd step, the AlGaN base deep ultraviolet LED 1P type layer surfaces after the cleaning that second step obtains, passes through electricity Beamlet evaporator or magnetic control platform prepare complex function P-type electrode first layer:Adhesive layer 2;
4th step, on the surface of adhesive layer 2 that the 3rd step obtains, prepared by electron beam evaporation platform or magnetic control platform compound The function P-type electrode second layer:Mirror layer 3;
5th step, on the surface of mirror layer 3 that the 4th step obtains, prepared by photoetching, nano impression or nanosphere mask 3 d function figure, complex function P-type electrode third layer is prepared by electron beam evaporation platform or magnetic control platform:Three-dimensional compound work( Ergosphere 4;
6th step, in the gap for the three-dimensional complex functional layer 4 that the 5th step obtains, splashed by electron beam evaporation platform or magnetic control Penetrate platform and prepare the 4th layer of complex function P-type electrode:Packed layer 5;
7th step, on the surface of packed layer 5 that the 6th step obtains, prepared by electron beam evaporation platform or magnetic control platform compound Function P-type electrode layer 5:Separation layer 6;
8th step, on the surface of separation layer 6 that the 7th step obtains, prepared by electron beam evaporation platform or magnetic control platform compound Function P-type electrode layer 6:Electrode layer 7.
Embodiment 1
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 5nm Ni adhesive layers, 30nm Al are deposited successively Mirror layer.
Sample is taken out, by nanosphere mask means, prepares a diameter of 1 μm, dutycycle 1:1 cylinder pattern mask.
Epitaxial wafer with nanosphere mask is put into electron beam evaporation platform, 100nm Al three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 100nm is deposited successively Ti packed layers, 200nm Ti separation layers and 500nm Au electrode layers.
Embodiment 2
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 20nm Pt adhesive layers, 10nm are deposited successively Ti mirror layers.
Sample is taken out, it is 400nm to prepare length by nano impression, is highly 500nm, dutycycle 1:0.5 four ribs Post (cuboid) mask.
Sample with mask is put into magnetic control platform, sputters 500nm Al three-dimensional complex functional layers.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 500nm is deposited successively Ag packed layers, 300nm Ti separation layers and 500nm Au electrode layers.
Embodiment 3
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 0.1nm Pd adhesive layers are deposited successively, do not steam Plate mirror layer.
Sample is taken out, by photoetching, it is 500nm to prepare width, is highly 1500nm, dutycycle 1:50 grid-type raceway groove Mask.
Sample with mask is put into electron beam evaporation platform, 1500nm Au three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, is put into magnetic control platform, 1500nm Al fillings are deposited successively Layer, 500nm Ti separation layers and 2000nm Au electrode layers.
Embodiment 4
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 10nm Cr adhesive layers, 100nm are deposited successively Al mirror layers.
Sample is taken out, by nano impression, the preparation length of side is 250nm, is highly 0.1nm, dutycycle 1:10 six ribs Post pattern mask.
Sample with mask is put into electron beam evaporation platform, 0.1nm Al three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 0.1nm is deposited successively Ni packed layers, 100nm Pt separation layers and 200nm Au electrode layers.
Embodiment 4
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 10nm Cr adhesive layers, 100nm are deposited successively Al mirror layers.
Sample is taken out, by nano impression, the preparation length of side is 250nm, is highly 0.1nm, dutycycle 1:10 six ribs Post pattern mask.
Sample with mask is put into electron beam evaporation platform, 0.1nm Al three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 0.1nm is deposited successively Ni packed layers, 100nm Pt separation layers and 200nm Au electrode layers.
Embodiment 5
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 3nm Ti adhesive layers, 60nm Al are deposited successively Mirror layer.
Sample is taken out, by photoetching, it is 400nm to prepare width, is highly 2000nm, dutycycle 1:2 tapering channel Mask.
Sample with mask is put into electron beam evaporation platform, 2000nm Pt three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 2000nm is deposited successively Al packed layers, 1nm Pd separation layers and 10nm Au electrode layers.
Embodiment 6
A piece of AlGaN bases deep ultraviolet LED is taken, it is 98%H to be put into mass percent concentration2SO4With mass percent Concentration is 30%H2O2By volume 3:1 mixed solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 Minute, finally dried up with nitrogen, complete sample clean.
Epitaxial wafer after cleaning is put on electron beam evaporation platform specimen holder, 15nm Ni adhesive layers, 20nm are deposited successively Al mirror layers.
Sample is taken out, by nanosphere mask means, the preparation length of side is 20nm, dutycycle 1:0.05 triangular pyramid figure is covered Mould.
Sample with mask is put into electron beam evaporation platform, 50nm Al three-dimensional complex functional layers are deposited.
Sample is taken out, by the common process such as removing photoresist, cleaning, electron beam evaporation platform is placed again into, 50nm Ag is deposited successively Packed layer, 100nm Ti separation layers and 100nm Au electrode layers.
Particular embodiments described above, the purpose of the present invention, technical scheme and beneficial effect are carried out further in detail Describe in detail bright, it should be understood that the foregoing is only the present invention specific embodiment, be not intended to limit the invention, it is all Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., the protection of the present invention should be included in Within the scope of.

Claims (10)

1. a kind of preparation method of vertical stratification deep ultraviolet LED complex function P-type electrode, it is characterised in that including following step Suddenly:
The first step, AlGaN base deep ultraviolet LED epitaxial structures are grown on a sapphire substrate, in-situ annealing is carried out after growth Realize carrier activation;
Second step, the AlGaN base deep ultraviolet LEDs H that will have been grown2SO4With H2O2Mixed solution heating, with backlash Wash, dry up;
3rd step, the epitaxial wafer P-type layer surface after the cleaning that second step obtains, passes through electron beam evaporation platform or magnetic control platform Prepare complex function P-type electrode first layer:Adhesive layer;
4th step, in the bonding layer surface that the 3rd step obtains, complex function P is prepared by electron beam evaporation platform or magnetic control platform The type electrode second layer:Mirror layer;
5th step, on the mirror layer surface that the 4th step obtains, three-dimensional work(is prepared by photoetching, nano impression or nanosphere mask Energy figure, passes through electron beam evaporation platform or magnetic control platform prepares complex function P-type electrode third layer:Three-dimensional complex functional layer;
6th step, in the gap for the three-dimensional complex functional layer that the 5th step obtains, pass through electron beam evaporation platform or magnetic control platform Prepare the 4th layer of complex function P-type electrode:Packed layer;
7th step, in the filling layer surface that the 6th step obtains, complex function P is prepared by electron beam evaporation platform or magnetic control platform Type electrode layer 5:Separation layer;
8th step, in the insulation surface that the 7th step obtains, complex function P is prepared by electron beam evaporation platform or magnetic control platform Type electrode layer 6:Electrode layer.
2. preparation method according to claim 1, it is characterised in that in second step, the AlGaN base deep ultraviolets that will grow LED is 98%H with mass percent concentration2SO4It is 30%H with mass percent concentration2O2By volume 3:1 it is mixed Conjunction solution is heated to 120 DEG C and soaked 20 minutes, then uses deionized water rinsing 10 minutes, is finally dried up with nitrogen.
3. preparation method according to claim 1, it is characterised in that in the 3rd step, bondline thickness be 0.1nm extremely 20nm, it is made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium.
4. preparation method according to claim 1, it is characterised in that in the 4th step, mirror layer thickness be 0nm extremely 100nm, it is made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium, and with the adhesion-layer materials in the 3rd step not Together.
5. preparation method according to claim 1, it is characterised in that in the 5th step, three-dimensional complex functional layer thickness is 0.1nm to 2000nm, it is made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium.
6. preparation method according to claim 1, it is characterised in that in the 6th step, packed layer thickness be 0.1nm extremely 2000nm, be made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium, and with the three-dimensional complex function in the 5th step Layer material is different.
7. preparation method according to claim 1, it is characterised in that in the 7th step, separation layer thickness is 1nm to 500nm, It is made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium.
8. preparation method according to claim 1, it is characterised in that in the 8th step, electrode layers thickness be 10nm extremely 2000nm, it is made up of a kind of metal in nickel, titanium, aluminium, silver, gold, chromium, platinum and palladium, and with the insolated layer materials in the 7th step not Together.
9. preparation method according to claim 1, it is characterised in that the 3-D graphic in three-dimensional complex functional layer is grid-type In raceway groove, tapered raceway groove, cylinder, pyramid and prism one in or it is several, be highly 1nm to 2 μm, width is 20nm to 500 μ M, round diameter are 20nm to 500 μm, dutycycle 1:0.05 to 1:Between 50, the dutycycle be sustained height at, figure The ratio of spacing between width and adjacent two figures corresponding points.
10. a kind of vertical stratification deep ultraviolet LED complex function P-type electrode, it is characterised in that appoint using in claim 1 to 9 Preparation method described in one is made.
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Publication number Priority date Publication date Assignee Title
CN102130259A (en) * 2011-01-14 2011-07-20 大连美明外延片科技有限公司 Composite electrode of light-emitting diode chip and manufacturing methods thereof
CN103325911A (en) * 2012-03-23 2013-09-25 奇力光电科技股份有限公司 Light emitting diode element and manufacturing method thereof
CN105679895A (en) * 2016-03-30 2016-06-15 河北工业大学 Preparation method of vertical ultraviolet LED chip
CN106972088A (en) * 2017-05-25 2017-07-21 合肥彩虹蓝光科技有限公司 A kind of LED metal electrode structures and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102130259A (en) * 2011-01-14 2011-07-20 大连美明外延片科技有限公司 Composite electrode of light-emitting diode chip and manufacturing methods thereof
CN103325911A (en) * 2012-03-23 2013-09-25 奇力光电科技股份有限公司 Light emitting diode element and manufacturing method thereof
CN105679895A (en) * 2016-03-30 2016-06-15 河北工业大学 Preparation method of vertical ultraviolet LED chip
CN106972088A (en) * 2017-05-25 2017-07-21 合肥彩虹蓝光科技有限公司 A kind of LED metal electrode structures and preparation method thereof

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