CN103094427A - Method for improving AlGaN-based-ultraviolet (UV)-light-emitting diode (LED) luminous efficiency by utilizing of double-faced patterned substrate - Google Patents
Method for improving AlGaN-based-ultraviolet (UV)-light-emitting diode (LED) luminous efficiency by utilizing of double-faced patterned substrate Download PDFInfo
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Abstract
The invention discloses a method of improving AlGaN-based-ultraviolet (UV)-light-emitting diode (LED) luminous efficiency by utilizing of a double-faced patterned substrate. Stress and dislocation density of the AlGaN-based-LED can be effectively reduced, an AlN template with high quality and a smooth surface atomic-scale is obtained, an AlGaN epitaxial layer with high quality can be further improved, and therefore internal quantum efficiency of the LED can be improved. In addition, due to the fact that the back of the substrate is etched to symmetrical sub-wavelength optical gratings with square patterns, transmission of the light can be further increased, and non-polarized light is obtained. The imaging sapphire substrate technology has the advantages of being simple in craft, low in cost, capable of increasing heat dissipation and the like. Crystal damage can be avoided.
Description
Technical field
The invention belongs to technical field of semiconductors, particularly a kind of basic UV-LED luminous efficiency of two-sided patterned substrate raising AlGaN method of utilizing.The method substrate face is graphical and reverse side two dimension sub-wave length grating effectively combines, and improves largely the exitance of AlGaN base UV-LED internal quantum efficiency and light, thereby has greatly improved the luminous efficiency of UV-LED.
Background technology
Ultraviolet light-emitting diode (UV-LED) is a kind of semiconductor device of launching ultraviolet band under current drives.Studying, develop the focus that such device becomes current wide bandgap semiconductor field of optoelectronic devices, is also to utilize semiconductor material with wide forbidden band to realize a study hotspot of ultraviolet source.At present, ultraviolet source commonly used has mercury lamp, xenon lamp, fluorescent lamp.But these lamp bodies are long-pending large, operating voltage is high and be not very environmental protection, are not very convenient thereby use.In contrast, the basic UV-LED of aluminum gallium nitride (AlGaN) is a kind of semiconductor solid-state optical source, and its volume is little, quality is light, the life-span is long, efficient is high, operating voltage is low.Thereby have broad application prospects in fields such as science and techniques of defence, computer data storage, biologic medical, false proof evaluation, environmental monitoring and public health.The AlGaN material of high alumina (Al) component is a kind of important material of the luminescent device of preparation deep ultraviolet wave band, and important effect is arranged in dual-use market.Aspect civilian, the UV-LED light source is having important application aspect illumination, virus killing, medical treatment, printing, highdensity information storage.
Since nearly more than ten years, the report of relevant UV-LED constantly occurs, particularly after the people such as the American South Carolina M.Khan of state university in 2005 adopted pulse atomic layer metal-organic chemical vapor deposition equipment (MOCVD) technology and superlattice, the emission wavelength of UV-LED constantly moved towards the shortwave direction.2006, the people such as Yoshitaka Taniyasu of Japanese NTT company reported that emission wavelength is the UV-LED based on AlN of 210nm.After this, people have obtained emission wavelength at 230nm-280nm UV-LED by regulating the Al component.Although people pass through to regulate the Al component, can realize from the UV-LED of 210-400nm wave band, along with the raising of Al component, the difficulty for preparing the aspect from the Material growth to the device has also correspondingly improved.The UV-LED of 210nm is under the galvanic driving of 40mA, and luminous power only has 0.02mW, and its external quantum efficiency is lower than 10
-5%.Therefore, improve the developing goal that luminous efficiency and power become UV-LED.
AlGaN base UV-LED is a kind of electro-optical conversioning device of broad stopband.Its transfer process comprises that three steps consist of, and is at first that electronics and hole are injected into active area, is secondly that electronics and hole are luminous in the active area radiation recombination, is that light penetrates from device surface at last.Obtain high luminous efficiency, just must have enough electronics and hole to carry out radiation recombination float to active area under the effect of electric field in, and the light of radiation recombination will shine device surface as much as possible.Yet the dislocation because the lattice mismatch band of sapphire and epitaxial loayer is introduced becomes Trapping Centers or the non-radiative center in electronics or hole, thereby causes the reduction of internal quantum efficiency.Some team adopts the method for extension UV-LED on patterned substrate or graphical AlN, to the crystal mass that obtains by the growth of controlling resilient coating (Buffer).2008, the people such as Amano reported on aluminium nitride (AlN) Buffer and have etched bar paten, then the method for epitaxial lateral overgrowth, and the luminous efficiency of UV-LED has been improved 27 times (with not adopting patterned comparing).But this UV-LED adopts positive luminous method for packing, thereby is difficult to avoid the problem brought because of the low heat conductivility of sapphire.And positive p-type gallium nitride (GaN) has strong absorption to ultraviolet light, makes the efficient of positive bright dipping lower.For this reason, many experts adopt the UV-LED of upside-down mounting (filp-chip) structure.But the refractive index of Sapphire Substrate (~ 1.8) is larger than airborne, and light easily in this interface formation total reflection, is not easy outgoing, thereby causes the recovery rate of light to descend, and luminous power is not high.In order to improve the light extraction efficiency of AlGaN base UV-LED, people have also carried out many-sided research, such as adopting surface coarsening processing, plated surface Bragg grating, utilizing the method such as photonic crystal.But surface coarsening is processed just and is improved the extraction efficiency of light in scattering at the interface by improving light, and its effect is not clearly, and emergent light is relatively dispersed.Although the plated surface Bragg grating can improve the outgoing of light, the design of this film system is subject to the restriction of Refractive Index of Material, and the film that plates easily weares and teares and come off, and unfavorable to dispelling the heat.Photonic crystal is based on photon band gap and comes leaded light, can improve the recovery rate of light, but preparation cost is higher, and most of emergent lights are that polarization is relevant, and have wearing and tearing and this shortcoming that comes off.So develop and a kind ofly can effectively improve AlGaN material crystals quality to improve again the method for light extraction efficiency imperative in the UV-LED R﹠D process.
Summary of the invention
The object of the invention is exactly to be to solve the problem that in above-mentioned UV-LED preparation process, crystal mass is poor and light extraction efficiency is low, proposes a kind of method that adopts two-sided graphical sapphire substrate to improve AlGaN base UV-LED luminous efficiency.
Technical scheme of the present invention is: a kind of two-sided patterned substrate raising AlGaN base UV-LED luminous efficiency method, its step: step 1: deposition layer of silicon dioxide film on Sapphire Substrate utilized; Step 2: utilize photoetching technique to prepare the photoetching offset plate figure array, its graphic element is rectangle;
Step 3: make mask with the photoetching offset plate figure array, utilize the mixed liquor of hydrofluoric acid, ammonium fluoride and water, etch the silica membrane with graphic structure; Step 4: as mask plate, utilize the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with silica membrane with figure, with pattern etching on Sapphire Substrate; Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film, and with deionized water, Sapphire Substrate is cleaned up; Step 6: utilize the metal-organic chemical vapor deposition equipment method, at patterned Grown on Sapphire Substrates low temperature nucleating layer, then the method for raise temperature and conversion III/ V ratio obtains high temperature AlN resilient coating; Step 7: utilize the method for pulsed atomic layer epitaxy, regrowth one deck high temperature AlN layer;
Step 8: the AlGaN of growing n-type doping on high temperature AlN layer; Step 9: extension goes out required multiple quantum well layer and p-type AlGaN electronic barrier layer and p-type AlGaN and p-type GaN layer on N-shaped AlGaN; Step 10: utilize the nano-imprint process of standard, etch again symmetrical rectangular patterns at the Sapphire Substrate back side.
The thickness of wherein said silicon dioxide film is 50 nanometers-2.5 micron.
Wherein said photoetching offset plate figure array is rectangle, and the size of graphic element and spacing are 0.2 micron-1 micron.
Wherein sulfuric acid used and phosphoric acid mixed volume are than being 1:3.
Wherein said etching temperature is at 350 ° of C-450 ° of C, and etch period is 30 seconds-20 minutes.During growing low temperature AlN layer, air pressure is 40torr, and growth temperature is 570 ° of C to 720 ° of C, and thickness is 50nm.
The thickness of wherein said low temperature AI N layer is 50nm, and the thickness of heat zone is 1.5 μ m, and the thickness of pulsed extension is 100nm.
Wherein said multiple quantum well layer is Al
xGa
1-xN/Al
yGa
1-yN, emission wavelength are 280nm.
The symmetrical expression two-dimensional rectangle figure degree of depth at the wherein said sapphire back side is 430nm-630nm, and the foursquare length of side is 80nm-160nm, and the one-period distance is 200nm.
The invention provides a kind of two-sided patterned substrate raising AlGaN base UV-LED luminous efficiency method of utilizing, this method can reduce stress and the dislocation density in AlGaN base UV-LED effectively, obtain the AlN template high-quality, that the surface atom level is smooth, and then obtain high-quality AlGaN epitaxial loayer, thereby improve the internal quantum efficiency of UV-LED.In addition due to the reverse side of the substrate sub-wave length grating of symmetrical square pattern that has been etched, thereby can increase optical transmission, obtain non-polarized light.This graphical sapphire substrate technology has also that technique is simple, cost is low and can strengthen heat radiation and avoid the advantage such as lens lesion.
The invention has the advantages that: there is the figure of specific direction in (1) front, can control the growth of AlN Buffer, thereby can reduce stress and the defective that produces because of lattice mismatch in the Buffer layer, obtains high-quality, the smooth AlN layer of surface atom level; (2) figure of this substrate face is Mitsubishi's taper, makes the refractive index of the material of extension on it change continuously between AlN refractive index and sapphire refractive index, thereby makes light reduce in the reflection at AlN and sapphire interface place; (3) be sub-wave length grating in substrate reverse side etching.The ultraviolet wavelength of this grating period ratio emission is little, by reasonable design etch thicknesses and duty ratio, can realize the enhancing at 0 order diffraction peak, the diffraction light of other grades time do not occur, thereby realizes the anti-reflection of light.Calculate by theory, the transmissivity of this grating can reach more than 99%; (4) this sub-wave length grating is symmetrical rectangular graph grating, thus the birefringence effect that can avoid general asymmetric sub-wave length grating to bring, and the light of outgoing remains non-polarized light; (5) this substrate reverse side micro-structural that is etching, be conducive to heat radiation.
Description of drawings
Fig. 1 is the structural section schematic diagram after the Sapphire Substrate litho pattern;
Fig. 2 is take photoresist array 3 as mask plate, utilizes mixed liquor etching silicon dioxide film 2 schematic cross-section afterwards of hydrofluoric acid, ammonium fluoride and water;
Fig. 3 utilizes etching silicon dioxide film afterwards as mask plate, mix (volume ratio is 3:1) wet method along (10-10) direction (a kind of crystal plane direction) etching Sapphire Substrate 1 with sulfuric acid and phosphoric acid, figure is transferred to generalized section after Sapphire Substrate;
Fig. 4 is that diluted hydrofluoric acid is gone out residual silicon dioxide film 1 and the generalized section after sapphire is cleaned up;
Fig. 5 is the mixed liquor etching Sapphire Substrate 1 that continues with sulfuric acid and phosphoric acid, and Formation cross-section is leg-of-mutton structure;
Fig. 6 is the even curface that forms after extension low temperature AI N nucleating layer and high temperature AlN on Sapphire Substrate;
Fig. 7 continues the N-shaped AlGaN of extension, AlGaN/AlGaN Multiple Quantum Well and p-type barrier layer and p-type GaN on smooth AlN Buffer layer;
Fig. 8 is the interface after sapphire reverse side etching two-dimension square shape sub-wave length grating;
Fig. 9 is the upward view after sapphire reverse side etching two-dimension square shape sub-wave length grating;
In figure: 1 is Sapphire Substrate, and 2 is silica membrane, and 3 is photoetching offset plate figure, and 4 is AlN Buffer layer, and 5 is N-shaped AlGaN, and 6 is Multiple Quantum Well, and 7 is electronic barrier layer, and 8 is p-type AlGaN, and 9 is p-type GaN layer, and 10 is the air gap.
Embodiment
See also Fig. 1-shown in Figure 9, the present invention includes following steps:
Step 1: deposit layer of silicon dioxide film 2(as shown in Figure 1 on Sapphire Substrate 1 with the method for chemical vapor deposition (CVD)), the thickness of this silicon dioxide is 50 nanometers-1.5 micron;
Step 2: utilize photoetching technique to prepare photoetching offset plate figure array 3, its graphic element is rectangle; The graphic element spacing is 0.5 micron-1 micron;
Step 3: make mask with photoetching offset plate figure array 3, utilize the mixed liquor of hydrofluoric acid, ammonium fluoride and water, etch the silica membrane (as shown in Figure 2) with graphic structure;
Step 4: as mask plate, utilize the mixed liquor wet etching Sapphire Substrate 1 of sulfuric acid and phosphoric acid with silica membrane 2 with figure, with pattern etching on Sapphire Substrate (as shown in Figure 3); This sulfuric acid and phosphoric acid mixed volume are than being 1:3, and etching temperature is between 350-450 ° of C, and etch period is 30 seconds-20 minutes;
Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film 2, and with deionized water, Sapphire Substrate is cleaned up (as shown in Figure 4);
Step 6: further etching, making the figure tee section is triangle, then substrate is cleaned up, and oven dry (as shown in Figure 5), etch period is 1min-5min;
Step 7: utilize the metal-organic chemical vapor deposition equipment method, first under the condition of 40torr, 570 ° of C-720 ° of C, growing low temperature AlN nucleating layer on patterned Sapphire Substrate 1, then increase the temperature to 1100 ° of C, first at III clan source and ammonia (NH
3) molar flow is than (V/III) is than being 120000 o'clock, growth 900nm AlN; Reducing V/III ratio is 30000 again, growth 700nm AlN;
Step 8: utilize the method for pulsed atomic layer epitaxy, regrowth one deck high temperature AlN layer 4; Growth temperature is 1050 ° of C, and the pulse period is 0.3min, NH
3Flow be 1500sccm, growth thickness be 100nm(as shown in Figure 6);
Step 9: the AlGaN of growing n-type doping on high temperature AlN layer, extension goes out required multiple quantum well layer and p-type electronic barrier layer and p-type GaN layer (as shown in Figure 7) on N-shaped AlGaN;
Step 10: utilize induction ion beam etching (ICP) technique of standard, etch again symmetrical rectangular patterns (as Fig. 8 and shown in Figure 9) at the Sapphire Substrate back side; The degree of depth of the symmetrical expression two-dimension square shape figure at the sapphire back side is 430nm-630nm, and the foursquare length of side is 80nm-160nm, and the one-period distance is 200nm.
Set forth further technical characterstic of the present invention below by specific embodiment.
The present embodiment is a kind of two-sided patterned substrate raising AlGaN base UV-LED luminous efficiency method of utilizing.
At first at 2 inches
cAdopt the silicon dioxide film 2 of chemical vapor deposition (CVD) deposition techniques 200nm on surface sapphire substrate 1, then utilize the photoetching offset plate figure display 3 of conventional photoetching technique fabrication cycle, graphic element is rectangle, and spacing is 500nm, and the sectional view after photoetching as shown in Figure 1;
Then take the photoresist array as mask plate, utilize the mixed liquor of hydrofluoric acid, ammonium fluoride and water, etch the silica membrane (as shown in Figure 2) with graphic structure;
Then take the silicon dioxide film 2 of graphic structure as mask plate, utilize sulfuric acid and phosphoric acid mixed liquor (volume ratio is 1:3) etching under 450 ° of C
c Surface sapphire substrate 1, the time is 10 minutes, its sectional view is as shown in Figure 3;
Utilize diluted hydrofluoric acid that residual silicon dioxide film 2 wet etchings are removed, the cross section as shown in Figure 4;
Continue the patterned Sapphire Substrate 1 of mixed liquor etching under the condition of 450 ° of C with sulfuric acid and phosphoric acid, make it the surface and form the triangular prism shape, its cross section as shown in Figure 5;
The graphical sapphire substrate that cleans and dry is put in MOCVD equipment, and at 620 ° of C growing AIN nucleating layers, the time is 4.4min, then 1100 ° the growth 30min high temperature AlN layer.At 1050 ° of C, adopt the high temperature AlN layer of the method regrowth 100nm of pulse atomic layer epitaxy at last.The cross section as shown in Figure 6;
Growing n-type AlGaN on high temperature AlN, the AlGaN/AlGaN Multiple Quantum Well in 10 cycles, p-type AlGaN electronic barrier layer, p-type AlGaN, p-type GaN.Its cross section as shown in Figure 7;
At last prepare symmetrical expression two-dimension square shape sub-wave length grating at the sapphire reverse side with the nano-imprint process of standard, the degree of depth of figure is 430nm-630nm, and the foursquare length of side is 80nm-160nm, and the one-period distance is 200nm.The cross section as shown in Figure 8, upward view is as shown in Figure 9.
Above-mentioned example has been described the method for utilizing two-sided graphical sapphire substrate to improve AlGaN base UV-LED luminous efficiency.Due to the front description wet etching, so surperficial smoother is favourable to follow-up crystal growth.And also adopt the pulsed atomic layer epitaxy on high temperature AlN layer, can obtain good AlN surface topography.In addition, what adopted at the back side is nano-imprint process, can accurately control the degree of depth and the width of etching, so preparation sub-wave length grating parameter drift-out design load is less, thereby can realize well anti-reflectionly, and then can improve further the luminous efficiency of AlGaN base UV-LED.
Claims (8)
1. one kind is utilized two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, its step:
Step 1: deposition layer of silicon dioxide film on Sapphire Substrate;
Step 2: utilize photoetching technique to prepare the photoetching offset plate figure array, its graphic element is rectangle;
Step 3: make mask with the photoetching offset plate figure array, utilize the mixed liquor of hydrofluoric acid, ammonium fluoride and water, etch the silica membrane with graphic structure;
Step 4: as mask plate, utilize the mixed liquor wet etching Sapphire Substrate of sulfuric acid and phosphoric acid with silica membrane with figure, with pattern etching on Sapphire Substrate;
Step 5: utilize hydrofluoric acid solution to remove remaining silicon dioxide film, and with deionized water, Sapphire Substrate is cleaned up;
Step 6: utilize the metal-organic chemical vapor deposition equipment method, at patterned Grown on Sapphire Substrates low temperature nucleating layer, then the method for raise temperature and conversion III/ V ratio obtains high temperature AlN resilient coating;
Step 7: utilize the method for pulsed atomic layer epitaxy, regrowth one deck high temperature AlN layer;
Step 8: the AlGaN of growing n-type doping on high temperature AlN layer;
Step 9: extension goes out required multiple quantum well layer and p-type AlGaN electronic barrier layer and p-type AlGaN and p-type GaN layer on N-shaped AlGaN;
Step 10: utilize the nano-imprint process of standard, etch again symmetrical rectangular patterns at the Sapphire Substrate back side.
2. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: the thickness of described silicon dioxide film is 50 nanometers-2.5 micron.
3. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: described photoetching offset plate figure array is rectangle, and the size of graphic element and spacing are 0.2 micron-1 micron.
4. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: sulfuric acid used and phosphoric acid mixed volume are than being 1:3.
5. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: described etching temperature is at 350 ℃-450 ℃, etch period is 30 seconds-20 minutes, during growing low temperature AlN layer, air pressure is 40torr, growth temperature is 570 ℃ to 720 ℃, and thickness is 50nm.
6. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: the thickness of described low temperature AI N layer is 50nm, and the thickness of heat zone is 1.5 μ m, and the thickness of pulsed extension is 100nm.
7. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: described multiple quantum well layer is Al
xGa
1-xN/Al
yGa
1-yN, emission wavelength are 280nm.
8. a kind ofly according to claim 1 utilize two-sided patterned substrate to improve AlGaN base UV-LED luminous efficiency method, it is characterized in that: the symmetrical expression two-dimensional rectangle figure degree of depth at the described sapphire back side is 430nm-630nm, the foursquare length of side is 80nm-160nm, and the one-period distance is 200nm.
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| CN106025025A (en) * | 2016-06-08 | 2016-10-12 | 南通同方半导体有限公司 | Epitaxial growth method capable of improving deep-ultraviolet LED luminous performance |
| CN107623058A (en) * | 2017-08-09 | 2018-01-23 | 甘志银 | It is a kind of to improve deep ultraviolet LED crystal quality and the method for light extraction efficiency simultaneously |
| CN108597988A (en) * | 2018-05-09 | 2018-09-28 | 河源市众拓光电科技有限公司 | A kind of AlGaN base deep ultraviolet LED epitaxial wafer and preparation method thereof grown on a si substrate |
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| CN106025025A (en) * | 2016-06-08 | 2016-10-12 | 南通同方半导体有限公司 | Epitaxial growth method capable of improving deep-ultraviolet LED luminous performance |
| CN107623058A (en) * | 2017-08-09 | 2018-01-23 | 甘志银 | It is a kind of to improve deep ultraviolet LED crystal quality and the method for light extraction efficiency simultaneously |
| CN109728144A (en) * | 2017-10-26 | 2019-05-07 | 丰田合成株式会社 | Template substrate and its manufacturing method and luminescent device |
| CN108597988A (en) * | 2018-05-09 | 2018-09-28 | 河源市众拓光电科技有限公司 | A kind of AlGaN base deep ultraviolet LED epitaxial wafer and preparation method thereof grown on a si substrate |
| CN109841709A (en) * | 2018-12-27 | 2019-06-04 | 江苏澳洋顺昌集成电路股份有限公司 | A kind of preparation method of graphical compound substrate |
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| CN114335280A (en) * | 2021-12-29 | 2022-04-12 | 湘能华磊光电股份有限公司 | Nano-scale patterned sapphire substrate structure suitable for UVC-LED and manufacturing method |
| CN114488362A (en) * | 2022-01-19 | 2022-05-13 | 中国科学院上海光学精密机械研究所 | Sapphire window with double-sided anti-reflection microstructure and preparation method thereof |
| CN115014532A (en) * | 2022-08-01 | 2022-09-06 | 中国工程物理研究院应用电子学研究所 | Three-dimensional polarization measurement system based on sub-wavelength unit structure |
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