CN102097548A - Method for preparing self-supported GaN-based light emitting diode - Google Patents
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Abstract
The invention relates to a method for preparing a self-supported GaN-based light emitting diode, which comprises the steps: based on the adoption of a metal-oxide chemical vapor deposition method, growing a ZnO buffer layer, a ZnO epitaxial and a GaN anticorrosive layer in sequence on a sapphire substrate at first to form a composite substrate; then growing a GaN or AlN buffer layer, a non-doped GaN transition layer, a n-type GaN epitaxial layer, a GaN/InGaN multi-quantuam-well light emitting layer, a p-type GaN epitaxial layer and a current diffusion layer in sequence on the composite substrate, plating a p-type GaN contact electrode on the current diffusion layer, and plating a n-type GaN contact electrode on the n-type GaN epitaxial layer in parallel to the GaN/InGaN multi-quantuam-well light emitting layer; and finally, peeling off the sapphire layer, the ZnO buffer layer, the ZnO epitaxial layer and the GaN anticorrosive layer by means of an acid liquor corrosion method. By using the method, radiation prominently can be improved and the light-emitting device with large power and high brightness can be obtained, and simultaneously, sapphires can be recovered and reused, which is beneficial for lowering production cost.
Description
Technical field
The present invention relates to a kind of preparation method of self-supporting GaN based light-emitting diode, belong to technical field of semiconductor luminescence.
Background technology
The GaN based light-emitting diode has important application prospects and commercial value in fields such as illumination, demonstration, scientific researches.Traditional GaN based light-emitting diode structure as shown in Figure 1, generally with sapphire sheet 201 as substrate, adopt Metalorganic Chemical Vapor Deposition growing GaN or AlN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively from bottom to top on substrate, p type GaN epitaxial loayer 206 and current-diffusion layer 207, and on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
Because Sapphire Substrate has big gap at crystal structure, thermal conductivity and GaN, is easy to generate lattice mismatch and thermal stress mismatch, because the sapphire insulation and thermal insulation is functional, is unfavorable for making the high-power light-emitting device simultaneously.Sapphire Substrate must be cut after element manufacturing was finished, thereby finished follow-up packaging technology, caused Sapphire Substrate to reuse.In sum, simple Sapphire Substrate can not satisfy the preparation requirement of the high-power GaN based light-emitting diode of high-performance.
Undoubtedly, the GaN monocrystalline is the best substrate of preparation GaN base luminescent device.Yet GaN single-chip diameter is very little and cost an arm and a leg.ZnO has a lot of similar character to GaN at aspects such as crystal structure, band structures, particularly importantly both are wurtzite structure, have identical stacking sequence, lattice mismatch and thermal mismatching are very little simultaneously, so ZnO can be used as the template of GaN base film growth.Since with respect to GaN, the ZnO abundant raw material, cheap, be easy to corrosion, in conjunction with having the technology that Sapphire Substrate prepares the GaN base luminescent device now, can realize peeling off of GaN base film and substrate easily, thus the good high-power and high-luminance device of preparation heat radiation.
Realize above-mentioned technical two major issues that need to solve that are envisaged in: the first, for suitability for industrialized production, the selling at exorbitant prices of ZnO monocrystalline; The second, in GaN outer layer growth temperature and ammonia atmosphere, the ZnO layer is corroded easily and influences the crystal mass of subsequent growth film.So adopting ZnO single crystalline substrate or metal organic chemical vapor deposition parameter commonly used to be not suitable for growing with ZnO is the GaN based light-emitting diode of transition zone.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of self-supporting GaN based light-emitting diode, improve the heat radiation of luminescent device, be easy to obtain high-power, high brightness light-emitting devices, and can effectively reduce production cost.
The preparation method of the GaN based light-emitting diode of self-supporting of the present invention, the GaN based light-emitting diode of this self-supporting has GaN or AlN resilient coating, non-Doped GaN transition zone, n type GaN epitaxial loayer, GaN/InGaN multiple quantum well light emitting layer from bottom to top successively on the GaN etch resistant layer, p type GaN epitaxial loayer and current-diffusion layer, and on current-diffusion layer plating p type GaN contact electrode, on n type GaN epitaxial loayer, be listed in GaN/InGaN multiple quantum well light emitting layer plating n type GaN contact electrode, what its preparation was adopted is Metalorganic Chemical Vapor Deposition, and step is as follows:
1) will vacuumize, at 250-400 ℃ through the Sapphire Substrate of the cleaning metal organic chemical vapor deposition device reaction chamber of packing into, organic zinc source flow 5-100sccm, the purity oxygen flow is 10-200sccm, and air pressure is 0.01-150Torr, and growth thickness is the ZnO resilient coating of 0.1-1 micron;
2) with the step 1) goods at 700-800 ℃ of in-situ annealing 10-30 minute, in 400-600 ℃, organic zinc source flow 5-100sccm, purity oxygen flow are 10-200sccm then, air pressure is 0.01-150Torr, and growth thickness is the ZnO epitaxial loayer of 0.5-30 micron on the ZnO resilient coating;
3) at 600-800 ℃, the organic gallium source flow is 5-100sccm, and the flow of pure ammonia is 100-2000sccm, and air pressure is 10-200Torr, and growth thickness is the GaN etch resistant layer of 0.1-1 micron on the ZnO epitaxial loayer;
4) on the compound substrate that above-mentioned sapphire, ZnO resilient coating, ZnO epitaxial loayer and GaN etch resistant layer constitute, growing GaN or AlN resilient coating, non-Doped GaN transition zone, n type GaN epitaxial loayer, GaN/InGaN multiple quantum well light emitting layer successively, p type GaN epitaxial loayer and current-diffusion layer, and on current-diffusion layer, plate p type GaN contact electrode, on n type GaN epitaxial loayer, be listed in GaN/InGaN multiple quantum well light emitting layer plating n type GaN contact electrode;
5) adopt the acid solution chemical corrosion method, Sapphire Substrate, ZnO resilient coating and ZnO epitaxial loayer and GaN etch resistant layer are peeled off, obtain the GaN based light-emitting diode of self-supporting.
The used acid solution of above-mentioned acid solution chemical corrosion is nitric acid, phosphoric acid or the hydrofluoric acid of pH 〉=4.
Beneficial effect of the present invention is: it is that transition zone is made the GaN based light-emitting diode with the ZnO monocrystal thin films that the present invention has designed a kind of, by obtaining the GaN based light-emitting diode of self-supporting at the bottom of the peeling liner, can significantly improve heat radiation, obtain high-power, high brightness light-emitting devices, sapphire sheet can reclaim repeated use simultaneously.The present invention is good to existing production technology compatibility, not only can significantly improve the performance of device, and help reducing production costs.
Description of drawings
Fig. 1 is present common preparation GaN based light-emitting diode structural representation;
Fig. 2 is a GaN based light-emitting diode structural representation of the present invention;
Fig. 3 is each layer schematic diagram in the GaN based light-emitting diode preparation process of the present invention.
Embodiment
Be described in detail the present invention below in conjunction with drawings and Examples.
Self-supporting GaN based light-emitting diode of the present invention as shown in Figure 2, GaN or AlN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 are arranged on GaN etch resistant layer 104 from bottom to top successively, p type GaN epitaxial loayer 206 and current-diffusion layer 207, and on current-diffusion layer 207 plating p type GaN contact electrode 208, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209 on n type GaN epitaxial loayer 204, its preparation process is referring to Fig. 3.
Embodiment 1.
1) will be through the polishing Sapphire Substrate 101 of the cleaning metal organic chemical vapor deposition device reaction chamber of packing into, vacuumize, at 250 ℃, diethyl zinc (purity 〉=99.9999%) flow 5sccm, oxygen (purity 〉=99.999%) flow is 10sccm, air pressure is 0.01Torr, and growth thickness is 0.1 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 700 ℃ of in-situ annealing 30 minutes, then at 400 ℃, diethyl zinc (purity 〉=99.9999%) flow 5sccm, oxygen (purity 〉=99.999%) flow is 10sccm, air pressure is 0.01Torr, and growth thickness is 0.5 micron a ZnO epitaxial loayer 103;
3) at 600 ℃, trimethyl gallium (purity 〉=99.9999%) flow is 5sccm, and the flow of ammonia (purity 〉=99.9997%) is 100sccm, and air pressure is 10Torr, and growth thickness is 0.01 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing GaN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively, p type GaN epitaxial loayer 206 and current-diffusion layer 207, and on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH 〉=4 salpeter solutions, its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104, corroded above-mentioned device 5 minutes, sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtain the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains by above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Embodiment 2.
1) will be through the polishing Sapphire Substrate 101 of the cleaning metal organic chemical vapor deposition device reaction chamber of packing into, vacuumize, at 350 ℃, diethyl zinc (purity 〉=99.9999%) flow 50sccm, oxygen (purity 〉=99.999%) flow is 100sccm, air pressure is 75Torr, and growth thickness is 0.5 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 800 ℃ of in-situ annealing 20 minutes, then at 500 ℃, diethyl zinc (purity 〉=99.9999%) flow 50sccm, oxygen (purity 〉=99.999%) flow is 100sccm, air pressure is 50Torr, and growth thickness is 10 microns a ZnO epitaxial loayer 103;
3) at 700 ℃, trimethyl gallium (purity 〉=99.9999%) flow is 50sccm, and the flow of ammonia (purity 〉=99.9997%) is 1000sccm, and air pressure is 100Torr, and growth thickness is 0.5 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing GaN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively, p type GaN epitaxial loayer 206 and current-diffusion layer 207, and on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH 〉=4 hydrofluoric acid solutions, its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104, corroded above-mentioned device 10 minutes, sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtain the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains by above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Embodiment 3
1) will be through the polishing Sapphire Substrate 101 of the cleaning metal organic chemical vapor deposition device reaction chamber of packing into, vacuumize, at 400 ℃, diethyl zinc (purity 〉=99.9999%) flow 100sccm, oxygen (purity 〉=99.999%) flow is 200sccm, air pressure is 150Torr, and growth thickness is 1 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 800 ℃ of in-situ annealing 30 minutes, then at 600 ℃, diethyl zinc (purity 〉=99.9999%) flow 100sccm, oxygen (purity 〉=99.999%) flow is 200sccm, air pressure is 150Torr, and growth thickness is 30 microns a ZnO epitaxial loayer 103;
3) at 800 ℃, trimethyl gallium (purity 〉=99.9999%) flow is 100sccm, and the flow of ammonia (purity 〉=99.9997%) is 2000sccm, and air pressure is 200Torr, and growth thickness is 1 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing AIN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively, p type GaN epitaxial loayer 206 and current-diffusion layer 207, and on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH 〉=4 phosphoric acid solutions, its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104, corroded above-mentioned device 5 minutes, sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtain the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains by above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Claims (2)
1. the preparation method of the GaN based light-emitting diode of a self-supporting, the GaN based light-emitting diode of this self-supporting has GaN or AlN resilient coating (202) from bottom to top successively on GaN etch resistant layer (104), non-Doped GaN transition zone (203), n type GaN epitaxial loayer (204), GaN/InGaN multiple quantum well light emitting layer (205), p type GaN epitaxial loayer (206) and current-diffusion layer (207), and at the last plating of current-diffusion layer (207) p type GaN contact electrode (208), on n type GaN epitaxial loayer (204), be listed in GaN/InGaN multiple quantum well light emitting layer (205) plating n type GaN contact electrode (209), what its preparation was adopted is Metalorganic Chemical Vapor Deposition, and step is as follows:
1) will be through the Sapphire Substrate (101) of the cleaning metal organic chemical vapor deposition device reaction chamber of packing into, vacuumize, at 250-400 ℃, organic zinc source flow 5-100sccm, the purity oxygen flow is 10-200sccm, air pressure is 0.01-150Torr, and growth thickness is the ZnO resilient coating (102) of 0.1-1 micron;
2) with the step 1) goods at 700-800 ℃ of in-situ annealing 10-30 minute, then in 400-600 ℃, organic zinc source flow 5-100sccm, the purity oxygen flow is 10-200sccm, air pressure is 0.01-150Torr, and going up growth thickness at ZnO resilient coating (102) is the ZnO epitaxial loayer (103) of 0.5-30 micron;
3) at 600-800 ℃, the organic gallium source flow is 5-100sccm, and the flow of pure ammonia is 100-2000sccm, and air pressure is 10-200Torr, and going up growth thickness at ZnO epitaxial loayer (103) is the GaN etch resistant layer (104) of 0.1-1 micron;
4) in above-mentioned sapphire (101), ZnO resilient coating (102), on the compound substrate that ZnO epitaxial loayer (103) and GaN etch resistant layer (104) constitute, growing GaN or AlN resilient coating (202) successively, non-Doped GaN transition zone (203), n type GaN epitaxial loayer (204), GaN/InGaN multiple quantum well light emitting layer (205), p type GaN epitaxial loayer (206) and current-diffusion layer (207), and, on n type GaN epitaxial loayer (204), be listed in GaN/InGaN multiple quantum well light emitting layer (205) plating n type GaN contact electrode (209) at the last plating of current-diffusion layer (207) p type GaN contact electrode (208);
5) adopt the acid solution chemical corrosion method, Sapphire Substrate (101), ZnO resilient coating (102) and ZnO epitaxial loayer (103) and GaN etch resistant layer (104) are peeled off the GaN based light-emitting diode of self-supporting.
2. the preparation method of the GaN based light-emitting diode of self-supporting according to claim 1 is characterized in that the used acid solution of acid solution chemical corrosion is nitric acid, phosphoric acid or the hydrofluoric acid of pH 〉=4.
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| CN102214749A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Light emitting diode having vertical structure, and method for peeling off thin film from substrate |
| CN102214748A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Epitaxial structure of LED (light-emitting diode) with GaN (gallium nitride)-based vertical structure and manufacturing method thereof |
| CN102867892A (en) * | 2012-09-06 | 2013-01-09 | 合肥彩虹蓝光科技有限公司 | In-doped low-temperature growth P type GaN epitaxial method |
| CN103022288A (en) * | 2011-09-27 | 2013-04-03 | 比亚迪股份有限公司 | Light emitting diode and manufacturing method thereof |
| CN103296159A (en) * | 2013-05-31 | 2013-09-11 | 华南理工大学 | InGaN/GaN multiple quantum well growing on La0.3Sr1.7AlTaO6 substrate and manufacturing method of InGaN/GaN multiple quantum well |
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| CN102214749A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Light emitting diode having vertical structure, and method for peeling off thin film from substrate |
| CN102214748A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Epitaxial structure of LED (light-emitting diode) with GaN (gallium nitride)-based vertical structure and manufacturing method thereof |
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| CN103296159A (en) * | 2013-05-31 | 2013-09-11 | 华南理工大学 | InGaN/GaN multiple quantum well growing on La0.3Sr1.7AlTaO6 substrate and manufacturing method of InGaN/GaN multiple quantum well |
| CN103296159B (en) * | 2013-05-31 | 2015-09-16 | 华南理工大学 | Grow the InGaN/GaN Multiple Quantum Well on strontium aluminate tantalum lanthanum substrate and preparation method |
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| CN106601881A (en) * | 2017-02-21 | 2017-04-26 | 南京大学 | ZnO conductive covariant substrate vertical structure type GaN UV LED |
| CN109216493A (en) * | 2018-08-09 | 2019-01-15 | 镇江镓芯光电科技有限公司 | A kind of p-i-n structure ultraviolet detector and preparation method thereof based on GaN material |
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