CN102867892A - In-doped low-temperature growth P type GaN epitaxial method - Google Patents

In-doped low-temperature growth P type GaN epitaxial method Download PDF

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CN102867892A
CN102867892A CN2012103267871A CN201210326787A CN102867892A CN 102867892 A CN102867892 A CN 102867892A CN 2012103267871 A CN2012103267871 A CN 2012103267871A CN 201210326787 A CN201210326787 A CN 201210326787A CN 102867892 A CN102867892 A CN 102867892A
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郭丽彬
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Hefei Irico Epilight Technology Co Ltd
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Hefei Irico Epilight Technology Co Ltd
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Abstract

The invention relates to an In-doped low-temperature growth P type GaN epitaxial method. The method comprises the following steps of: annealing a substrate and carrying out nitriding treatment; reducing the temperature to grow a low-temperature GaN buffering layer; rising the temperature of the substrate and carrying out heat annealing treatment on the low-temperature GaN buffering layer in situ; growing a high-temperature GaN buffering layer in an epitaxial manner; then, growing one layer of an N type GaN layer with stable doping concentration; growing a shallow quantum well; growing a multi-quantum well of a light-emitting layer; taking N2 as carrier gas to grow an in-doped P type GaN layer; growing a p type AlGaN layer; growing a p type GaN layer; growing a p contact layer; reducing the temperature of a reaction chamber and annealing; and reducing the temperature to the room temperature. According to the in-doped low-temperature growth P type GaN epitaxial method, the quality of a P type gallium nitride crystal is improved, the doping efficiency is improved, the hole concentration is increased, the piezoelectric efficiency in a multi-quantum well light-emitting region is reduced and the dispersion effect of a P type doping agent is reduced, so that the brightness is improved, the steps are simple, and the operation is convenient.

Description

Has the low-temperature epitaxy P type GaN epitaxy method that In mixes
Technical field
The invention belongs to gallium nitride based technical field of material, be specifically related to the low-temperature epitaxy P type GaN epitaxy method under a kind of In doping condition.
Background technology
In the epitaxial growth method of existing GaN series LED, because the self compensation effect of magnesium addition is apparent in view, the hole concentration of gallium nitride-based material of usually mixing magnesium is not high, only has 10 17-10 18Cm-3; Mobility is less than 10 cm 2/ v.s; Doping efficiency is low, and doping efficiency only has 0.1-1%; The activation efficiency of magnesium is low; Magnesium spreads in the Multiple Quantum Well active area.Above-mentioned phenomenon all produces light-emitting diode and has a strong impact on, and can not finely satisfy requirement on devices, and namely magnesium is difficult to obtain the P type gallium nitride material of high-quality, high hole concentration by separately as P type dopant the time.
Summary of the invention
For the problem that P type gallium nitride layer crystal mass is bad in the GaN based light-emitting diode of prior art making, doping efficiency is low, hole concentration is not high and magnesium causes quantum well radiation efficient to reduce to the diffusion of Multiple Quantum Well active area, the invention provides the low-temperature epitaxy P type GaN epitaxy method under a kind of In doping condition.Utilize the present invention can obtain the P type gallium nitride-based material of high-quality, high hole concentration, and then obtain the GaN series LED of high luminous intensity.
The present invention is achieved through the following technical solutions:
A kind of low-temperature epitaxy P type GaN epitaxy method with In doping comprises following concrete steps:
Step 1 is annealed substrate 1 in hydrogen atmosphere, clean described substrate 1 surface, and temperature is controlled between 1030-1200 ℃, then carries out nitrogen treatment;
Step 2, with drop in temperature between 500-650 ℃, the thick low temperature GaN resilient coating 2 of growth 20-30 nm, growth pressure is controlled between the 300-760 Torr, V/III mol ratio is between 500-3200;
Step 3, after described low temperature GaN resilient coating 2 growths finish, stop to pass into TMGa, underlayer temperature is increased between 900-1200 ℃, described low temperature GaN resilient coating 2 original positions are carried out thermal anneal process, annealing time is between 5-30min, after the annealing, between 1000-1200 ℃, epitaxial growth thickness is the high temperature GaN resilient coating 3 between 0.5-2um with adjustment, growth pressure is between 100-500 Torr, and V/III mol ratio is between 300-3000;
Step 4, after described high temperature GaN resilient coating 3 growths finish, the stable N-type GaN layer 4 of growth one deck doping content, thickness is at 1.2-4.2um, growth temperature is between 1000-1200 ℃, and pressure is between 100-600 Torr, and V/III mol ratio is between 300-3000;
Step 5, after described N-type GaN layer 4 growth finished, the shallow quantum well 5 of growing, growth temperature were between 700-900 ℃, and growth pressure is between 100-600 Torr, and V/III mol ratio is between 300-5000, and described shallow quantum well 5 is by the In in 2-10 cycle xGa 1-XN (0.04＜x＜0.4)/GaN Multiple Quantum Well forms, and the thickness of described shallow quantum well 5 is between 2-5nm;
Step 6, after described shallow quantum well 5 growths finish, light-emitting layer grows Multiple Quantum Well 6, growth temperature is between 720-820 ℃, pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000, and described luminescent layer Multiple Quantum Well 6 is by the In in 3-15 cycle yGa 1-yN (x＜y＜1)/GaN Multiple Quantum Well forms, and the thickness of described luminescent layer Multiple Quantum Well 6 is between 2-5nm; The molar constituent content of In remains unchanged between 10%-50% in the described luminescent layer Multiple Quantum Well 6; Barrier layer thickness is constant, and thickness is between 10-15nm, and growth temperature is between 820-920 ℃, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 7 is after described luminescent layer Multiple Quantum Well 6 growths finish, with N 2As the In doping p type GaN layer 7 between the carrier gas growth thickness 10-100nm, growth temperature is between 620-820 ℃, and growth time is between 5-35min, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 8, after described p type GaN layer 7 growth finish, the p type AlGaN layer 8 between the growth thickness 10-50nm, growth temperature is between 900-1100 ℃, growth time is between 5-15min, and pressure is between 50-500 Torr, and V/III mol ratio is between 1000-20000;
Step 9, after described p type AlGaN layer 8 growth finish, the p type GaN layer 9 between the growth thickness 100-800nm, growth temperature is between 850-950 ℃, growth time is between 5-30min, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 10, after described P type GaN layer 9 growth finish, the p contact layer 10 between the growth thickness 5-20nm, growth temperature is between 850-1050 ℃, growth time is between 1-10min, and pressure is between 100-500 Torr, and V/III mol ratio is between 1000-20000;
Step 11 is down to the temperature of reative cell between 650-800 ℃, adopts the pure nitrogen gas atmosphere to carry out annealing in process 2～15min, then is down to room temperature, and get final product.
Preferably, in described step 1, described backing material is sapphire, GaN monocrystalline, monocrystalline silicon or single-crystal silicon carbide, to be fit to GaN and semiconductor epitaxial Material growth thereof.
Preferably, in described step 7, the molar constituent content of the In of described In doping p type GaN layer 7 is 5%-30%.
Preferably, in described step 8, the molar constituent content of the Al of described p type AlGaN layer 8 is controlled between the 10%-30%.
Compare with the epitaxial growth method of existing GaN series LED, the Main Differences of the low-temperature epitaxy P type GaN epitaxy method that the In of having provided by the invention mixes is: growth has the P type gallium nitride layer that In mixes between InGaN/GaN multiple quantum well light emitting layer and P type AlGaN, and the growth temperature of this layer temperature in whole P layer is minimum; Connect lower rising temperature growing P-type AlGaN layer, the unnecessary In of P type gallium nitride layer that this P type of growing AlGaN layer can mix the In of before growth again separates out.In mixes, and can improve the doping content of Mg, reduces the activation energy of Mg, thereby improves hole concentration; Low-temperature epitaxy P type GaN can reduce Mg and spread in InGaN/GaN Multiple Quantum Well active area, reduces the injury to mqw light emitting layer, obtains the GaN series LED of high luminous intensity.As from the foregoing, the present invention has improved P type gallium nitride quality, has improved doping efficiency, increase hole concentration, reduced the piezoelectric effect in the multiple quantum well light emitting district, reduced the diffusion of P type dopant, thereby improved brightness, and step is simple, easy to operate.
Description of drawings
Fig. 1 is the structural representation that utilizes the LED epitaxial structure that the present invention prepares.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit in any form the present invention.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiments of the invention utilize Vecco MOCVD System Implementation.
LED epitaxial structure as shown in Figure 1, order from bottom to top comprises successively: Sapphire Substrate 1, low temperature GaN resilient coating 2, high temperature GaN resilient coating 3, N-type GaN layer 4, shallow quantum well 5, luminescent layer Multiple Quantum Well 6, p type GaN layer 7, p type AlGaN layer 8, p type GaN layer 9, p type contact layer 10.Its preparation method is as follows:
A kind of low-temperature epitaxy P type GaN epitaxy method with In doping comprises following concrete steps:
Step 1 is annealed substrate 1 in hydrogen atmosphere, clean described substrate 1 surface, and temperature is controlled at 1030-
Between 1200 ℃, then carry out nitrogen treatment, substrate is the material that is fit to GaN and semiconductor epitaxial Material growth thereof, such as sapphire, and GaN monocrystalline, monocrystalline silicon, single-crystal silicon carbide etc.;
Step 2, with drop in temperature between 500-650 ℃, the thick low temperature GaN resilient coating 2 of growth 20-30 nm, growth pressure is controlled between the 300-760 Torr, V/III mol ratio is between 500-3200;
Step 3, after described low temperature GaN resilient coating 2 growths finish, stop to pass into TMGa, underlayer temperature is increased between 900-1200 ℃, and described low temperature GaN resilient coating 2 original positions are carried out thermal anneal process, annealing time is between 5-30min, after the annealing, between 1000-1200 ℃, epitaxial growth thickness is the high temperature GaN resilient coating 3 between 0.5-2um with adjustment, growth pressure is between 100-500 Torr, and V/III mol ratio is between 300-3000;
Step 4, after described high temperature GaN resilient coating 3 growths finish, the stable N-type GaN layer 4 of growth one deck doping content, thickness is at 1.2-4.2um, growth temperature is between 1000-1200 ℃, and pressure is between 100-600 Torr, and V/III mol ratio is between 300-3000;
Step 5, after described N-type GaN layer 4 growth finished, the shallow quantum well 5 of growing, growth temperature were between 700-900 ℃, and growth pressure is between 100-600 Torr, and V/III mol ratio is between 300-5000, and described shallow quantum well 5 is by the In in 2-10 cycle xGa 1-XN (0.04＜x＜0.4)/GaN Multiple Quantum Well forms, and the thickness of described shallow quantum well 5 is between 2-5nm;
Step 6, after described shallow quantum well 5 growths finish, light-emitting layer grows Multiple Quantum Well 6, growth temperature is between 720-820 ℃, pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000, and described luminescent layer Multiple Quantum Well 6 is by the In in 3-15 cycle yGa 1-yN (x＜y＜1)/GaN Multiple Quantum Well forms, and the thickness of described luminescent layer Multiple Quantum Well 6 is between 2-5nm; The molar constituent content of In is constant in the described luminescent layer Multiple Quantum Well 6, between 10%-50%; Barrier layer thickness is constant, and thickness is between 10-15nm, and growth temperature is between 820-920 ℃, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 7 is after described luminescent layer Multiple Quantum Well 6 growths finish, with N 2As the In doping p type GaN layer 7 between the carrier gas growth thickness 10-100nm, growth temperature is between 620-820 ℃, growth time is between 5-35min, pressure is between 100-500 Torr, V/III mol ratio is between 300-5000, and the molar constituent content of the In of In doping p type GaN layer 7 is 5%-30%;
Step 8, after described p type GaN layer 7 growth finish, p type AlGaN layer 8 between the growth thickness 10-50nm, growth temperature is between 900-1100 ℃, growth time is between 5-15min, pressure is between 50-500 Torr, and V/III mol ratio is between 1000-20000, and the molar constituent content of the Al of p type AlGaN layer 8 is controlled between the 10%-30%;
Step 9, after described p type AlGaN layer 8 growth finish, the p type GaN layer 9 between the growth thickness 100-800nm, growth temperature is between 850-950 ℃, growth time is between 5-30min, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 10, after described P type GaN layer 9 growth finish, the p contact layer 10 between the growth thickness 5-20nm, growth temperature is between 850-1050 ℃, growth time is between 1-10min, and pressure is between 100-500 Torr, and V/III mol ratio is between 1000-20000;
Step 11, epitaxial growth is down to the temperature of reative cell between 650-800 ℃ after finishing, and adopts the pure nitrogen gas atmosphere to carry out annealing in process 2～15min, then is down to room temperature, namely gets LED epitaxial structure as shown in Figure 1.
Epitaxial structure (epitaxial wafer) is made the branch small-size chips through subsequent machining technologies such as cleaning, deposition, photoetching and etchings.
Present embodiment with high-purity hydrogen or nitrogen as carrier gas, with trimethyl gallium (TMGa), triethyl-gallium (TEGa), trimethyl aluminium (TMAl), trimethyl indium (TMIn) and ammonia (NH 3) respectively as Ga, Al, In and N source, with silane (SiH 4) and two luxuriant magnesium (Cp 2Mg) respectively as n, p-type dopant.
Present embodiment is grown by mixing and be controlled under the cryogenic conditions at P type GaN layer In, improve doping efficiency, obtained the P type gallium nitride material of high hole concentration, reduced the piezoelectric effect in the multiple quantum well light emitting district, also reduce the diffusion of P type dopant, thereby improve brightness.

Claims (4)

1. one kind has the low-temperature epitaxy P type GaN epitaxy method that In mixes, and it is characterized in that, comprises following concrete steps:
Step 1 is annealed substrate in hydrogen atmosphere, clean described substrate surface, and temperature is controlled at 1030～
Between 1200 ℃, then carry out nitrogen treatment;
Step 2, with drop in temperature between 500-650 ℃, the thick low temperature GaN resilient coating of growth 20-30 nm, growth pressure is controlled between the 300-760 Torr, V/III mol ratio is between 500-3200;
Step 3, after described low temperature GaN buffer growth finishes, stop to pass into TMGa, underlayer temperature is increased between 900-1200 ℃, described low temperature GaN resilient coating original position is carried out thermal anneal process, annealing time is between 5-30min, after the annealing, between 1000-1200 ℃, epitaxial growth thickness is the high temperature GaN resilient coating between 0.5-2 μ m with adjustment, growth pressure is between 100-500 Torr, and V/III mol ratio is between 300-3000;
Step 4, after described high temperature GaN buffer growth finishes, the stable N-type GaN layer of growth one deck doping content, thickness is at 1.2-4.2 um, growth temperature is between 1000-1200 ℃, and pressure is between 100-600 Torr, and V/III mol ratio is between 300-3000;
Step 5, after described N-type GaN layer growth finished, the shallow quantum well of growing, growth temperature were between 700-900 ℃, and growth pressure is between 100-600 Torr, and V/III mol ratio is between 300-5000, and described shallow quantum well is by the In in 2-10 cycle xGa 1-XN (0.04＜x＜0.4)/GaN Multiple Quantum Well forms, and the thickness of described shallow quantum well is between 2-5 nm;
Step 6, after described shallow quantum trap growth finished, light-emitting layer grows Multiple Quantum Well, growth temperature were between 720-820 ℃, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000, and described luminescent layer Multiple Quantum Well is by the In in 3-15 cycle yGa 1-yN (x＜y＜1)/GaN Multiple Quantum Well forms, and the thickness of described luminescent layer Multiple Quantum Well is between 2-5 nm; The molar constituent content of In remains unchanged between 10%-50% in the described luminescent layer Multiple Quantum Well; Barrier layer thickness is constant, and thickness is between 10-15 nm, and growth temperature is between 820-920 ℃, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 7 is after described luminescent layer Multiple Quantum Well growth finishes, with N 2As the In doping p type GaN layer between the carrier gas growth thickness 10-100nm, growth temperature is between 620-820 ℃, and growth time is between 5-35min, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 8, after described p type GaN layer growth finishes, the p type AlGaN layer between the growth thickness 10-50nm, growth temperature is between 900-1100 ℃, growth time is between 5-15min, and pressure is between 50-500 Torr, and V/III mol ratio is between 1000-20000;
Step 9, after described p type AlGaN layer growth finishes, the p type GaN layer between the growth thickness 100-800nm, growth temperature is between 850-950 ℃, growth time is between 5-30min, and pressure is between 100-500 Torr, and V/III mol ratio is between 300-5000;
Step 10, after described P type GaN layer growth finishes, the p contact layer between the growth thickness 5-20nm, growth temperature is between 850-1050 ℃, and growth time is between 1-10min, and pressure is between 100-500 Torr, and V/III mol ratio is between 1000-20000;
Step 11 is down to the temperature of reative cell between 650-800 ℃, adopts the pure nitrogen gas atmosphere to carry out annealing in process 2～15min, then is down to room temperature, and get final product.
2. the low-temperature epitaxy P type GaN epitaxy method with In doping according to claim 1 is characterized in that in described step 1, described backing material is sapphire, GaN monocrystalline, monocrystalline silicon or single-crystal silicon carbide.
3. the low-temperature epitaxy P type GaN epitaxy method with In doping according to claim 1 is characterized in that in described step 7, the molar constituent content of the In of described In doping p type GaN layer is 5%-30%.
4. according to claim 1,2 or 3 describedly have low-temperature epitaxy P type GaN epitaxy methods that In mixes, it is characterized in that in described step 8, the molar constituent content of the Al of described p type AlGaN layer is controlled between the 10%-30%.
CN2012103267871A 2012-09-06 2012-09-06 In-doped low-temperature growth P type GaN epitaxial method Pending CN102867892A (en)

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CN103208571A (en) * 2013-04-08 2013-07-17 合肥彩虹蓝光科技有限公司 GaN-based LED (light emitting diode) epitaxial wafer and production method thereof
CN103700745A (en) * 2014-01-03 2014-04-02 合肥彩虹蓝光科技有限公司 High-brightness GaN-based light emitting diode epitaxial growth method
CN103824913A (en) * 2014-03-12 2014-05-28 合肥彩虹蓝光科技有限公司 Epitaxial growth method of Mg-doped P-type GaN
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CN110246753A (en) * 2019-06-20 2019-09-17 江苏能华微电子科技发展有限公司 A kind of preparation method and structure of the epitaxial structure promoting p-type GaN doping concentration

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CN104157761A (en) * 2014-08-30 2014-11-19 太原理工大学 GaN-based light-emitting diode structure improving light extraction rate and preparation method
CN110246753A (en) * 2019-06-20 2019-09-17 江苏能华微电子科技发展有限公司 A kind of preparation method and structure of the epitaxial structure promoting p-type GaN doping concentration
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Application publication date: 20130109