CN109378371B - LED epitaxial wafer growth method - Google Patents
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Abstract
The application discloses a method for growing an LED epitaxial wafer, which comprises the steps of processing a sapphire substrate with an AlN thin film on the surface, sequentially growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third gradient AlGaN layer on the sapphire substrate, growing a low-temperature buffer layer, growing an undoped GaN layer, growing an Si-doped N-type GaN layer, periodically growing an active layer MQW, growing a P-type AlGaN layer, growing a Mg-doped P-type GaN layer, and cooling. The first gradient AlGaN layer, the second gradient AlGaN layer and the third gradient AlGaN layer grow in sequence, so that the dislocation density is reduced, the warping of the epitaxial wafer is reduced, and the qualification rate of the GaN epitaxial wafer, the LED luminous efficiency and the antistatic capacity are improved. And the gradient AlGaN layer is annealed, so that the surface of the whole epitaxial layer is smoother, the surface hexagonal defects and concave pits are fewer, and the whole appearance is better.
Description
Technical Field
The invention relates to the technical field of LED epitaxial wafer growth, in particular to a method for growing an LED epitaxial wafer.
Background
The currently widely used GaN growth method is patterning on a sapphire substrate. The sapphire crystal is one of the best substrate materials for growing the third generation semiconductor material GaN epitaxial layer, and the single crystal preparation process is mature. GaN is a substrate for manufacturing the blue LED. The substrate material SiC of the GaN epitaxial layer has small lattice mismatch with GaN, and is only 3.4%, but the difference between the thermal expansion coefficient of the substrate material SiC and the GaN is large, so that the GaN epitaxial layer is easy to break, and the manufacturing cost is high and is 10 times of that of sapphire; the substrate material Si has low cost, the lattice mismatch degree with GaN is large and reaches 17 percent, the GaN is difficult to grow, and the luminous efficiency is too low compared with sapphire; the sapphire crystal structure of the substrate material is the same (the wurtzite crystal structure with hexagonal symmetry) and the lattice mismatch degree with GaN is 13 percent, so that the high dislocation density of a GaN epitaxial layer is easily caused, and therefore, AlN or a low-temperature GaN epitaxial layer or a SiO2 layer and the like are added on the sapphire substrate, and the dislocation density of the GaN epitaxial layer can be reduced.
The large lattice mismatch (13-16%) and thermal mismatch between sapphire and GaN lead to a high (10-10%) misfit dislocation density in the GaN epitaxial layer10cm-2) Affecting the quality of the GaN epitaxial layerAffecting device quality (light emitting efficiency, drain electrode, lifetime, etc.).
The conventional method is to adopt a low-temperature buffer layer, and improve the crystal quality of the GaN epitaxial layer by adjusting the nitridation of the sapphire substrate, the growth temperature of the low-temperature buffer layer, the thickness of the buffer layer and the like. However, since the low temperature buffer layer is also heteroepitaxial, the improved crystal quality is limited. In addition, because of the large lattice mismatch among the epitaxial thin film layers, the epitaxial crystal thin film is always stressed in the growth process, and the epitaxial wafer is bent and warped. When epitaxial crystal growth is carried out on a large-size sapphire substrate by using the traditional low-temperature buffer layer method, the warping of an epitaxial wafer is large, so that the grinding fragment rate is high in the subsequent chip manufacturing process, and the product yield is low.
Disclosure of Invention
In view of the above, the present invention provides a method for growing an LED epitaxial wafer, comprising the steps of:
processing a sapphire substrate with an AlN thin film on the surface;
sequentially growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third AlGaN layer on the sapphire substrate, wherein,
the growing a first graded AlGaN layer comprises: controlling the pressure of the reaction cavity with the pressure of 400-600mbar, and introducing NH with the flow rate of 60-70L/min into the reaction cavity390-95L/min N2100-110sccm TMGa and 230-250sccm TMAl source, gradually reducing the growth temperature from 550 ℃ to 500 ℃ by reducing the temperature by 0.1 ℃ per second in the growth process, and growing a first gradient AlGaN layer with the thickness D1 of 8-10nm on the sapphire substrate, wherein the molar composition of Al is 10-12%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow constant, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradient AlGaN layer with the thickness of D2 being 8-10nm on the first gradient AlGaN layer, wherein the molar composition of Al is 10-12%, and D2 is D1;
the growing a third AlGaN layer includes: increasing the pressure of the reaction cavity to 850-;
keeping the pressure of the reaction cavity between 850 and 900mbar, and controlling N2The flow rate is 150-;
growing a low-temperature buffer layer;
growing an undoped GaN layer;
growing an N-type GaN layer doped with Si;
periodically growing an active layer MQW;
growing a P-type AlGaN layer;
growing a P-type GaN layer doped with Mg;
and cooling.
Preferably, the sapphire substrate with the AlN thin film on the surface is treated at high temperature for 5-10 minutes at the temperature of 1000-1200 ℃ and under the condition that the pressure of the reaction cavity is maintained at 100-150mbar hydrogen atmosphere.
Preferably, the growth of the low temperature buffer layer is further performed by cooling to 550-3TMGa 50-100sccm, H100-130L/min2And growing a low-temperature buffer layer with the thickness of 20-50nm on the third AlGaN layer.
Preferably, the undoped GaN layer is grown, further, the temperature is raised to 1000-3200-400sccm TMGa, 100-130L/min H2And continuously growing an undoped GaN layer of 2-4 mu m on the low-temperature buffer layer.
Preferably, the Si-doped N-type GaN layer is grown by further keeping the pressure of the reaction chamber at 150-3200-300sccm TMGa, 50-90L/min H2And 20-50sccm SiH4Continuously growing a 2-4 μm Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 5E +18-1E +19atoms/cm3。
Preferably, the periodically grown active layer MQW, further,
the pressure of the reaction chamber is maintained at 300-400mbar, the low temperature is 700-750 ℃, NH of 50000-60000sccm is introduced3100-150sccm TEGa and TMIn, the flow rate of TMIn is gradually increased from 150-170sccm to 1500-1700sccm by increasing 25-52sccm per second, and 30-50s of In are growny1Ga(1-y1)N with a growth thickness of D4, and In doping concentration increased by 4E +17-7E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
The growth condition is maintained unchanged, the flow rate of the stable TMIn is 1500-1700sccm, and 100-150s of In is growny2Ga(1-y2)N, the growth thickness is D5, the In doping concentration is 1E +20-3E +20atoms/cm3D4+ D5 in the range of 3-3.5nm, y1 and y2 in the range of 0.015-0.25, wherein y1 and y2 are not equal;
raising the temperature to 800-y1Ga(1-y1)N/Iny2Ga(1-y2)The number of N/GaN cycles is 10-15.
Preferably, the growth of the P-type AlGaN layer is further carried out by raising the temperature to 900-3Mg doping concentration of 5E +18-1E +19atoms/cm3。
Preferably, the growth of the Mg-doped P-type GaN layer is further carried out by raising the temperature to 930-3。
Preferably, the temperature is reduced to 800 ℃ for 20-30min, and then the furnace is cooled.
Compared with the prior art, the LED epitaxial wafer growth method provided by the invention has the following beneficial effects:
firstly, a first gradient AlGaN layer with slightly low crystallization quality is grown on a sapphire substrate of an AlN thin film, so that the first gradient AlGaN layer can be better matched with the substrate, the lattice mismatch degree is smaller, epitaxial atoms can be uniformly filled upwards, and the uniformity in a chip is improved.
And secondly, growing a second gradient AlGaN layer with high crystallization quality on the first gradient AlGaN layer, wherein the epitaxial layer atoms can release sheet internal stress, block upward extension of the defects generated by lattice mismatch in the early stage, and block upward extension of the defects when the defects are directly pushed upward in parallel when the growth is continued, so that the dislocation density is reduced, and the crystal quality is improved.
And thirdly, a low-temperature high-pressure third AlGaN layer grows on the second gradient AlGaN layer, so that the doping efficiency of Al is improved, the crystallization quality of the layer is improved, the stress accumulation effect of the sapphire substrate on the GaN film is favorably eliminated, and the stress control window of the epitaxial film material is remarkably increased, so that the warping of the epitaxial wafer can be reduced, the qualification rate of the GaN epitaxial wafer is favorably improved, and the luminous efficiency and the antistatic capacity of the LED are improved.
Fourthly, the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are subjected to short annealing treatment for 20s, so that lattices of the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are subjected to new regular arrangement under the thermal action, a neat surface is obtained, the growth of a low-temperature buffer layer on the next step is facilitated, the surface of the whole epitaxial layer is more smooth, the surface hexagonal defects and concave pits are fewer, and the whole appearance is better.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flowchart of a method for growing an LED epitaxial wafer in embodiment 1 of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It should be noted that the described embodiments are merely some embodiments, rather than all embodiments, of the invention and are merely illustrative in nature and in no way intended to limit the invention, its application, or uses. The protection scope of the present application shall be subject to the definitions of the appended claims.
Example 1:
referring to fig. 1, a specific embodiment of a method for growing an LED epitaxial wafer according to the present application is shown, the method including:
and 101, processing the sapphire substrate with the AlN thin film on the surface, specifically, processing the sapphire substrate with the AlN thin film on the surface at a high temperature for 5 minutes at 1000 ℃ under the condition that the pressure of a reaction cavity is maintained at 100mbar in hydrogen atmosphere.
Step 102, growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third gradient AlGaN layer on the sapphire substrate in sequence:
the growing a first graded AlGaN layer comprises: controlling the pressure of a reaction cavity at 400mbar, and introducing NH with the flow rate of 60L/min into the reaction cavity390L/min N2TMGa of 100sccm and TMAl source of 230sccm, wherein the growth temperature is gradually reduced from 550 ℃ to 500 ℃ by reducing 0.1 ℃ per second in the growth process, and a first gradually-changed AlGaN layer with the thickness D1 of 8nm is grown on the sapphire substrate, wherein the molar component of Al is 10%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow unchanged, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradient AlGaN layer with the thickness D2 of 8nm on the first gradient AlGaN layer, wherein the molar component of Al is 10%;
the growing a third AlGaN layer includes: the growing a third AlGaN layer includes: increasing the pressure of a reaction cavity to 850mbar, reducing the growth temperature from 800 ℃ to 480 ℃, keeping the flow of gas introduced unchanged, maintaining the pressure of the reaction cavity to be 850mbar and the growth temperature to be 480 ℃ in the growth process, and growing a third AlGaN layer with the thickness D3 of 8nm on the second gradient AlGaN layer, wherein the molar component of Al is 10%;
maintaining the pressure in the reaction chamber at 850mbar and controlling N2And controlling the flow rate to be 150L/min and the temperature of the reaction chamber to be 680 ℃, and carrying out 20s of annealing treatment on the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer.
Step 103, growing a low-temperature buffer layer: cooling to 550 deg.C, maintaining the pressure in the reaction chamber at 400mbar, and introducing NH with a flow rate of 10000sccm3TMGa of 50sccm, H of 100L/min2And growing a low-temperature buffer layer with the thickness of 20nm on the third AlGaN layer.
Step 104, growing an undoped GaN layer: the temperature is raised to 1000 ℃, the pressure of the reaction cavity is maintained at 150mbar, and NH with the flow rate of 30000sccm is introduced3TMGa of 200sccm, H of 100L/min2And continuously growing an undoped GaN layer of 2 mu m on the low-temperature buffer layer.
Step 105, growing an N-type GaN layer doped with Si: keeping the pressure of the reaction cavity at 150mbar, keeping the temperature at 1000 ℃, and introducing NH with the flow rate of 40L/min3TMGa of 200sccm, H of 50L/min2And 20sccm of SiH4Continuously growing a 2 μm Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 5E +18atoms/cm3。
Step 106, periodically growing an active layer MQW:
the pressure of the reaction cavity is maintained at 300mbar, the temperature is 700 ℃, and NH of 50000sccm is introduced3TEGa of 100sccm, and TMIn, the flow rate of TMIn is gradually increased from 150sccm to 1500sccm at an increase of 45sccm per second, and In is grown for 30s0.015Ga0.985N, growth thickness of 1nm, In doping concentration increased by 6.7E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
Maintaining the growth condition unchanged, stabilizing the flow of TMIn to 1500sccm, and growing 100s of In0.25Ga0.75N with a growth thickness of 2nm and an In doping concentration of 1E +20atoms/cm3；
Raising the temperature to 800 ℃, maintaining the pressure at 300mbar, introducing 50000sccm NH3 and 400sccm TEGa, and growing a 10nm GaN layer In0.015Ga0.985N/In0.25Ga0.75The number of N/GaN cycles was 10.
Step 107, growing a P-type AlGaN layer: raising the temperature to 900 ℃, maintaining the pressure of a reaction cavity at 200mbar, continuously growing a 20nm P-type AlGaN layer on the MQW of the active layer, wherein the doping concentration of Al is 1E +20atoms/cm3The Mg doping concentration is 5E +18atoms/cm3。
Step 108, growing a P-type GaN layer doped with Mg: raising the temperature to 930 ℃, maintaining the pressure of the reaction cavity at 200mbar, and continuously growing a 100nm magnesium-doped P-type GaN layer on the P-type AlGaN layer, wherein the Mg doping concentration is 1E +19atoms/cm3。
Step 109, cooling: cooling to 700 deg.C, maintaining the temperature for 20min, and cooling in furnace.
Example 2:
the embodiment provides a method for growing an LED epitaxial wafer, which comprises the following steps:
step 201, processing the sapphire substrate with the AlN thin film on the surface, specifically, processing the sapphire substrate with the AlN thin film on the surface at high temperature for 10 minutes at 1200 ℃ under the condition that the pressure of a reaction cavity is maintained at 150mbar hydrogen atmosphere.
Step 202, growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third gradient AlGaN layer on the sapphire substrate in sequence:
the growing a first graded AlGaN layer comprises: controlling the pressure of a reaction cavity at 600mbar, and introducing NH with the flow rate of 70L/min into the reaction cavity395L/min N2TMGa of 110sccm and TMAl source of 250sccm, wherein the growth temperature is gradually reduced from 550 ℃ to 500 ℃ by reducing 0.1 ℃ per second in the growth process, and a first gradually-changed AlGaN layer with the thickness D1 of 10nm is grown on the sapphire substrate, wherein the molar component of Al is 12%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow unchanged, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradient AlGaN layer with the thickness D2 of 10nm on the first gradient AlGaN layer, wherein the molar component of Al is 12%;
the growing a third AlGaN layer includes: the growing a third AlGaN layer includes: increasing the pressure of a reaction cavity to 900mbar, reducing the growth temperature from 800 ℃ to 480 ℃, keeping the flow of gas introduced unchanged, maintaining the pressure of the reaction cavity at 900mbar and the growth temperature at 480 ℃ in the growth process, and growing a third AlGaN layer with the thickness D3 of 10nm on the second gradient AlGaN layer, wherein the molar component of Al is 12%;
maintaining the pressure in the reaction chamber at 900mbar and controlling N2The flow rate is 160L/min, the temperature of the reaction chamber is controlled to be 720 ℃, and the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are annealed for 20 s.
Step 203, growing a low-temperature buffer layer: cooling to 650 deg.C, maintaining the pressure in the reaction chamber at 600mbar, and introducing NH with a flow rate of 20000sccm3TMGa of 100sccm, H of 130L/min2And growing a low-temperature buffer layer with the thickness of 50nm on the third AlGaN layer.
Step 204, growing an undoped GaN layer: the temperature is raised to 1200 ℃, the pressure of the reaction cavity is maintained at 300mbar, NH with the flow rate of 40000sccm is introduced3TMGa of 400sccm, H of 130L/min2And continuously growing an undoped GaN layer with the thickness of 4 mu m on the low-temperature buffer layer.
Step 205, growing an N-type GaN layer doped with Si: keeping the pressure of the reaction cavity at 300mbar, keeping the temperature at 1100 ℃, and introducing NH with the flow rate of 60L/min3TMGa of 300sccm, H of 90L/min2And 50sccm of SiH4Continuously growing a 4 μm Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 1E +19atoms/cm3。
Step 206, periodically growing an active layer MQW:
the pressure of the reaction cavity is maintained at 400mbar, the temperature is 750 ℃, and NH of 60000sccm is introduced3TEGa of 150sccm, and TMIn, the flow rate of TMIn is gradually increased from 170sccm to 1700sccm by an increase of 30.6sccm per second, and 50s of In is grown0.010Ga0.990N, growth thickness of 1.5nm, In doping concentration increased by 4E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
Maintaining the growth condition unchanged, stabilizing the flow of TMIn at 1700sccm, and growing 150s of In0.2Ga0.8N with a growth thickness of 2nm and an In doping concentration of 3E +20atoms/cm3；
Raising the temperature to 850 ℃, maintaining the pressure at 400mbar, introducing 60000sccm NH3 and 500sccm TEGa, and growing a 10nm GaN layer In0.010Ga0.990N/In0.2Ga0.8The number of N/GaN cycles was 15.
Step 207, growing a P-type AlGaN layer: raising the temperature to 1000 ℃, maintaining the pressure of a reaction cavity at 400mbar, continuously growing a 50nm P-type AlGaN layer on the MQW of the active layer, wherein the doping concentration of Al is 3E +20atoms/cm3The Mg doping concentration is 1E +19atoms/cm3。
Step 208, growing a P-type GaN layer doped with Mg: raising the temperature to 950 ℃, maintaining the pressure of a reaction cavity at 600mbar, and continuously growing a 300nm magnesium-doped P-type GaN layer on the P-type AlGaN layer, wherein the Mg doping concentration is 1E +20atoms/cm3。
Step 209, cooling: cooling to 800 deg.C, maintaining the temperature for 30min, and cooling in furnace.
Example 3
And 301, processing the sapphire substrate with the AlN thin film on the surface, specifically, processing the sapphire substrate with the AlN thin film on the surface at the high temperature of 1100 ℃ and in the atmosphere of hydrogen with the reaction cavity pressure of 125mbar for 7 minutes.
Step 302, growing a first graded AlGaN layer, a second graded AlGaN layer and a third AlGaN layer on the sapphire substrate in sequence:
the growing a first graded AlGaN layer comprises: controlling the pressure of a reaction cavity at 500mbar, and introducing NH with the flow rate of 65L/min into the reaction cavity393L/min N2TMGa of 105sccm and TMAl source of 240sccm, the growth temperature is gradually reduced from 550 ℃ to 500 ℃ at the temperature of 0.1 ℃ per second in the growth process, and the second layer with the thickness D1 of 9nm is grown on the sapphire substrateA gradient AlGaN layer, wherein the molar composition of Al is 11%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow unchanged, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradient AlGaN layer with the thickness D2 of 9nm on the first gradient AlGaN layer, wherein the molar component of Al is 11%;
the growing a third AlGaN layer includes: the growing a third AlGaN layer includes: increasing the pressure of a reaction cavity to 870mbar, reducing the growth temperature from 800 ℃ to 480 ℃, keeping the flow of gas introduced unchanged, maintaining the pressure of the reaction cavity to 870mbar and the growth temperature to 480 ℃ in the growth process, and growing a third AlGaN layer with the thickness D3 of 9nm on the second gradient AlGaN layer, wherein the molar component of Al is 11%;
keeping the pressure of the reaction cavity at 870mbar and controlling N2And controlling the temperature of the reaction chamber to be 700 ℃ at a flow rate of 155L/min, and performing annealing treatment on the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer for 20 s.
Step 303, growing a low-temperature buffer layer: cooling to 600 deg.C, maintaining the pressure in the reaction chamber at 500mbar, and introducing 15000sccm NH3TMGa of 70sccm, H of 115L/min2And growing a low-temperature buffer layer with the thickness of 35nm on the third AlGaN layer.
Step 304, growing an undoped GaN layer: the temperature is raised to 1100 ℃, the pressure of the reaction cavity is maintained at 225mbar, NH with the flow rate of 35000sccm is introduced3TMGa of 300sccm, H of 115L/min2And continuously growing an undoped GaN layer with the thickness of 3 mu m on the low-temperature buffer layer.
Step 305, growing an N-type GaN layer doped with Si: keeping the pressure of the reaction cavity at 225mbar, keeping the temperature at 1050 ℃, and introducing NH with the flow rate of 50L/min3TMGa of 250sccm, H of 70L/min2And 35sccm of SiH4Continuously growing a 3 mu m Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 7E +18atoms/cm3。
Step 306, periodically growing an active layer MQW:
the pressure of the reaction cavity is maintained at 350mbar, the low temperature is 725 ℃, and 55000sccm NH is introduced3TEGa of 125sccm, and TMIn, the flow rate of TMIn is gradually increased from 160sccm to 1600sccm by 36sccm per second, and In is grown for 40s0.1Ga0.9N, growth thickness of 1.15nm, In doping concentration increased by 5E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
Keeping the growth condition unchanged, stabilizing the flow of TMIn to 1600sccm, and growing 125s of In0.15Ga0.85N, growth thickness of 2.1nm, In doping concentration of 2E +20atoms/cm3；
Raising the temperature to 825 deg.C, maintaining the pressure at 350mbar, introducing 55000sccm NH3 and 450sccm TEGa, and growing 10nm GaN layer In0.1Ga0.9N/In0.15Ga0.85The number of N/GaN cycles was 13.
Step 307, growing a P-type AlGaN layer: raising the temperature to 950 ℃, maintaining the pressure of a reaction cavity at 300mbar, continuously growing a 35nm P-type AlGaN layer on the active layer MQW, wherein the doping concentration of Al is 2E +20atoms/cm3The Mg doping concentration is 7.5E +18atoms/cm3。
Step 308, growing a P-type GaN layer doped with Mg: raising the temperature to 940 ℃, maintaining the pressure of a reaction cavity at 400mbar, continuously growing a 200nm magnesium-doped P-type GaN layer on the P-type AlGaN layer, wherein the Mg doping concentration is 5E +19atoms/cm3。
Step 309, cooling: cooling to 750 deg.C, keeping the temperature for 25min, and cooling in furnace.
Example 4
Step 401, processing the sapphire substrate with the AlN thin film on the surface, specifically, processing the sapphire substrate with the AlN thin film on the surface at 1050 ℃ and under the condition that the pressure of the reaction cavity is maintained at 110mbar and hydrogen atmosphere for 6 minutes.
Step 402, growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third gradient AlGaN layer on the sapphire substrate in sequence:
the growing a first graded AlGaN layer comprises: controlling 450mbarThe pressure of the reaction cavity is increased, NH with the flow rate of 63L/min is introduced into the reaction cavity391L/min N2TMGa of 102sccm and TMAl source of 235sccm, wherein the growth temperature is gradually reduced from 550 ℃ to 500 ℃ by reducing 0.1 ℃ per second in the growth process, and a first gradually-changed AlGaN layer with the thickness D1 of 8.5nm is grown on the sapphire substrate, wherein the molar component of Al is 10.5%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow unchanged, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradually-changed AlGaN layer with the thickness D2 of 8.5nm on the first gradually-changed AlGaN layer, wherein the molar composition of Al is 10.5%;
the growing a third AlGaN layer includes: the growing a third AlGaN layer includes: increasing the pressure of a reaction cavity to 860mbar, reducing the growth temperature from 800 ℃ to 480 ℃, keeping the flow of gas introduced unchanged, maintaining the pressure of the reaction cavity to 860mbar and the growth temperature to 480 ℃ in the growth process, and growing a third AlGaN layer with the thickness D3 of 8.5nm on the second gradually-changed AlGaN layer, wherein the molar component of Al is 10.5%;
maintaining the pressure in the reaction cavity at 860mbar, and controlling N2The flow rate is 152L/min, the temperature of the reaction chamber is controlled to be 690 ℃, and the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are annealed for 20 s.
Step 403, growing a low-temperature buffer layer: the temperature is reduced to 560 ℃, the pressure of the reaction cavity is maintained at 450mbar, and 13000sccm NH is introduced3TMGa of 60sccm, H of 110L/min2And growing a low-temperature buffer layer with the thickness of 30nm on the third AlGaN layer.
Step 404, growing an undoped GaN layer: raising the temperature to 1050 ℃, maintaining the pressure of the reaction cavity at 180mbar, and introducing NH with the flow rate of 33000sccm3TMGa of 250sccm, H of 110L/min2And continuously growing an undoped GaN layer of 2.5 mu m on the low-temperature buffer layer.
Step 405, growing a Si-doped N-type GaN layer: keeping the pressure of the reaction cavity at 190mbar and the temperatureNH with a flow rate of 45L/min is introduced at 1010 DEG C3TMGa of 220sccm, H of 60L/min2And 25sccm of SiH4Continuously growing a 2.5 mu m Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 6E +18atoms/cm3。
Step 406, periodically growing an active layer MQW:
the pressure of the reaction chamber is maintained at 330mbar, the temperature is 710 ℃, and NH of 53000sccm is introduced3TEGa at 110sccm, and TMIn at a flow rate of increasing from 155sccm to 1550sccm at an increase of 39.8sccm per second, growing 35s of In0.2Ga0.8N, growth thickness of 1.2nm, In doping concentration increased by 5.7E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
Maintaining the growth condition unchanged, stabilizing the flow of TMIn at 1550sccm, and growing 110s of In0.22Ga0.78N, growth thickness of 2.15nm, In doping concentration of 1.5E +20atoms/cm3；
Increasing the temperature to 810 ℃, maintaining the pressure at 330mbar, introducing 53000sccm NH3 and 430sccm TEGa, and growing a 10nm GaN layer In0.2Ga0.8N/In0.22Ga0.78The number of N/GaN cycles was 11.
Step 407, growing a P-type AlGaN layer: raising the temperature to 930 ℃, maintaining the pressure of a reaction cavity at 250mbar, continuously growing a 25nm P-type AlGaN layer on the MQW of the active layer, wherein the doping concentration of Al is 1.5E +20atoms/cm3The Mg doping concentration is 6E +18atoms/cm3。
Step 408, growing a Mg-doped P-type GaN layer: raising the temperature to 910 ℃, maintaining the pressure of a reaction cavity at 300mbar, and continuously growing a 150nm magnesium-doped P-type GaN layer on the P-type AlGaN layer, wherein the Mg doping concentration is 3E +19atoms/cm3。
Step 409, cooling: cooling to 720 deg.C, maintaining the temperature for 22min, and cooling in furnace.
Comparative experiment:
the LED structure epitaxial growth method based on the traditional process comprises the following specific steps:
1. and (3) processing the sapphire substrate with the AlN film on the surface for 5-10 minutes at the temperature of 1000-1200 ℃ and under the hydrogen atmosphere of 100-150mbar of reaction chamber pressure.
2. Cooling to 550-650 deg.C, maintaining the pressure in the reaction chamber at 400-600mbar, and introducing 10000-20000sccm NH3TMGa 50-100sccm, H100-130L/min2And growing a low-temperature buffer layer GaN with the thickness of 20-50nm on the sapphire substrate.
3. The temperature is raised to 1000-3200-400sccm TMGa, 100-130L/min H2Continuously growing 2-4 mu m undoped GaN;
4. continuously growing Si-doped N-type GaN with the Si doping concentration of 5E +18-1E +19atoms/cm3The total thickness is controlled to be 2-4 μm.
5. The active layer MQW is periodically grown, including the steps,
the pressure of the reaction chamber is maintained at 300-400mbar, the low temperature is 700-750 ℃, NH of 50000-60000sccm is introduced3100-150sccm TEGa and TMIn, the flow rate of the TMIn is gradually increased from 150-170sccm to 1500-1700sccm, and 30-50s of In is growny1Ga(1-y1)N is grown to a thickness of D6, and the In doping concentration is from 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
The growth condition is maintained unchanged, the flow rate of the stable TMIn is 1500-1700sccm, and 100-150s of In is growny2Ga(1-y2)N, the growth thickness is D7, the In doping concentration is 1E +20-3E +20atoms/cm3D6+ D7 in the range of 3-3.5nm, y1 and y2 in the range of 0.015-0.25, wherein y1 and y2 are not equal;
raising the temperature to 800-y1Ga(1-y1)N/Iny2Ga(1-y2)The number of N/GaN cycles is 10-15.
6. Then raising the temperature to 900-3Mg doping concentration of 5E +18-1E +19atoms/cm3。
7. Then raising the temperature to 930-3。
8. Finally, the temperature is reduced to 700 ℃ and 800 ℃, the temperature is preserved for 20-30min, and then the furnace is cooled.
A group of epitaxial wafer samples W1 were grown using the growth method provided by the present invention, and a group of epitaxial wafer samples W2 were grown using the growth method of the conventional process. The epitaxial wafer sample W1 is made into a chip sample C1 with the size of 254 microns multiplied by 686 microns according to the standard process on the production line, and the epitaxial wafer sample W2 is made into a chip sample C2 with the size of 254 microns multiplied by 686 microns according to the standard process on the production line.
The crystal quality of the GaN epitaxial wafer samples was characterized using a high resolution X-ray diffractometer (HRXRD) model D8 Discover, and the photoelectric properties of the chip samples were tested using a semi-integrating sphere full-automatic wafer spot tester model LEDA-8F P7202, as shown in table 1:
TABLE 1 FWHM (full width at half maximum) and dislocation density of XRD rocking curve for sample W1W 2
By analyzing table 1, the following conclusions can be drawn: compared with the sample W2, the threading dislocation density and the edge dislocation density of the sample W1 are both obviously reduced, and the half-height width is smaller, which shows that the method of the invention can effectively improve the crystal quality of the epitaxial thin film. In addition, statistics on the appearance yield of the samples W1 and W2 show that the ratio of the hexagonal defects and the concave pits existing on the surface of the W2 sample is 0.7%, and the ratio of the hexagonal defects and the concave pits existing on the surface of the W1 sample is 0.3%, which shows that the method can obviously improve the appearance condition of the surface of the epitaxial wafer.
The warping BOW value data (um) of the epitaxial wafer samples W1 and W2 are counted, the mean value of the warping degrees of the W1 samples is 5.6um, and the mean value of the warping degrees of the W2 samples is 6.4 um.
In order to clarify the influence of the crystal quality of the GaN epitaxial wafer grown by the method of the present invention and the conventional method on the photoelectric parameters of the LED device, samples W1 and W2 were fabricated as chips, respectively. Specifically, the sample W1 was fabricated into a chip, and a chip sample C1 of 254 μm × 686 μm in size was obtained; preparing a chip from the sample W2 to obtain a chip sample C2 with the size of 254 microns multiplied by 686 microns; the luminous power (LOP) was measured by a point tester at 150mA in the forward direction, the leakage current (IR) was measured at-5V in the reverse direction, the antistatic ability (ESD pass rate) was measured at 2000V and 4000V in the Human Body Mode (HBM), and the average value of all core particle photoelectric parameters was obtained as shown in Table 2:
TABLE 2 test values for the main optoelectronic parameters of chip samples C1 and C2
By analyzing table 2, the following conclusions can be drawn: the chip sample manufactured by the growth method provided by the invention has high luminous power, obvious small electric leakage and high antistatic yield. The main reasons of high luminous power, small electric leakage and strong antistatic capability are that the method of the invention increases the defect blocking and isolating mechanism during the growth of epitaxial crystal, reduces dislocation ascending layer by layer, gradually improves lattice matching, reduces dislocation density, reduces defect proportion and improves crystal quality, thereby improving LED luminous efficiency and antistatic capability.
According to the embodiments, the application has the following beneficial effects:
firstly, a first gradient AlGaN layer with slightly low crystallization quality is grown on a sapphire substrate of an AlN thin film, so that the first gradient AlGaN layer can be better matched with the substrate, the lattice mismatch degree is smaller, epitaxial atoms can be uniformly filled upwards, and the uniformity in a chip is improved.
And secondly, growing a second gradient AlGaN layer with high crystallization quality on the first gradient AlGaN layer, wherein the epitaxial layer atoms can release sheet internal stress, block upward extension of the defects generated by lattice mismatch in the early stage, and block upward extension of the defects when the defects are directly pushed upward in parallel when the growth is continued, so that the dislocation density is reduced, and the crystal quality is improved.
And thirdly, a low-temperature high-pressure third AlGaN layer grows on the second gradient AlGaN layer, so that the doping efficiency of Al is improved, the crystallization quality of the layer is improved, the stress accumulation effect of the sapphire substrate on the GaN film is favorably eliminated, and the stress control window of the epitaxial film material is remarkably increased, so that the warping of the epitaxial wafer can be reduced, the qualification rate of the GaN epitaxial wafer is favorably improved, and the luminous efficiency and the antistatic capacity of the LED are improved.
Fourthly, the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are subjected to short annealing treatment for 20s, so that lattices of the first gradient AlGaN layer, the second gradient AlGaN layer and the third AlGaN layer are subjected to new regular arrangement under the thermal action, a neat surface is obtained, the growth of a low-temperature buffer layer on the next step is facilitated, the surface of the whole epitaxial layer is more smooth, the surface hexagonal defects and concave pits are fewer, and the whole appearance is better.
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (9)
1. A method for growing an LED epitaxial wafer is characterized by comprising the following steps:
processing a sapphire substrate with an AlN thin film on the surface;
sequentially growing a first gradient AlGaN layer, a second gradient AlGaN layer and a third AlGaN layer on the sapphire substrate, wherein,
first gradual change of growthThe AlGaN layer includes: controlling the pressure of the reaction cavity with the pressure of 400-600mbar, and introducing NH with the flow rate of 60-70L/min into the reaction cavity390-95L/min N2100-110sccm TMGa and 230-250sccm TMAl source, gradually reducing the growth temperature from 550 ℃ to 500 ℃ by reducing the temperature by 0.1 ℃ per second in the growth process, and growing a first gradient AlGaN layer with the thickness D1 of 8-10nm on the sapphire substrate, wherein the molar composition of Al is 10-12%;
the growing a second graded AlGaN layer includes: increasing the growth temperature to 700 ℃, keeping the pressure of a reaction cavity and the gas inlet flow constant, gradually increasing the growth temperature from 700 ℃ to 800 ℃ by increasing the temperature by 0.2 ℃ per second in the growth process, and growing a second gradient AlGaN layer with the thickness of D2 being 8-10nm on the first gradient AlGaN layer, wherein the molar composition of Al is 10-12%, D2 is D1, and the crystalline quality of the first gradient AlGaN layer is lower than that of the second gradient AlGaN layer;
the growing a third AlGaN layer includes: increasing the pressure of the reaction cavity to 850-;
keeping the pressure of the reaction cavity between 850 and 900mbar, and controlling N2The flow rate is 150-;
growing a low-temperature buffer layer;
growing an undoped GaN layer;
growing an N-type GaN layer doped with Si;
periodically growing an active layer MQW;
growing a P-type AlGaN layer;
growing a P-type GaN layer doped with Mg;
and cooling.
2. The method for growing the LED epitaxial wafer according to claim 1, wherein the sapphire substrate with the AlN thin film on the surface is processed at a high temperature for 5-10 minutes at 1000-1200 ℃ and under a hydrogen atmosphere with a reaction chamber pressure of 100-150 mbar.
3. The method as claimed in claim 1, wherein the growth of the low temperature buffer layer is further characterized by cooling to 550-650 ℃, maintaining the pressure in the reaction chamber at 400-600mbar, and introducing a flow of 10000-20000sccmnH3TMGa 50-100sccm, H100-130L/min2And growing a low-temperature buffer layer with the thickness of 20-50nm on the third AlGaN layer.
4. The method as claimed in claim 1, wherein the growing of the undoped GaN layer is further performed by raising the temperature to 1000-3200-400sccm TMGa, 100-130L/min H2And continuously growing an undoped GaN layer of 2-4 mu m on the low-temperature buffer layer.
5. The method as claimed in claim 1, wherein the Si-doped N-type GaN layer is grown by maintaining the pressure in the reaction chamber at 150-3200-300sccm TMGa, 50-90L/min H2And 20-50sccm SiH4Continuously growing a 2-4 μm Si-doped N-type GaN layer on the undoped GaN layer, wherein the doping concentration of Si is 5E +18-1E +19atoms/cm3。
6. The LED epitaxial wafer growth method according to claim 1, wherein the active layer MQW is periodically grown, further,
the pressure of the reaction chamber is maintained at 300-400mbar, the low temperature is 700-750 ℃, NH of 50000-60000sccm is introduced3100-150sccm TEGa and TMIn, the flow rate of TMIn is gradually increased from 150-170sccm to 1500-1700sccm by increasing 25-52sccm per second, and 30-50s of In are growny1Ga(1-y1)N with a growth thickness of D4, and In doping concentration increased by 4E +17-7E +17atoms/cm per second3From 1E +19atoms/cm3Gradually changed into 3E +19atoms/cm3；
The growth condition is maintained unchanged, the flow rate of the stable TMIn is 1500-1700sccm, and 100-150s of In is growny2Ga(1-y2)N, the growth thickness is D5, the In doping concentration is 1E +20-3E +20atoms/cm3D4+ D5 in the range of 3-3.5nm, y1 and y2 in the range of 0.015-0.25, wherein y1 and y2 are not equal;
raising the temperature to 800-y1Ga(1-y1)N/Iny2Ga(1-y2)The number of N/GaN cycles is 10-15.
7. The method as claimed in claim 1, wherein the P-type AlGaN layer is grown by raising the temperature to 900-1000 ℃ and maintaining the pressure in the reaction chamber at 200-400mbar, and the P-type AlGaN layer with a thickness of 20-50nm is continuously grown on the MQW of the active layer, wherein the Al doping concentration is 1E +20-3E +20atoms/cm3Mg doping concentration of 5E +18-1E +19atoms/cm3。
8. The method as claimed in claim 1, wherein the growing of the Mg-doped P-type GaN layer is further performed by raising the temperature to 930-3。
9. The method as claimed in claim 1, wherein the temperature is lowered to 800 ℃ for 20-30min, and then the epitaxial wafer is cooled in a furnace.
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Denomination of invention: Growth method of LED epitaxial wafer Granted publication date: 20201009 Pledgee: Huaxia Bank Co.,Ltd. Chenzhou Branch Pledgor: XIANGNENG HUALEI OPTOELECTRONIC Co.,Ltd. Registration number: Y2024980045783 |