CN110379895B - LED epitaxial growth method - Google Patents

LED epitaxial growth method Download PDF

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CN110379895B
CN110379895B CN201910676755.6A CN201910676755A CN110379895B CN 110379895 B CN110379895 B CN 110379895B CN 201910676755 A CN201910676755 A CN 201910676755A CN 110379895 B CN110379895 B CN 110379895B
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徐平
胡耀武
龚彬彬
黄胜蓝
蒋东风
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Xiangneng Hualei Optoelectrical Co Ltd
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Abstract

The application discloses an LED epitaxial growth method, which sequentially comprises the following steps: processing a substrate, growing a low-temperature nucleation layer GaN, growing a high-temperature GaN buffer layer, growing an undoped u-GaN layer, and growing N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, growth H2Medium temperature InGaN in atmosphere: si layer, growth of N2Atmosphere high-temperature GaN: the method comprises the following steps of Mg layer growing, light emitting layer growing, P type AlGaN layer growing, P type GaN contact layer growing, and cooling. The method of the invention is realized by introducing N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer, N2Atmosphere high-temperature GaN: the structure of the Mg layer promotes electron hole pairs in a light emitting area of the quantum well, enhances the luminous radiation efficiency, improves the luminous efficiency of the LED, and reduces the warping of the epitaxial wafer.

Description

LED epitaxial growth method
Technical Field
The application relates to the technical field of LED epitaxial design application, in particular to an LED epitaxial growth method.
Background
The LED (Light Emitting Diode) is a solid lighting, and has the advantages of small volume, low power consumption, long service life, high brightness, environmental protection, firmness, durability and the like, which are accepted by consumers, and the scale of the domestic production of the LED is gradually enlarged; the demands for the brightness and the light effect of the LED in the market are increased day by day, and customers pay attention to the fact that the LED is more power-saving, higher in brightness and better in light effect, and therefore higher requirements are provided for epitaxial growth of the LED.
At present, the LED market requires low driving voltage of an LED chip, and particularly, the smaller the driving voltage under large current, the better the driving voltage, and the higher the lighting effect, the better the lighting effect; the market value of the LED is reflected in (light efficiency)/unit price, the better the light efficiency is, the higher the price is, so that the high light efficiency of the LED is always the target pursued by LED research institutes of LED manufacturers and universities. And most manufacturers currently produce LEDs with dimensions that have been upgraded to 4 inches from 2 inches. After the size of the LED is upgraded to 4 inches, the LED generally has the technical problems of large warping of an epitaxial wafer, low luminous efficiency and the like.
Therefore, how to improve the light emitting efficiency of the LED by epitaxial growth of the LED and reduce the warpage of the epitaxial wafer is an urgent technical problem to be solved at the present stage.
Disclosure of Invention
In view of the above, the present application provides an LED epitaxial growth method, in which a conventional N-type GaN layer is designed to be N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer, N2Atmosphere high-temperature GaN: the Mg layer is used for enhancing the luminous radiation efficiency, improving the luminous efficiency of the LED and reducing the warping of the epitaxial wafer.
In order to solve the technical problem, the following technical scheme is adopted:
an LED epitaxial growth method is characterized by sequentially comprising the following steps: processing a substrate, growing a low-temperature nucleation layer GaN, growing a high-temperature GaN buffer layer, growing an undoped u-GaN layer, and growing N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, growth H2Medium temperature InGaN in atmosphere: si layer, growth of N2Atmosphere high-temperature GaN: mg layer, growing luminous layer, growing P-type AlGaN layer, growing P-type GaN contact layer, cooling,
the growth of N2And H2Mixed atmosphere low temperature AlInGaN: the Zn layer includes:
introduction of N2、H2And dimethylzinc DMZn in N2And H2In a mixed atmosphere of (1), the growth temperature is maintained at 500 ℃ to 550 ℃, the growth pressure is maintained at 450Torr to 550Torr, and 50-70sccm is introducedThe TMGa, 1200-1400sccm TMIn and 100-130sccm TMAl are used to grow N with the thickness of 70nm to 110nm2And H2Mixed atmosphere low temperature AlInGaN: a Zn layer with a Zn doping concentration of 2E18atoms/cm3To 5E18atoms/cm3；
The growth H2Medium temperature InGaN in atmosphere: the Si layer includes:
raising the temperature to 750-850 ℃, and introducing H2And SiH4In H2Under the atmosphere, the growth temperature is kept at 750 ℃ to 850 ℃, the growth pressure is kept at 450Torr to 550Torr, and 80-95sccm of TMGa, 900-1000sccm of TMIn and 60nm to 80nm of H are introduced to grow2Medium temperature InGaN in atmosphere: a Si layer with Si doping concentration of 1E19atoms/cm3To 3E19atoms/cm3；
The growth of N2Atmosphere high-temperature GaN: the Mg layer includes:
raising the temperature to 1050 to 1150 ℃ and introducing N2And CP2Mg in N2Under the atmosphere, the growth temperature is kept at 1050-1150 ℃, the growth pressure is kept at 450-550 Torr, and 110-130sccm TMGa is introduced to grow N with the thickness of 40-55 nm2Atmosphere high-temperature GaN: a Mg layer with Mg doping concentration of 1E20atoms/cm3To 1E21atoms/cm3。
Optionally, wherein:
the processing substrate specifically comprises: placing the sapphire substrate in H2Annealing in the atmosphere, and cleaning the surface of the substrate at 1050-1150 ℃.
Optionally, wherein:
the growth of the low-temperature nucleation layer GaN and the growth of the high-temperature GaN buffer layer are as follows:
reducing the temperature to 500-620 ℃, keeping the pressure of the reaction cavity at 400-650 Torr, and introducing NH3And TMGa, growing a low-temperature nucleation layer GaN with the thickness of 20nm to 40nm on the sapphire substrate;
stopping introducing TMGa, and carrying out in-situ annealing treatment, wherein the annealing temperature is raised to 1000-1100 ℃, and the annealing time is 5-10 min;
after annealing, adjusting the temperature to 900-1050 ℃, continuously introducing TMGa, epitaxially growing a high-temperature GaN buffer layer with the thickness of 0.2-1 μm, and controlling the growth pressure at 400-650 Torr.
Optionally, wherein:
the growing of the non-doped u-GaN layer specifically comprises the following steps:
raising the temperature to 1050-1200 ℃, keeping the pressure of the reaction cavity at 100-500 Torr, and introducing NH3And TMGa continuously growing the non-doped u-GaN layer with the thickness of 1 to 3 mu m.
Optionally, wherein:
the growing luminescent layer is specifically as follows:
maintaining the reaction chamber at a pressure of 100Torr to 500Torr and a temperature of 700 ℃ to 800 ℃, using MO sources of TEGa, TMIn and SiH4Growing In-doped quantum well layer In with thickness of 2nm to 5nmyGa (1-y)N, y ═ 0.1 to 0.3;
then raising the temperature to 800 ℃ to 950 ℃, and maintaining the pressure of the reaction chamber at 100Torr to 500Torr, the MO sources used being TEGa, TMIn and SiH4Growing a barrier layer GaN with the thickness of 8nm to 15nm, and carrying out Si doping on the barrier layer GaN, wherein the Si doping concentration is 8E16atoms/cm3To 6E17atoms/cm3；
Repeating InyGa(1-y)Growth of N, and then repeating growth of GaN to alternately grow InyGa(1-y)N/GaN light emitting layer, the number of control cycles is 5 to 15.
Optionally, wherein:
the growing of the P-type AlGaN layer specifically comprises the following steps:
keeping the pressure of the reaction chamber at 20Torr to 200Torr and the temperature at 900 ℃ to 1100 ℃, and introducing MO sources of TMAl, TMGa and CP2Mg, continuously growing a P-type AlGaN layer with the thickness of 50nm to 200nm for 3min to 10min, wherein the molar composition of Al is 10 percent to 30 percent, and the doping concentration of Mg is 1E18atoms/cm3-1E21atoms/cm3。
Optionally, wherein:
the growing of the P-type GaN layer specifically comprises the following steps:
keeping the pressure of the reaction cavity between 100Torr and 500Torr and the temperature between 850 ℃ and 1000 ℃, and introducingThe MO sources are TMGa and CP2Mg, continuously growing a P-type GaN layer with the thickness of 100nm to 800nm, wherein the Mg doping concentration is 1E18atoms/cm3-1E21atoms/cm3。
Optionally, wherein:
the growing P-type GaN contact layer specifically comprises the following steps:
keeping the pressure of the reaction cavity between 100Torr and 500Torr and the temperature between 850 ℃ and 1050 ℃, and introducing MO sources of TEGa and CP2Mg, continuously growing a P-type GaN contact layer doped with Mg with the thickness of 5nm to 20nm and the Mg doping concentration of 1E19atoms/cm3-1E22atoms/cm3。
Optionally, wherein:
the cooling specifically comprises the following steps:
after the epitaxial growth is finished, the temperature in the reaction is reduced to 650 ℃ to 800 ℃, and pure N is adopted2Annealing for 5-10 min in the atmosphere, and cooling to room temperature to finish growth.
Compared with the prior art, the method has the following effects:
first, the LED epitaxial growth method of the present invention, compared with the conventional method, designs the conventional N-type GaN layer as N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer and N2Atmosphere high-temperature GaN: mg layer structure, in which N is grown in the region closest to the quantum well2And H2Mixed atmosphere low temperature AlInGaN: a Zn layer capable of providing more holes into the quantum well region while N is added2And H2In the mixed atmosphere, atoms are difficult to reach the surface of the substrate for reaction, the transverse growth is inhibited, a thick interface can be formed, and the reflected light of the quantum well is more favorably emitted. Followed by growth of H2Medium temperature InGaN in atmosphere: si layer for accelerating lateral growth and filling low-temperature N2And H2Atmosphere grown pits defects. And finally growing high-temperature GaN: the Mg layer can effectively improve the hole concentration, the difficulty of leakage of electrons to the p type is gradually increased, the electrons can be better inhibited from leaking out of the luminous zone of the quantum well, the holes can be effectively promoted to be injected into the luminous zone of the quantum well, and the electron space of the luminous zone of the quantum well is improvedThe cavity pairs enhance the luminous radiation efficiency and improve the luminous efficiency of the LED.
Secondly, the LED epitaxial growth method of the invention introduces N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer and N2Atmosphere high-temperature GaN: the Mg layer structure is beneficial to eliminating the stress accumulation effect of the large-size sapphire substrate on the GaN film, and can remarkably increase the stress control window of the epitaxial film material, thereby reducing the warping of the epitaxial wafer, being beneficial to improving the qualification rate of the GaN epitaxial wafer, and improving the luminous efficiency and the antistatic capability of the LED.
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 schematic structural diagram of an epitaxial layer of an LED according to the present invention;
FIG. 2 is a schematic structural view of an epitaxial layer of an LED in a comparative example;
wherein, 1, a substrate, 2, a low-temperature nucleation layer GaN, 3, a buffer layer GaN, 4, a u-GaN layer, 5, N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, 6, H2Medium temperature InGaN in atmosphere: si layer, 7, N2Atmosphere high-temperature GaN: the LED comprises a Mg layer, 8a light-emitting layer, 9a P-type AlGaN layer, 10 a P-type GaN layer, 11 a P-type GaN contact layer; 12. a conventional n-GaN layer.
Detailed Description
As used in the specification and in the claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
Example 1
The following provides an application example of the LED epitaxial growth method of the present invention, and the epitaxial structure thereof is shown in fig. 1, fig. 1 is a schematic structural diagram of the LED epitaxial layer of the present invention, and the growth method is shown in fig. 1. The VEECO MOCVD is applied to grow the high-brightness GaN-based LED epitaxial wafer. By using high-purity H2Or high purity N2Or high purity H2And high purity N2The mixed gas of (2) is used as a carrier gas, high-purity NH3(NH399.999%) as an N source, a metal-organic source of trimethyl gallium (TMGa) and metal-organic source of triethyl gallium (TEGa) as a gallium source, trimethyl indium (TMIn) as an indium source, and an N-type dopant of Silane (SiH)4) Trimethylaluminum (TMAl) as the aluminum source and magnesium diclomelate (CP) as the P-type dopant2Mg), the substrate is (0001) plane sapphire, and the reaction pressure is between 100Torr and 1000 Torr. The specific growth mode is as follows:
step 1, processing a substrate 1:
annealing the sapphire substrate 1 in a hydrogen atmosphere, and cleaning the surface of the substrate at 1050-1150 ℃.
Step 2, growing a low-temperature nucleation layer GaN 2:
reducing the temperature to 500-620 ℃, keeping the pressure of the reaction cavity at 400-650 Torr, and introducing NH3And TMGa, a low-temperature nucleation layer GaN2 having a thickness of 20nm to 40nm was grown on the sapphire substrate.
Step 3, growing a high-temperature GaN buffer layer 3:
stopping introducing TMGa, and carrying out in-situ annealing treatment, wherein the annealing temperature is raised to 1000-1100 ℃, and the annealing time is 5-10 min;
after annealing, the temperature is adjusted to 900 ℃ to 1050 ℃, TMGa is continuously introduced, the high-temperature GaN buffer layer 3 with the thickness of 0.2 mu m to 1 mu m is epitaxially grown, and the growth pressure is controlled to be 400Torr-650 Torr.
Step 4, growing an undoped u-GaN layer 4:
raising the temperature to 1050-1200 ℃, keeping the pressure of the reaction cavity at 100-500 Torr, and introducing NH3And TMGa, the undoped u-GaN layer 4 is continuously grown to a thickness of 1 to 3 μm.
Step 5, growing N2And H2Mixed atmosphere low temperature AlInGaN: zn layer 5:
introduction of N2、H2And dimethylzinc DMZn in N2And H2The growth temperature is kept at 500-550 ℃, the growth pressure is kept at 450-550 Torr, 50-70sccm of TMGa, 1200-1400sccm of TMIn and 100-130sccm of TMAl are introduced, and N with the thickness of 70-110 nm is grown2And H2Mixed atmosphere low temperature AlInGaN: a Zn layer 5 with a Zn doping concentration of 2E18atoms/cm3To 5E18atoms/cm3。
In this application, 2E18 represents the 18 th power of 2 times 10, i.e. 1 x 1018By analogy, atoms/cm3Is the unit of doping concentration, the same as below.
Step 6, growing H2Medium temperature InGaN in atmosphere: si layer 6:
raising the temperature to 750-850 ℃, and introducing H2And SiH4In H2Under the atmosphere, the growth temperature is kept at 750 ℃ to 850 ℃, the growth pressure is kept at 450Torr to 550Torr, and 80-95sccm of TMGa, 900-1000sccm of TMIn and 60nm to 80nm of H are introduced to grow2Medium temperature InGaN in atmosphere: a Si layer 6 with Si doping concentration of 1E19atoms/cm3To 3E19atoms/cm3。
Step 7, growing N2Atmosphere high-temperature GaN: mg layer 7:
raising the temperature to 1050 to 1150 ℃ and introducing N2And CP2Mg in N2Under the atmosphere, the growth temperature is kept at 1050-1150 ℃, the growth pressure is kept at 450-550 Torr, and 110-130sccm TMGa is introduced to grow N with the thickness of 40-55 nm2Atmosphere high-temperature GaN: a Mg layer 7 with Mg doping concentration of 1E20atoms/cm3To 1E21atoms/cm3。
Step 8, growing a luminescent layer 8:
maintaining the reaction chamber at a pressure of 100Torr to 500Torr and a temperature of 700 ℃ to 800 ℃, using MO sources of TEGa, TMIn and SiH4Growing In-doped quantum well layer In with thickness of 2nm to 5nmyGa (1-y)N, y ═ 0.1 to 0.3;
then raising the temperature to 800 ℃ to 950 ℃, and maintaining the pressure of the reaction chamber at 100Torr to 500Torr, the MO sources used being TEGa, TMIn and SiH4Growing a barrier layer GaN with the thickness of 8nm to 15nm, and carrying out Si doping on the barrier layer GaN, wherein the Si doping concentration is 8E16atoms/cm3To 6E17atoms/cm3；
Repeating InyGa(1-y)Growth of N, and then repeating growth of GaN to alternately grow InyGa(1-y)The number of control cycles of the N/GaN light emitting layer 8 is 5 to 15.
Step 9, growing a P-type AlGaN layer 9:
keeping the pressure of the reaction chamber at 20Torr to 200Torr and the temperature at 900 ℃ to 1100 ℃, and introducing MO sources of TMAl, TMGa and CP2Mg, continuously growing a P-type AlGaN layer 9 with the thickness of 50nm to 200nm for 3min to 10min, wherein the molar composition of Al is 10 percent to 30 percent, and the doping concentration of Mg is 1E18atoms/cm3-1E21atoms/cm3。
Step 10, growing a P-type GaN layer 10:
the pressure of the reaction cavity is kept between 100Torr and 500Torr, the temperature is kept between 850 ℃ and 1000 ℃, and MO sources of TMGa and CP are introduced2Mg, a P-type GaN layer 10 with the continuous growth thickness of 100nm to 800nm and the Mg doping concentration of 1E18atoms/cm3-1E21atoms/cm3。
Step 11, growing a P-type GaN contact layer 11:
keeping the pressure of the reaction cavity between 100Torr and 500Torr and the temperature between 850 ℃ and 1050 ℃, and introducing MO sources of TEGa and CP2Mg, continuously growing a Mg-doped P-type GaN contact layer 11 with the thickness of 5nm to 20nm and the Mg doping concentration of 1E19atoms/cm3-1E22atoms/cm3。
Step 12, cooling:
after the epitaxial growth is finished, the temperature of the reaction is adjustedCooling to 650-800 deg.C, and adding pure N2Annealing for 5-10 min in the atmosphere, and cooling to room temperature to finish growth.
Example 2
A conventional LED epitaxial growth method is provided as a comparative example of the present invention, and fig. 2 is a schematic structural view of an LED epitaxial layer in the comparative example.
The conventional LED epitaxial growth method comprises the following steps (an epitaxial layer structure is shown in figure 2):
1. annealing the sapphire substrate 1 in a hydrogen atmosphere, and cleaning the surface of the substrate at 1050-1150 ℃.
2. Reducing the temperature to 500-620 ℃, keeping the pressure of the reaction cavity at 400-650 Torr, and introducing NH3And TMGa, a low-temperature nucleation layer GaN2 having a thickness of 20nm to 40nm was grown on the sapphire substrate.
3. Stopping introducing TMGa, and carrying out in-situ annealing treatment, wherein the annealing temperature is raised to 1000-1100 ℃, and the annealing time is 5-10 min; after annealing, the temperature is adjusted to 900 ℃ to 1050 ℃, TMGa is continuously introduced, the high-temperature GaN buffer layer 3 with the thickness of 0.2 mu m to 1 mu m is epitaxially grown, and the growth pressure is controlled to be 400Torr-650 Torr.
4. Keeping the temperature to 1050 ℃ to 1200 ℃, keeping the pressure of the reaction cavity at 100Torr-500Torr, and introducing NH3And TMGa, the undoped u-GaN layer 4 is continuously grown to a thickness of 1 to 3 μm.
5. Keeping the temperature of the reaction cavity at 1050-1200 ℃, keeping the pressure of the reaction cavity at 100-600 Torr, and introducing NH3TMGa and SiH4Continuously growing a Si-doped n-GaN layer 12 with a stable doping concentration and a thickness of 2 μm to 4 μm, wherein the doping concentration of Si is 8E18atoms/cm3-2E19atoms/cm3。
6. Maintaining the reaction chamber at a pressure of 100Torr to 500Torr and a temperature of 700 ℃ to 800 ℃, using MO sources of TEGa, TMIn and SiH4Growing In-doped quantum well layer In with thickness of 2nm to 5nmyGa (1-y)N, y ═ 0.1 to 0.3;
then raising the temperature to 800 ℃ to 950 ℃, maintaining the pressure of the reaction chamber at 100Torr to 500Torr, and usingThe MO sources are TEGa, TMIn and SiH4Growing a barrier layer GaN with the thickness of 8nm to 15nm, and carrying out Si doping on the barrier layer GaN, wherein the Si doping concentration is 8E16atoms/cm3To 6E17atoms/cm3；
Repeating InyGa(1-y)Growth of N, and then repeating growth of GaN to alternately grow InyGa(1-y)The number of control cycles of the N/GaN light emitting layer 8 is 5 to 15.
7. Keeping the pressure of the reaction chamber at 20Torr to 200Torr and the temperature at 900 ℃ to 1100 ℃, and introducing MO sources of TMAl, TMGa and CP2Mg, continuously growing a P-type AlGaN layer 9 with the thickness of 50nm to 200nm for 3min to 10min, wherein the molar composition of Al is 10 percent to 30 percent, and the doping concentration of Mg is 1E18atoms/cm3-1E21atoms/cm3。
8. The pressure of the reaction cavity is kept between 100Torr and 500Torr, the temperature is kept between 850 ℃ and 1000 ℃, and MO sources are introduced into the reaction cavity to obtain TMGa and Cp2Mg, a P-type GaN layer 10 with the continuous growth thickness of 100nm to 800nm and the Mg doping concentration of 1E18atoms/cm3-1E21atoms/cm3。
9. Keeping the pressure of the reaction cavity between 100Torr and 500Torr and the temperature between 850 ℃ and 1050 ℃, and introducing MO sources of TEGa and CP2Mg, continuously growing a Mg-doped P-type GaN contact layer 11 with the thickness of 5nm to 20nm and the Mg doping concentration of 1E19atoms/cm3-1E22atoms/cm3。
10. And after the epitaxial growth is finished, reducing the temperature in the reaction to 650-800 ℃, annealing for 5-10 min in a pure nitrogen atmosphere, and then reducing the temperature to room temperature to finish the growth.
The epitaxial structure is manufactured into a single small-size chip through subsequent semiconductor processing technologies such as cleaning, deposition, photoetching and etching.
On the same bench, sample 1 was prepared according to the conventional LED growth method (method of comparative example), and sample 2 was prepared according to the method described in this patent; the difference between the parameters of the epitaxial growth methods of sample 1 and sample 2 is that the conventional N-type GaN layer is designed to be N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer and N2Atmosphere high-temperature GaN: mg layer structure, other epitaxial growthThe conditions were identical.
Sample 1 and sample 2 were coated with an ITO layer of about 150nm under the same pre-process conditions, a Cr/Pt/Au electrode of about 70nm under the same conditions, and a protective layer of SiO under the same conditions2About 30nm, the sample was then ground and cut into 762 μm (30 mil) chip particles under the same conditions, and then 150 dies were individually picked at the same positions for sample 1 and sample 2, and packaged into white LEDs under the same packaging process. The photoelectric properties of sample 1 and sample 2 were then tested using an integrating sphere at a drive current of 350 mA. The photoelectric properties of sample 1 and sample 2 were tested in the same LED spotter at a drive current of 350mA, see table 1. Table 1 shows the LED tester opto-electronic test data for sample 1 and sample 2.
Table 1 sample 1 and sample 2LED tester photoelectric test data
Figure RE-GDA0002160059650000091
Figure RE-GDA0002160059650000101
The data obtained from the integrating sphere were analyzed and compared, and it was found from the data in Table 1 that the brightness of sample 2 increased from 488mw to 535mw, and the driving voltage of sample 2 decreased from 3.32V to 3.05V, compared to sample 1. The antistatic 4KV capacity is improved from 88.4% to 94.5%.
In addition, statistics on grinding and fragment conditions of 1000 samples 1 and 1000 samples 2 shows that 36 samples 1 and 18 samples 2 are fragmented, namely the fragment rate of the sample 1 is 3.6% and the fragment rate of the sample 2 is 1.8%. The following conclusions can therefore be drawn:
the growing method provided by the patent improves the brightness of the LED chip, enhances the antistatic capability, reduces the driving voltage, reduces the warping degree of the epitaxial wafer, effectively reduces the wafer breakage rate and improves the product yield.
According to the embodiments, the application has the following beneficial effects:
first, the LED epitaxial growth method of the present invention, compared with the conventional method, designs the conventional N-type GaN layer as N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer and N2Atmosphere high-temperature GaN: mg layer structure, in which N is grown in the region closest to the quantum well2And H2Mixed atmosphere low temperature AlInGaN: a Zn layer capable of providing more holes into the quantum well region while N is added2And H2In the mixed atmosphere, atoms are difficult to reach the surface of the substrate for reaction, the transverse growth is inhibited, a thick interface can be formed, and the reflected light of the quantum well is more favorably emitted. Followed by growth of H2Medium temperature InGaN in atmosphere: si layer for accelerating lateral growth and filling low-temperature N2And H2Atmosphere grown pits defects. And finally growing high-temperature GaN: the Mg layer can effectively promote the hole concentration, and make the electron increase gradually to the degree of difficulty that the p type was revealed, the suppression electron that can be better reveals the quantum well light-emitting area, can also effectively promote the hole and pour into the quantum well light-emitting area into, promote the electron hole pair in the quantum well light-emitting area, reinforcing luminous radiant efficiency improves LED's luminous efficacy.
Secondly, the LED epitaxial growth method of the invention introduces N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, H2Medium temperature InGaN in atmosphere: si layer and N2Atmosphere high-temperature GaN: the Mg layer structure is beneficial to eliminating the stress accumulation effect of the large-size sapphire substrate on the GaN film, and can remarkably increase the stress control window of the epitaxial film material, thereby reducing the warping of the epitaxial wafer, being beneficial to improving the qualification rate of the GaN epitaxial wafer, and improving the luminous efficiency and the antistatic capability of the LED.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as a method, apparatus, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-usable storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and the like) having computer-usable program code embodied therein.
The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.

Claims (9)

1. An LED epitaxial growth method is characterized by sequentially comprising the following steps: processing a substrate, growing a low-temperature nucleation layer GaN, growing a high-temperature GaN buffer layer, growing an undoped u-GaN layer, and growing N2And H2Mixed atmosphere low temperature AlInGaN: zn layer, growth H2Medium temperature InGaN in atmosphere: si layer, growth of N2Atmosphere high-temperature GaN: mg layer, growing luminous layer, growing P-type AlGaN layer, growing P-type GaN contact layer, cooling,
the growth of N2And H2Mixed atmosphere low temperature AlInGaN: the Zn layer includes:
introduction of N2、H2And dimethylzinc DMZn in N2And H2The growth temperature is kept at 500-550 ℃, the growth pressure is kept at 450-550 Torr, 50-70sccm of TMGa, 1200-1400sccm of TMIn and 100-130sccm of TMAl are introduced, and N with the thickness of 70-110 nm is grown2And H2Mixed atmosphere low temperature AlInGaN: a Zn layer with a Zn doping concentration of 2E18atoms/cm3To 5E18atoms/cm3；
The growth H2Medium temperature InGaN in atmosphere: the Si layer includes:
raising the temperature to 750-850 ℃, and introducing H2And SiH4In H2Under the atmosphere, the growth temperature is kept at750 ℃ to 850 ℃, the growth pressure is kept at 450Torr to 550Torr, and 80-95sccm of TMGa, 900-1000sccm of TMIn and 60nm to 80nm of H are introduced to grow2Medium temperature InGaN in atmosphere: a Si layer with Si doping concentration of 1E19atoms/cm3To 3E19atoms/cm3；
The growth of N2Atmosphere high-temperature GaN: the Mg layer includes:
raising the temperature to 1050 to 1150 ℃ and introducing N2And CP2Mg in N2Under the atmosphere, the growth temperature is kept at 1050-1150 ℃, the growth pressure is kept at 450-550 Torr, and 110-130sccm TMGa is introduced to grow N with the thickness of 40-55 nm2Atmosphere high-temperature GaN: a Mg layer with Mg doping concentration of 1E20atoms/cm3To 1E21atoms/cm3。
2. LED epitaxial growth method according to claim 1,
the processing substrate specifically comprises: placing the sapphire substrate in H2Annealing in the atmosphere, and cleaning the surface of the substrate at 1050-1150 ℃.
3. LED epitaxial growth method according to claim 1,
the growth of the low-temperature nucleation layer GaN and the growth of the high-temperature GaN buffer layer are as follows:
reducing the temperature to 500-620 ℃, keeping the pressure of the reaction cavity at 400-650 Torr, and introducing NH3And TMGa, growing a low-temperature nucleation layer GaN with the thickness of 20nm to 40nm on the sapphire substrate;
stopping introducing TMGa, and carrying out in-situ annealing treatment, wherein the annealing temperature is raised to 1000-1100 ℃, and the annealing time is 5-10 min;
after annealing, adjusting the temperature to 900-1050 ℃, continuously introducing TMGa, epitaxially growing a high-temperature GaN buffer layer with the thickness of 0.2-1 μm, and controlling the growth pressure at 400-650 Torr.
4. LED epitaxial growth method according to claim 1,
the growing of the non-doped u-GaN layer specifically comprises the following steps:
raising the temperature to 1050-1200 ℃, keeping the pressure of the reaction cavity at 100-500 Torr, and introducing NH3And TMGa continuously growing the non-doped u-GaN layer with the thickness of 1 to 3 mu m.
5. LED epitaxial growth method according to claim 1,
the growing luminescent layer is specifically as follows:
maintaining the reaction chamber at a pressure of 100Torr to 500Torr and a temperature of 700 ℃ to 800 ℃, using MO sources of TEGa, TMIn and SiH4Growing In-doped quantum well layer In with thickness of 2nm to 5nmyGa(1-y)N, y ═ 0.1 to 0.3;
then raising the temperature to 800 ℃ to 950 ℃, and maintaining the pressure of the reaction chamber at 100Torr to 500Torr, the MO sources used being TEGa, TMIn and SiH4Growing a barrier layer GaN with the thickness of 8nm to 15nm, and carrying out Si doping on the barrier layer GaN, wherein the Si doping concentration is 8E16atoms/cm3To 6E17atoms/cm3；
Repeating InyGa(1-y)Growth of N, and then repeating growth of GaN to alternately grow InyGa(1-y)N/GaN light emitting layer, the number of control cycles is 5 to 15.
6. LED epitaxial growth method according to claim 1,
the growing of the P-type AlGaN layer specifically comprises the following steps:
keeping the pressure of the reaction chamber at 20Torr to 200Torr and the temperature at 900 ℃ to 1100 ℃, and introducing MO sources of TMAl, TMGa and CP2Mg, continuously growing a P-type AlGaN layer with the thickness of 50nm to 200nm for 3min to 10min, wherein the molar composition of Al is 10 percent to 30 percent, and the doping concentration of Mg is 1E18atoms/cm3-1E21atoms/cm3。
7. LED epitaxial growth method according to claim 1,
the growing of the P-type GaN layer specifically comprises the following steps:
the pressure of the reaction cavity is kept between 100Torr and 500Torr, the temperature is kept between 850 ℃ and 1000 ℃, and MO sources of TMGa and CP are introduced2Mg, continuously growing a P-type GaN layer with the thickness of 100nm to 800nm, wherein the Mg doping concentration is 1E18atoms/cm3-1E21atoms/cm3。
8. LED epitaxial growth method according to claim 1,
the growing P-type GaN contact layer specifically comprises the following steps:
keeping the pressure of the reaction cavity between 100Torr and 500Torr and the temperature between 850 ℃ and 1050 ℃, and introducing MO sources of TEGa and CP2Mg, continuously growing a P-type GaN contact layer doped with Mg with the thickness of 5nm to 20nm and the Mg doping concentration of 1E19atoms/cm3-1E22atoms/cm3。
9. LED epitaxial growth method according to claim 1,
the cooling specifically comprises the following steps:
after the epitaxial growth is finished, the temperature in the reaction is reduced to 650 ℃ to 800 ℃, and pure N is adopted2Annealing for 5-10 min in the atmosphere, and cooling to room temperature to finish growth.
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