CN115377265B - Method for growing semi-polar (11-22) surface gallium nitride on silicon substrate - Google Patents

Method for growing semi-polar (11-22) surface gallium nitride on silicon substrate Download PDF

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CN115377265B
CN115377265B CN202211083705.5A CN202211083705A CN115377265B CN 115377265 B CN115377265 B CN 115377265B CN 202211083705 A CN202211083705 A CN 202211083705A CN 115377265 B CN115377265 B CN 115377265B
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gallium nitride
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赵桂娟
茆邦耀
邢树安
刘贵鹏
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Lanzhou University
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Abstract

The invention relates to a method for epitaxially growing high-quality semi-polar (11-22) surface gallium nitride on a silicon patterned substrate. According to the invention, through an improved high-temperature-low-temperature gallium nitride layer growth method, firstly, a layer of aluminum nitride is grown on the (1-11) surface of a patterned silicon substrate, then, a layer of gallium nitride is grown at a high temperature to fill a pattern groove, finally, gallium nitride is grown at a low temperature, and finally, a semi-polar (11-22) surface gallium nitride epitaxial layer with a smooth surface is obtained. The sample prepared by the method can effectively improve the quantum confinement Stark effect of the polar plane gallium nitride, and reduce the influence of the quantum confinement Stark effect on the luminous performance of the photoelectric semiconductor device.

Description

Method for growing semi-polar (11-22) surface gallium nitride on silicon substrate
Technical Field
The invention relates to the field of semiconductors, in particular to a method for preparing a high-quality semi-polar (11-22) surface gallium nitride epitaxial layer on a patterned silicon substrate by adopting an improved high-temperature-low-temperature growth method.
Background
With the rapid development of lighting technology, light Emitting Diodes (LEDs) have gradually replaced incandescent lamps, which are the common lighting means in our lives. LEDs have higher luminous efficiency and are more environmentally friendly than incandescent lamps. The development of LEDs is not separated from the rapid development of group III nitrides, such as GaN. The crystal quality of GaN greatly restricts the improvement of the luminous efficiency of GaN-based LEDs. At present, the (0001) plane GaN material growth and the preparation process of the light-emitting device are mature, but two problems to be solved still exist: one in the presence of polarization effects and the other in the absence of a suitable substrate.
In the prior art, gallium nitride (11-22) faces are generally grown on a sapphire substrate, but the lattice mismatch and thermal mismatch of the sapphire substrate and GaN are large, and the problems of poor electrical conductivity, low thermal conductivity and the like also exist. Therefore, gaN dislocation density epitaxially grown on the sapphire substrate is high, and meanwhile, the device processing technology is complex due to high material hardness and difficult cleavage. On the other hand, the epitaxy process of gallium nitride is mainly a direct growth method at present, and the upper surface of GaN grown by the method cannot be completely healed, and the service performance of the GaN is still affected.
Disclosure of Invention
The invention aims to overcome the incompleteness of the prior art and provides a method for epitaxially growing high-quality semi-polar (11-22) surface gallium nitride on a silicon patterned substrate.
The invention relates to a method for growing semi-polar (11-22) surface gallium nitride on a silicon substrate, which comprises the following steps:
1) Preparing a silicon patterned substrate, wherein a groove and a mask layer SiO are arranged on the silicon patterned substrate 2 ；
2) Growing an AlN layer on the (1-11) surface of silicon by adopting an MOCVD method;
3) Growing a first layer of GaN on the AlN layer at a high temperature by adopting an MOCVD method, so that the first layer of GaN just fills the groove of the silicon patterned substrate;
4) And continuously growing a second layer of GaN on the first layer of GaN at a low temperature, and healing the first layer of GaN and the second layer of GaN to finally obtain a sample of the semi-polar (11-22) surface gallium nitride epitaxial layer with a smooth surface.
Further, in the method, a mask layer SiO 2 Located on the (113) plane of the silicon, the grooves are along the [21-1 ] plane of the silicon]Parallel grooves are formed, and long oblique sides of the grooves are (1-11) faces of silicon.
Further, in the step 2) of the method, the growth temperature of the AlN layer is 1100-1200 ℃, the growth time is 8-12min, and the V/III ratio of the AlN layer is 600-800.
Further, in the step 3) of the method, the growth temperature of the high-temperature growth first layer GaN is 1050-1150 ℃, the growth time is 50-70min, and the V/III ratio of the first layer GaN is 1200-1700.
Further, in the step 4) of the method, the growth temperature of the second layer GaN is 1000-1100 ℃, the growth time is 80-100min, and the V/III ratio of the second layer GaN is 1200-1700.
Further, the surface roughness of the gallium nitride epitaxial layer in step 4) of the method is 5-50nm.
Further, the method of MOCVD described in the method specifically comprises the following steps: a source of metal organic compound (MO) and a source of N are carried by a carrier gas (hydrogen or nitrogen) in gaseous form to a reaction chamber for reaction. In this method, the gas molecules introduced reach the surface of the substrate in a diffuse manner. In the gas phase, the metal-organic compound may react with the non-metal hydride or the organic compound, and the adduct formed by the reaction may gradually decompose or nucleate in the gas phase when the temperature increases. The source molecules adsorb to the substrate surface during diffusion and then migrate to the crystallization area. The source molecules in the crystalline region react chemically to form an epitaxial layer. The byproducts generated by the reaction are desorbed on the growth surface, returned to the main gas flow by diffusion, and carried out of the reaction chamber together with part of the gas phase product by the carrier gas.
Further, when the AlN layer is grown in the step 2) of the method, the Al source is Trimethylaluminum (TMAL), and the N source is ammonia (NH 3); when GaN grows in the steps 3) and 4), the Ga source is trimethyl gallium (TMGa), and the N source is ammonia (NH 3)
According to the invention, a gallium nitride epitaxial layer with a (11-22) surface is epitaxially grown on a silicon substrate with a (113) surface, wherein the included angle between the (113) surface and the (1-11) surface of the silicon substrate is found to be 58.5 degrees through calculation of a crystal phase; the included angle between the (11-22) plane and the (0001) plane of gallium nitride is 58.4 degrees, and the two planes are very close. The growth habit of gallium nitride is that the growth rate of c-axis (0001) orientation is far higher than that of other crystal orientations, and when the (0001) plane of GaN grows and heals along the (1-11) plane direction of silicon, the upper surface of the grown GaN epitaxial layer is the (11-22) plane.
Compared with the prior art, the invention has the following beneficial technical effects:
the high-temperature-low-temperature growth method adopted by the invention can grow high-quality semi-polar (11-22) surface gallium nitride. On one hand, the method of the invention adopts the silicon substrate, so that the cost can be reduced, the silicon material has mature process, strong operability and strong controllability, and the heat conduction and the electric conductivity are very good; on the other hand, the grown semi-polar gallium nitride can effectively reduce the quantum confinement Stark effect. And a main peak at 69.19℃representing the (11-22) plane of gallium nitride was detected by XRD (irradiation from the [1-100] direction); the surface roughness under AFM testing is on the order of nanometers; in the SEM image, it can be seen intuitively that there is a smooth surface.
Drawings
FIG. 1 is a schematic diagram of the MOCVD method;
FIG. 2 is an SEM sectional view of the sample of example 1;
FIG. 3 is an SEM surface view of the sample of example 1;
FIG. 4 is an SEM sectional view of the sample of comparative example 1;
FIG. 5 is an SEM surface view of the sample of comparative example 1;
FIG. 6 is an SEM sectional view of the sample of comparative example 2;
FIG. 7 is an SEM surface view of the sample of comparative example 2;
FIG. 8 is an SEM sectional view of the sample of comparative example 3;
fig. 9 is an SEM surface view of the sample described in comparative example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
the invention relates to a method for growing semi-polar (11-22) surface gallium nitride on a silicon substrate, which comprises the following steps:
1) Preparing a silicon patterned substrate;
a silicon patterned substrate comprising a silicon oxide film having a mask layer (SiO) 2 ) Has parallel grooves along (21-1), and the long oblique sides of the grooves are the (1-11) surfaces of silicon;
2) Growing an AlN layer on the (1-11) surface of silicon by adopting an MOCVD method;
growing a first layer of GaN on the AlN layer at a high temperature by adopting an MOCVD method, so that the first layer of GaN just fills the groove of the silicon patterned substrate;
4) And continuously growing a second layer of GaN on the first layer of GaN at a low temperature, and healing the first layer of GaN and the second layer of GaN to finally obtain a sample of the semi-polar (11-22) surface gallium nitride epitaxial layer with a smooth surface.
As shown in fig. 1, the method of MOCVD in the steps 2) to 4) specifically includes: a source of metal organic compound (MO) and a source of N are carried by a carrier gas (hydrogen or nitrogen) in gaseous form to a reaction chamber for reaction. Wherein, when growing the AlN layer in the step 2), the Al source is Trimethylaluminum (TMAL), and the N source is ammonia (NH 3); when GaN grows in the steps 3) and 4), the Ga source is trimethyl gallium (TMGa), and the N source is ammonia (NH 3)
The growth temperature of the AlN layer grown in the step 2) is 1120 ℃, the growth time is 10min, and the V/III ratio of the AlN layer is 700. The growth temperature of the first layer GaN grown at high temperature in the step 3) is 1100 ℃, the growth time is 60min, and the V/III ratio of the first layer GaN is 1500; and 4) growing the second layer GaN at the low temperature in the step 4) at 1040 ℃ for 90min, wherein the V/III ratio of the second layer GaN is 700.
The prepared sample with the GaN epitaxial layer is subjected to crystal orientation determination by an X-ray diffraction spectrometer, and the surface quality is detected by a scanning electron microscope and an atomic force microscope. The grown gallium nitride epitaxial layer was found to have a smooth high quality semi-polar (11-22) surface with a surface roughness of only 6.375, as shown in fig. 2 and 3.
Comparative example 1: this comparative example 1 differs from example 1 only in that: and 4) growing the second layer GaN layer at low temperature in the step for 30min.
Comparative example 2: this comparative example 2 differs from example 1 only in that: the V/III ratio of the first layer GaN in the step 3) is 700, and the V/III ratio of the second layer GaN in the step 4) is 700.
Comparative example 3: this comparative example 3 differs from example 2 only in that: the V/III ratio of the first layer GaN in the step 3) is 1500, and the V/III ratio of the second layer GaN in the step 4) is 3000.
As is apparent from the above examples and comparative examples in combination with fig. 4 to 9, increasing the growth time of the low temperature GaN layer can promote better healing of the GaN epitaxial layer; increasing the V/III ratio promotes the lateral growth of GaN, and is beneficial to the rapid healing of GaN grown on different stripes; however, if the V/III ratio is too large, the GaN layers are difficult to heal, and grains of other crystal orientations grow at the positions where the GaN layers are in contact with each other.

Claims (4)

1. A method of growing semi-polar (11-22) plane gallium nitride on a silicon substrate, the method comprising the steps of:
1) Preparing a silicon patterned substrate, wherein a groove and a mask layer SiO are arranged on the silicon patterned substrate 2 The method comprises the steps of carrying out a first treatment on the surface of the The mask layer SiO 2 Located on the (113) plane of the silicon, the grooves are along the [21-1 ] plane of the silicon]Parallel grooves are formed, and the long oblique sides of the grooves are (1-11) surfaces of silicon;
2) Growing an AlN layer on the (1-11) surface of silicon by adopting an MOCVD method, wherein the growth temperature of the grown AlN layer is 1100-1200 ℃, the growth time is 8-12min, and the V/III ratio of the AlN layer is 600-800;
3) Growing a first layer of GaN on the AlN layer at a high temperature by adopting an MOCVD method, so that the first layer of GaN just fills the groove of the silicon patterned substrate, wherein the growth temperature of the first layer of GaN grown at the high temperature is 1050-1150 ℃ and the growth time is 50-70min, and the V/III ratio of the first layer of GaN is 1200-1700;
4) And continuously growing a second layer of GaN on the first layer of GaN at a low temperature, healing the first layer of GaN and the second layer of GaN, and finally obtaining a sample of the gallium nitride epitaxial layer with a semi-polar (11-22) surface with a smooth surface, wherein the growth temperature of the second layer of GaN is 1000-1100 ℃, the growth time is 80-100min, and the V/III ratio of the second layer of GaN is 1200-1700.
2. The method of growing semi-polar (11-22) plane gallium nitride on a silicon substrate according to claim 1, wherein the surface roughness of the gallium nitride epitaxial layer in said step 4) is 5-50nm.
3. The method for growing semi-polar (11-22) plane gallium nitride on a silicon substrate according to claim 2, wherein the method for MOCVD in steps 2) to 4) is specifically as follows: the reaction is carried out by carrying a metal organic compound (MO) source and an N source in gaseous form with hydrogen or nitrogen gas into a reaction chamber.
4. A method of growing semi-polar (11-22) plane gallium nitride on a silicon substrate as recited in claim 3The method is characterized in that when the AlN layer is grown in the step 2), the Al source is Trimethylaluminum (TMAL) and the N source is ammonia (NH) 3 ) The method comprises the steps of carrying out a first treatment on the surface of the When GaN grows in the steps 3) and 4), the Ga source is trimethyl gallium (TMGa), and the N source is ammonia (NH) 3 ）。
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