CN111192942B - Growth method for improving AlGaN/AlN multi-quantum well interface quality - Google Patents
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- 229910002704 AlGaN Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 230000004888 barrier function Effects 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract 2
- 239000002184 metal Substances 0.000 claims abstract 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical group C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical group C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 14
- 238000011065 in-situ storage Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
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- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0075—Processes for devices with an active region comprising only III-V compounds comprising nitride compounds
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- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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Abstract
The invention relates to a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, which is carried out in MOCVD equipment, and the growth is interrupted when the AlGaN quantum well and the AlN quantum barrier are periodically switched, so that the formation of an interface component gradient layer is inhibited; meanwhile, the III and V group sources are periodically and alternately provided in the AlN growth process, the pre-reaction between the reaction sources is reduced, the lateral migration capability of metal atoms is increased, the surface appearance of AlN is improved, the interface steepness is enhanced, and the interface quality between AlGaN and AlN is improved. The invention has the advantages that: the method can reduce the growth temperature of AlN, ensure the surface smoothness of AlN, realize the growth of AlGaN and AlN at the same temperature, inhibit the formation of a gradient layer of interface components, enhance the steepness of an interface, improve the quality of the interface, save the method economically, is simple and easy to implement, has good performance of epitaxial materials, and is an effective solution for realizing the growth of AlGaN/AlN multiple quantum well structures with high quality and low cost.
Description
Technical Field
The invention discloses a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, and belongs to the technical field of semiconductors.
Background
The AlGaN semiconductor material has a wider direct band gap, and the forbidden band width is continuously adjustable from 3.4-6.2eV, so that the corresponding band of the spectrum covers the band from near ultraviolet to deep ultraviolet (200-365 nm). In addition, AlGaN materials also have the characteristics of large thermal conductivity, high electron saturation rate, strong breakdown field, good thermal stability, and the like, and thus have attracted attention in the field of manufacturing ultraviolet Light Emitting Diodes (LEDs), ultraviolet laser diodes, ultraviolet detectors, and other optoelectronic devices. Compared with a traditional ultraviolet mercury lamp, the ultraviolet LED light source has the following advantages: the energy-saving and power-saving device has the advantages of no mercury, small beam angle, less required lenses, small size, high response speed, long service life, less heat generation, safety in use and the like. Therefore, the ultraviolet LED has wide application prospect and huge market demand in the fields of high-color-rendering-index white light illumination, drinking water sterilization, air purification, biological analysis, medical treatment, printing, photoetching and the like.
The AlGaN/AlN multiple quantum well is one of important active layer structures of an ultraviolet photoelectric device, and the precise control of specific light emitting and absorbing wave bands can be realized by setting parameters such as components, thickness and the like of the multiple quantum well structure. Meanwhile, the quality of the quantum well interface is closely related to the quantum efficiency, the electronic structure of the active layer and the quantum state, and the improvement of the quantum well interface quality is the key for realizing the high-performance AlGaN photoelectric device. However, the epitaxial growth conditions of AlGaN and AlN materials have great difference, the AlN growth temperature needs higher growth temperature, and the low-temperature AlN easily presents an island-shaped growth mode, so that the problems of large surface fluctuation, fuzzy interface and the like are caused; the AlGaN material has a lower growth temperature than AlN, and the decomposition of the AlGaN material can be caused by too high temperature, so that the surface is coarsened, and non-radiative recombination centers such as vacancy defects, dislocation pits and the like are formed on the surface, so that the quantum efficiency is reduced. Therefore, what method is adopted in the epitaxial growth process to solve the problem of the contradiction is important for the epitaxial growth of the high-quality AlGaN/AlN multi-quantum well structure.
Disclosure of Invention
The invention provides a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, and aims to reduce the growth temperature of AlN, improve the gradient of the AlGaN/AlN multiple quantum well interface and reduce interface defects, thereby obtaining a high-quality AlGaN/AlN multiple quantum well active layer structure and providing a higher-quality epitaxial material for a high-performance AlGaN-based ultraviolet light electric device.
The technical solution of the invention is as follows: in the growth process of the AlN quantum barrier, in order to make up the problem of low growth temperature and weak Al atom migration capability, a method of alternately introducing TMAl and NH3 is adopted to reduce the pre-reaction between reaction sources and improve the lateral migration capability of active Al atoms, so that the surface flatness of AlN is improved; when the growth of the quantum well and the growth of the quantum barrier are switched, the growth is suspended and the pipeline is purged, so that the growth of an aluminum component gradient layer is reduced, and the interface steepness of the multiple quantum wells is further improved. The problem of inconsistent growth temperature of AlGaN and AlN is solved, and the growth of a high-quality AlGaN/AlN multiple quantum well structure at the same temperature is realized.
The method specifically comprises the following steps in the process of growing the multiple quantum well:
1) and selecting a substrate, transferring the substrate into an MOCVD system, and sequentially growing a nucleating layer, a buffer layer and an n-type doping layer. The substrate is a (0001) plane sapphire substrate; the nucleating layer is an AlN film with the thickness of 20-100 nm; the buffer layer is an AlGaN film, the aluminum component is 1-0.5, and the thickness is 1000-; the n-type doped layer is AlGaN film, the aluminum component is 0.6-0.4, the thickness is 1000-2500nm, and the doping concentration is 5E17-2E19cm3。
2) Carrying out quantaAnd (4) growing a base. The quantum barrier is AlN layer, the III group source is trimethylaluminum (TMAl), the V group source is high-purity ammonia (NH)3)，TMAl、NH3Alternately introducing into the reaction chamber, first introducing TMAl for 2-6s, then introducing NH3 for 2-6s, alternately cycling for 2-20, the V/III ratio (the molar ratio of the III source to the V source) being 500-1000, the growth temperature being 1050-1150 ℃, the pressure being 50-150torr, and the thickness being 2-20 nm.
3) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 2), stopping introducing TMAl, and suspending growth for 5-10 s.
4) And growing the quantum well. The quantum well is AlGaN layer, the III group source is trimethyl gallium (TMGa) and TMAl, the V group source is NH3，TMGa 、TMAl、NH3Simultaneously, the reaction chamber is filled with the solution for 10-60s, the V/III ratio is 1500-3000, the aluminum component is 0.5-0, the growth temperature is 1050-1150 ℃, the pressure is 50-150torr, and the thickness is 2-10 nm.
5) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 4), stopping introducing TMGa and TMAl, and pausing the growth for 5-10 s.
6) And repeating the steps 2) -5) in multiple periods to grow the active layer with the multiple quantum well structure. The number of the repeating cycles is 2-20, and the total thickness of the active layer is 20-200 nm.
7) And growing a p-type doped layer, and reducing the temperature to perform in-situ nitrogen annealing. The p-type doped layer is AlGaN film, the aluminum component is 0.5-0, the thickness is 100-350nm, and the doping concentration is 5E17-2E19cm3The nitrogen in-situ annealing temperature is 650-850 ℃, and the annealing time is 60-600 s.
8) And after the growth is finished, cooling and taking out the film material.
The invention has the beneficial effects that:
1) the temperature suitable for epitaxial growth of the AlGaN quantum well is adopted, and meanwhile, the growth temperature is also adopted by the AlN quantum barrier, so that the temperature switching of the growth of the quantum well and the quantum barrier is reduced, and the decomposition of AlGaN in the temperature rise process is avoided.
1) TMAl and NH3 are alternately introduced in the AlN growth process, pre-reaction between reaction sources is reduced, and the lateral migration capability of active Al atoms is improved, so that the epitaxial growth of a high-quality AlN quantum barrier at a lower temperature is realized.
3) When the growth of the quantum well and the growth of the quantum barrier are switched, TMAl and TMGa sources are stopped to be introduced, the growth is suspended for purging, the growth of a component gradient layer in the switching process is reduced, and the interface steepness of the multiple quantum well is further improved.
2) The method is simple and easy to implement, can reduce the time for heating and cooling in the process of growing the multiple quantum wells, saves time and labor, obtains the AlGaN/AlN multiple quantum well structure with clear interface, smooth surface and low defect density, and is an effective method for realizing the high-performance and low-cost growth of the AlGaN/AlN multiple quantum well structure.
Drawings
FIG. 1 is a schematic diagram of AlGaN/AlN multiple quantum well growth in the present invention.
FIG. 2 is a sectional image of a transmission electron microscope of an AlGaN/AlN multiple quantum well structure obtained by epitaxy according to the present invention.
FIG. 3 is an atomic force microscope surface topography image of an AlGaN/AlN multiple quantum well structure obtained by epitaxy according to the present invention.
Detailed Description
In order to further explain the present disclosure, the present disclosure is further described in detail below with reference to the attached drawings and examples.
Example 1
The invention provides a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, which comprises the following steps:
1) selecting a (0001) plane sapphire substrate, transferring the substrate into an MOCVD system, and sequentially growing a nucleation layer, a buffer layer and an n-type doping layer. The nucleating layer is an AlN film and has the thickness of 20 nm; the buffer layer is an AlN thin film and the thickness is 1000 nm; the n-type doped layer is AlGaN film, the aluminum component is 0.6, the thickness is 2500nm, and the doping concentration is 2E19cm3。
2) And (5) growing a quantum barrier. The quantum barrier is AlN layer, the III group source is TMAl, the V group source is high-purity NH3，TMAl、NH3Alternately introducing into the reaction chamber for 4 periods, introducing TMAl for 6s, and introducing NH3The flow-in time was 6s, the V/III ratio (molar ratio of group III source to group V source) was 500, the growth temperature was 1150 ℃, the pressure was 50torr, and the thickness was 4 nm.
3) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 2), stopping introducing TMAl, and pausing the growth for 5 s.
4) And growing the quantum well. The quantum well is AlGaN layer, the III group source is TMGa and TMAl, the V group source is NH3，TMGa 、TMAl、NH3And simultaneously introducing into a reaction chamber for 30s, wherein the V/III ratio is 1500, the aluminum component is 0.4, the growth temperature is 1150 ℃, the pressure is 50torr, and the thickness is 6 nm.
5) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 4), stopping introducing TMGa and TMAl, and pausing the growth for 5 s.
6) And repeating the steps 2) -5) in multiple periods to grow the active layer with the multiple quantum well structure. The number of the repetition cycles was 20, and the total thickness of the active layer was 200 nm.
7) And growing a p-type doped layer, and reducing the temperature to perform in-situ nitrogen annealing. The p-type doped layer is AlGaN film, the aluminum component is 0.5, the thickness is 250nm, and the doping concentration is 2E19cm3The nitrogen in-situ annealing temperature is 850 ℃, and the annealing time is 600 s.
8) And after the growth is finished, cooling and taking out the film material.
Example 2
The invention provides a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, which comprises the following steps:
1) selecting a (0001) plane sapphire substrate, transferring the substrate into an MOCVD system, and sequentially growing a nucleation layer, a buffer layer and an n-type doping layer. The nucleating layer is an AlN thin film and has the thickness of 100 nm; the buffer layer is an AlGaN film, the aluminum component is 0.5, and the thickness is 2500 nm; the n-type doped layer is AlGaN film, the aluminum component is 0.4, the thickness is 1000nm, and the doping concentration is 5E17cm3。
2) And (5) growing a quantum barrier. The quantum barrier is AlN layer, the III group source is TMAl, the V group source is high-purity NH3，TMAl、NH3Alternately introducing into the reaction chamber at 20 alternate periods, introducing TMAl for 2s, and introducing NH3The flow-in time was 2s, the V/III ratio (molar ratio of group III source to group V source) was 1000, the growth temperature was 1050 ℃, the pressure was 150torr, and the thickness was 20 nm.
3) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 2), stopping introducing TMAl, and pausing the growth for 10 s.
4) And growing the quantum well. The quantum well is AlGaN layer, the III group source is trimethyl gallium TMGa and TMAl, the V group source is NH3，TMGa 、TMAl、NH3And simultaneously introducing into a reaction chamber for 60s, wherein the V/III ratio is 3000, the aluminum component is 0.2, the growth temperature is 1050 ℃, the pressure is 150torr, and the thickness is 10 nm.
5) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 4), stopping introducing TMGa and TMAl, and pausing the growth for 10 s.
6) And repeating the steps 2) -5) in multiple periods to grow the active layer with the multiple quantum well structure. The number of the repetition cycles was 2, and the total thickness of the active layer was 60 nm.
7) And growing a p-type doped layer, and reducing the temperature to perform in-situ nitrogen annealing. The p-type doped layer is AlGaN film, the aluminum component is 0.2, the thickness is 350nm, and the doping concentration is 1E18cm3The nitrogen in-situ annealing temperature is 750 ℃, and the annealing time is 300 s.
8) And after the growth is finished, cooling and taking out the film material.
Example 3
The invention provides a growth method for improving the quality of an AlGaN/AlN multiple quantum well interface, which comprises the following steps:
1) selecting a (0001) plane sapphire substrate, transferring the substrate into an MOCVD system, and sequentially growing a nucleation layer, a buffer layer and an n-type doping layer. The nucleating layer is an AlN film with the thickness of 50 nm; the buffer layer is an AlN thin film and the thickness is 1500 nm; the n-type doped layer is AlGaN film, the aluminum component is 0.4, the thickness is 2500nm, and the doping concentration is 1E19cm3。
2) And (5) growing a quantum barrier. The quantum barrier is AlN layer, the III group source is TMAl, the V group source is high-purity NH3，TMAl、NH3Alternately introducing into the reaction chamber for 2 periods, introducing TMAl for 6s, and introducing NH3The flow-in time was 6s, the V/III ratio (molar ratio of group III source to group V source) was 500, the growth temperature was 1050 ℃, the pressure was 100torr, and the thickness was 2 nm.
3) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 2), stopping introducing TMAl, and pausing the growth for 8 s.
4) And growing the quantum well. The quantum well is a GaN layer, the III group source is trimethyl gallium (TMGa), and the V group source is NH3，TMGa、NH3And simultaneously introducing the mixture into a reaction chamber, wherein the introducing time is 10s, the V/III ratio is 1500, the growth temperature is 1050 ℃, the pressure is 100torr, and the thickness is 2 nm.
5) Growth was suspended and purged. Chamber temperature, pressure, carrier gas and NH3Keeping the flow rate unchanged with the step 4), stopping introducing the TMGa, and pausing the growth for 8 s.
6) And repeating the steps 2) -5) in multiple periods to grow the active layer with the multiple quantum well structure. The number of the repetition periods was 5, and the total thickness of the active layer was 20 nm.
7) And growing a p-type doped layer, and reducing the temperature to perform in-situ nitrogen annealing. The p-type doped layer is a GaN film with a thickness of 100nm and a doping concentration of 5E17cm3The nitrogen in-situ annealing temperature is 650 ℃, and the annealing time is 60 s.
8) And after the growth is finished, cooling and taking out the film material.
The samples obtained by the steps are tested and analyzed, and the AlGaN/AlN multi-quantum well interface grown by the method is proved to be steep and smooth in surface. The AlGaN/AlN multi-quantum well structure obtained by the method is subjected to section test analysis by adopting a transmission electron microscope test method, as shown in figure 2, the AlGaN quantum well and the AlN quantum barrier are arranged in parallel in a multi-period mode, the interface is clear and visible, and the method effectively improves the interface quality of the AlGaN/AlN multi-quantum well. The surface morphology of the AlGaN/AlN multiple quantum well structure grown by the method is characterized by adopting an atomic force microscope test method, and the scanning size is 10 microns multiplied by 10 microns as shown in figure 3. The result shows that atomic steps on the surface of the AlGaN/AlN multi-quantum well film material obtained by the method are clear and visible, the surface flatness is high, and the Root Mean Square (RMS) of the surface roughness is only 1.0 nm.
The invention alternately introduces TMAl and NH3The method reduces the pre-reaction of the reaction source, improves the lateral migration capability of the active Al atoms, and improves the surface flatness of the AlN quantum barrier; meanwhile, when the growth of the quantum well and the growth of the quantum barrier are switched, the growth is suspended and the pipeline is purged, so that the growth of an aluminum component gradient layer is reduced, and the interface steepness of the multiple quantum wells is further improved. The method can overcome the problem of inconsistent growth temperatures of AlGaN and AlN, and realizes the growth of a high-quality AlGaN/AlN multiple quantum well structure at the same temperature. The method is simple and easy to implement, has good material performance, and is an effective method for realizing the growth of the AlGaN/AlN multiple quantum well structure with high quality and low cost.
Claims (6)
1. The growth method for improving the interface quality of the AlGaN/AlN multi-quantum well is characterized by comprising the following steps in the growth process of the multi-quantum well:
1) selecting a substrate, transferring the substrate into a metal organic chemical vapor deposition system, and sequentially growing a nucleation layer, a buffer layer and an n-type doping layer;
2) growing a quantum barrier;
3) suspending growth and purging;
4) carrying out the growth of a quantum well;
5) suspending growth and purging;
6) repeating the steps 2) -5) in multiple periods to grow the active layer with the multiple quantum well structure;
7) growing a p-type doping layer, reducing the temperature and carrying out in-situ nitrogen annealing;
8) after the growth is finished, cooling and taking out the film material;
in the step 2), the quantum barrier is an AlN layer, the III group source is trimethylaluminum, the V group source is high-purity ammonia gas in the growth process, the trimethylaluminum and the high-purity ammonia gas are alternately introduced into the reaction chamber, the trimethylaluminum introduction time is 2-6s, the high-purity ammonia gas introduction time is 2-6s, the alternate period is 2-20, the molar ratio of the III group source to the V group source is 500-1000, the growth temperature in the reaction chamber is 1050-1150 ℃, the pressure is 50-150torr, and the thickness is 2-20 nm;
in the step 4), the quantum well is an AlGaN layer, the III group source is trimethyl gallium and trimethyl aluminum, the V group source is high-purity ammonia gas, the trimethyl gallium, the trimethyl aluminum and the high-purity ammonia gas are simultaneously introduced into the reaction chamber, the introduction time is 10-60s, the molar ratio of the III group source to the V group source is 1500-3000, the aluminum component is 0.5-0, the growth temperature is 1050-1150 ℃, the pressure is 50-150torr, and the thickness is 2-10 nm.
2. The growth method for improving the interface quality of the AlGaN/AlN multiple quantum well according to claim 1, wherein in the step 1), the substrate is a (0001) plane sapphire substrate; the nucleating layer is an AlN film with the thickness of 20-100 nm; the buffer layer is an AlGaN film, the aluminum component is 1-0.5, and the thickness is 1000-; the n-type doped layer is AlGaN film, the aluminum component is 0.6-0.4, the thickness is 1000-2500nm, and the doping concentration is 5E17-2E19cm3。
3. The growth method for improving the quality of AlGaN/AlN multiple quantum well interface as claimed in claim 1, wherein in the step 3), the temperature of the reaction chamber is 1050-.
4. The growth method for improving the quality of AlGaN/AlN multiple quantum well interface as claimed in claim 1, wherein in the step 5), the temperature of the reaction chamber is 1050-.
5. The growth method for improving the quality of an AlGaN/AlN multiple quantum well interface according to claim 1, wherein the number of repetition cycles of the step 6) is 2 to 20, and the total thickness of the active layer is 20 to 200 nm.
6. The carrier of claim 1The growth method for improving the quality of the AlGaN/AlN multi-quantum well interface is characterized in that the p-type doping layer in the step 7) is an AlGaN film, the aluminum component is 0.5-0, the thickness is 100-350nm, and the doping concentration is 5E17-2E19cm3The nitrogen in-situ annealing temperature is 650-850 ℃, and the annealing time is 60-600 s.
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