CN106783948B - InN nano-pillar epitaxial wafer grown on Si substrate and preparation method thereof - Google Patents

InN nano-pillar epitaxial wafer grown on Si substrate and preparation method thereof Download PDF

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CN106783948B
CN106783948B CN201611166965.3A CN201611166965A CN106783948B CN 106783948 B CN106783948 B CN 106783948B CN 201611166965 A CN201611166965 A CN 201611166965A CN 106783948 B CN106783948 B CN 106783948B
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CN106783948A (en
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李国强
高芳亮
温雷
张曙光
徐珍珠
韩晶磊
余粤锋
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South China University of Technology SCUT
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Abstract

The invention discloses an InN nano-pillar epitaxial wafer grown on a Si substrate, which sequentially comprises the Si substrate, an In metal nano-microsphere layer and an InN nano-pillar layer from bottom to top. The diameter of the In metal nano microsphere In the In metal nano microsphere layer is 20-70nm. The diameter of the InN nano-pillar in the InN nano-pillar layer is 40-80nm. The invention also discloses a preparation method of the InN nano-pillar epitaxial wafer grown on the Si substrate. The nano-pillar has uniform diameter, solves the technical problem that a large amount of dislocation is generated in InN due to larger lattice mismatch with Si, greatly reduces the defect density of an InN nano-pillar epitaxial layer, is beneficial to improving the radiation recombination efficiency of carriers, and can greatly improve the luminous efficiency of nitride devices such as semiconductor lasers and light-emitting diodes.

Description

InN nano-pillar epitaxial wafer grown on Si substrate and preparation method thereof
Technical Field
The invention relates to an InN nano-pillar epitaxial wafer and a preparation method thereof, in particular to an InN nano-pillar epitaxial wafer grown on a Si substrate and a preparation method thereof.
Background
III-V nitrides are widely used in Light Emitting Diodes (LEDs), lasers, optoelectronic devices, and the like due to their stable physicochemical properties, high thermal conductivity, and high electron saturation velocity. Among the group III-V nitrides, indium nitride (InN) is receiving increasing attention from researchers due to its own unique advantages. In group III nitride semiconductors, inN has the smallest effective electron mass, highest carrier mobility, and highest saturation transit speed, which are extremely advantageous for developing high-speed electronic devices. Furthermore, inN has the smallest direct band gap, and the forbidden bandwidth is about 0.7eV, so that the light emitting range of the nitride-based light emitting diode is widened from ultraviolet (6.2 eV) to near infrared (0.7 eV), and the method has great application prospect in the aspects of infrared lasers, full spectrum display, high conversion efficiency solar cells and the like. Compared with other III-V nitride semiconductor materials, the InN material has the advantages, and besides the advantages, the nanoscale material also has more novel characteristics in the aspects of quantum effect, interface effect, volume effect, size effect and the like.
Currently, III-V nitride semiconductor devices are mainly based on epitaxial growth and fabrication on sapphire substrates. However, sapphire has a low thermal conductivity, and the high-power nitride semiconductor device using sapphire as a substrate cannot release heat effectively, so that the heat is accumulated continuously to raise the temperature, thereby accelerating the degradation of the nitride semiconductor device, and the device has disadvantages such as poor performance and short service life. In contrast, si has a higher thermal conductivity than sapphire and is less costly. There is a necessary trend to produce high-performance, low-cost nitride semiconductor devices on Si substrates. However, growing InN nanopillars of uniform diameter and high order on Si substrates is a prerequisite for the production of high performance nitride semiconductor optoelectronic devices. Since lattice mismatch and thermal mismatch between Si and InN are large; meanwhile, in the initial growth stage, the difference of In and N atom distribution proportion on the surface of the substrate causes the conditions of uneven height, uneven diameter length, poor order and the like of the grown InN nano-pillars.
At present, most of InN nano-pillars are directly grown on a Si substrate, and the nano-pillars obtained by the growth method have nonuniform diameters, namely, the diameters of the top and the bottom are inconsistent, and the nano-pillars are in the shape of an inverted pyramid, a softball bat and the like. If In, ni, au and the like are used as catalysts for growing InN nano-pillars, metals such as In, ni, au and the like serving as catalysts exist at the top ends of InN after growth, and the metal catalysts at the top ends need to be removed when the device is manufactured subsequently, so that the complexity of the device process is increased.
Disclosure of Invention
In order to overcome the defects and shortcomings In the prior art, the invention aims to provide an InN nano-pillar epitaxial wafer grown on a Si substrate, through In metal nano-microspheres on the Si substrate, firstly, the In metal nano-microspheres are used as an In supplementing source In the growth process of the InN nano-pillars, so that the nucleation and the growth of the InN nano-pillars with high order and uniform diameters are facilitated; secondly, the technical problem that a large amount of dislocation is generated in InN due to larger lattice mismatch with Si is solved, the defect density of an InN nano-pillar epitaxial layer is greatly reduced, the radiation recombination efficiency of carriers is favorably improved, and the luminous efficiency of nitride devices such as semiconductor lasers and light-emitting diodes can be greatly improved.
The invention further aims to provide a preparation method of the InN nano-pillar epitaxial wafer grown on the Si substrate, which has the advantages of simple growth process, controllable nano-pillar morphology and low preparation cost.
The aim of the invention is achieved by the following technical scheme:
the InN nano-pillar epitaxial wafer grown on the Si substrate sequentially comprises the Si substrate, the In metal nano-microsphere layer and the InN nano-pillar layer from bottom to top.
The diameter of the In metal nano microsphere In the In metal nano microsphere layer is 20-70nm.
The diameter of the InN nano-pillar in the InN nano-pillar layer is 40-80nm.
The preparation method of the InN nano-pillar epitaxial wafer grown on the Si substrate comprises the following steps:
(1) Cleaning a Si substrate;
(2) Depositing an In metal nano microsphere layer: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 400-550 ℃, and the pressure in the reaction chamber is 5.0-6.0x10 -10 Depositing an In film on a Si substrate under the condition of Torr, and annealing to obtain an In metal nano microsphere;
(3) Growth of InN nanopillar layers: using molecular beamsEpitaxial growth process, substrate temperature controlled at 500-700 deg.c and pressure in the reaction chamber of 4.0-10.0x10 -5 And (3) growing InN nano-columns with uniform diameters on the In metal nano-microspheres obtained In the step (2) under the condition that the Torr and the beam current ratio V/III are 30-40.
The annealing temperature in the step (2) is 400-550 ℃, and the annealing time is 50-300 seconds.
The substrate cleaning in the step (1) specifically comprises the following steps:
placing the Si substrate into a mixed solution of HF and deionized water in a volume ratio of 1:20 for ultrasonic treatment for 1-2 minutes, removing oxide and dirt adhering particles on the surface of the Si substrate, then placing into deionized water for ultrasonic treatment for 1-2 minutes, removing surface impurities, and drying by high-purity dry nitrogen.
The diameter of the In metal nano microsphere In the In metal nano microsphere layer is 20-70nm.
The diameter of the InN nano-pillar in the InN nano-pillar layer is 40-80nm.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) According to the InN nano-pillar epitaxial wafer grown on the Si substrate, through the In metal nano-microsphere on the Si substrate, the technical problem that a large amount of dislocation is generated In the InN nano-pillar epitaxial wafer due to larger lattice mismatch with Si is solved, the defect density of an InN nano-pillar epitaxial layer is greatly reduced, the radiation recombination efficiency of carriers is favorably improved, and the luminous efficiency of nitride devices such as semiconductor lasers and light-emitting diodes can be greatly improved.
(2) The InN nano-pillar epitaxial wafer grown on the Si substrate has the advantage of easy removal by adopting the Si substrate, and the electrode is manufactured on the InN nano-pillar semiconductor epitaxial wafer after the Si substrate is removed, so that the preparation of the nitride semiconductor device with the vertical structure is facilitated. Meanwhile, the Si substrate has the advantages of radiation resistance, high heat conductivity, high temperature resistance, stable chemical property, high strength and the like, has high reliability, and can be widely applied to high-temperature devices based on the InN nano-pillar epitaxial wafer of the Si substrate.
(3) According to the invention, si is used as a substrate, in is deposited on the Si substrate and annealed to form the In metal nano-microsphere by adopting a molecular beam epitaxy technology, the In metal nano-microsphere pre-deposited on the Si substrate is used as an In supplementing source In the growth process of InN nano-pillars, so that the phenomenon that the diameter of the top of the InN nano-pillars is larger than that of the bottom of the InN nano-pillars and the diameter of the nano-pillars is nonuniform due to insufficient In source In the growth process is avoided, the nucleation and the growth of the InN nano-pillars with high order and uniform diameter are facilitated, and the technical problem that the InN nano-pillars with uniform diameter are difficult to directly grow on the Si substrate is solved.
(4) The growth process of the invention is unique, simple and easy to implement, and has repeatability.
Drawings
Fig. 1 is a schematic structural diagram of an InN nanopillar epitaxial wafer grown on a Si substrate in accordance with the present invention.
Fig. 2 is a scanning electron micrograph of In metal nanoballs deposited on a Si substrate according to example 1 of the present invention.
Fig. 3 is a scanning electron micrograph of InN nanopillars deposited on an In metal nanoparticle layer on a Si substrate according to example 1 of the present invention.
Fig. 4 is a cross-sectional scanning electron micrograph of an InN nanopillar grown directly on a Si substrate.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
Fig. 1 is a schematic structural diagram of an InN nanopillar epitaxial wafer grown on a silicon substrate according to the present embodiment, which sequentially includes a Si substrate 1, an In metal nanoparticle layer 2, and an InN nanopillar layer 3 from bottom to top.
The preparation method of the InN nano-pillar epitaxial wafer grown on the silicon substrate comprises the following steps:
(1) Selecting a substrate and a crystal orientation: a common Si substrate is adopted;
(2) And (3) cleaning a substrate: placing the Si substrate into a mixed solution of HF and deionized water in a volume ratio of 1:20 for ultrasonic treatment for 2 minutes, removing oxide and dirt adhering particles on the surface of the Si substrate, placing into deionized water for ultrasonic treatment for 2 minutes, removing surface impurities, and drying by high-purity dry nitrogen;
(3) Depositing In metal nano microspheres: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 400 ℃, and the pressure in the reaction chamber is 6.0x10 -10 And depositing an In film on the Si substrate under the condition of Torr, and annealing for 50 seconds In situ to form the In metal nano microsphere with the diameter of 30-50 nm.
(4) Growth of InN nano-pillars with uniform diameter: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 600 ℃, and the pressure in the reaction chamber is 6.0x10 -5 Growing InN nano-columns with uniform top and bottom diameters and 30-80nm diameter distribution on the Si substrate of the In metal nano-microsphere obtained In the step (3) under the condition that the Torr and the beam current ratio V/III value are 30.
As shown In fig. 2, in metal nano-micro-spheres with diameters of 30-50nm were pre-deposited on a Si substrate In this example.
Fig. 3 is a scanning electron microscope photograph of an InN nanorod grown on a Si substrate In example 1, which has high order, uniform diameter, and no metal In residue on the top, showing that the InN nanorod epitaxial wafer prepared by the present invention has excellent performance. The sectional scanning electron microscope photograph of the InN nano-pillars directly grown on the Si substrate is shown in FIG. 4, and it is known that the nano-pillars obtained by the growth method of the InN nano-pillars directly grown on the Si substrate have nonuniform diameters, that is, the diameters of the top and the bottom are inconsistent, and the nano-pillars have the shapes of inverted pyramids, softbats and the like.
Example 2
The InN nano-pillar epitaxial wafer grown on the silicon substrate In the embodiment sequentially comprises the Si substrate, the In metal nano-microsphere layer and the InN nano-pillar layer from bottom to top.
The preparation method of the GaN nano-pillar LED epitaxial wafer grown on the Si substrate comprises the following steps:
(1) Selecting a substrate and a crystal orientation: a common Si substrate is adopted;
(2) And (3) cleaning a substrate: placing the Si substrate into a mixed solution of HF and deionized water in a volume ratio of 1:20 for ultrasonic treatment for 2 minutes, removing oxide and dirt adhering particles on the surface of the Si substrate, placing into deionized water for ultrasonic treatment for 1 minute, removing surface impurities, and drying by high-purity dry nitrogen;
(3) Depositing In metal nano microspheres: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 550 ℃, and the pressure in the reaction chamber is 6.0x10 -10 And depositing an In film on the Si substrate under the condition of Torr, and annealing In situ for 300 seconds to form the In metal nano microsphere with the diameter of 50-70 nm.
(4) Growth of InN nano-pillars with uniform diameter: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 700 ℃, and the pressure in the reaction chamber is 6.0x10 -5 Growing InN nano-columns with uniform top and bottom diameters and 30-80nm diameter distribution on the Si substrate of the In metal nano-microsphere obtained In the step (3) under the condition that the Torr and the beam current ratio V/III value are 40.
The InN nanopillar epitaxial wafer on the Si substrate prepared in this embodiment has very good performance in both electrical property and optical property, and defect density and crystallization quality, and the test data are similar to those of embodiment 1, and are not described here again.
The embodiments described above are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention should be made in the equivalent manner, and are included in the scope of the present invention.

Claims (3)

1. The preparation method of the InN nano-pillar epitaxial wafer grown on the Si substrate is characterized by comprising the following steps of:
(1) Cleaning a Si substrate;
(2) Depositing an In metal nano microsphere layer: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled at 400 ℃, and the pressure in the reaction chamber is 6.0x10 -10 Depositing an In film on a Si substrate under the condition of Torr, and annealing In situ to obtain an In metal nano microsphere with the diameter of 30-50 nm; the annealing temperature is 400 ℃, and the annealing time is 50 seconds;
(3) Growth of InN nanopillar layers: the molecular beam epitaxial growth process is adopted, the temperature of the substrate is controlled between 500 and 700℃, and the temperature of the substrate is controlled betweenThe pressure of the reaction chamber is 4.0-10.0X10 -5 And (3) growing InN nano-columns with uniform diameters on the In metal nano-microspheres obtained In the step (2) under the condition that the Torr and the beam current ratio V/III are 30-40.
2. The method for preparing an InN nanopillar epitaxial wafer grown on a Si substrate according to claim 1, wherein the Si substrate cleaning in step (1) specifically comprises:
placing the Si substrate into a mixed solution of HF and deionized water in a volume ratio of 1:20 for ultrasonic treatment for 1-2 minutes, removing oxide and dirt adhering particles on the surface of the Si substrate, then placing into deionized water for ultrasonic treatment for 1-2 minutes, removing surface impurities, and drying by high-purity dry nitrogen.
3. The method for producing an InN nanopillar epitaxial wafer grown on a Si substrate according to claim 1, wherein the diameter of the InN nanopillar in the InN nanopillar layer is 40-80nm.
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CN108206130B (en) * 2018-01-11 2023-10-10 华南理工大学 Indium nitride nano-pillar epitaxial wafer grown on aluminum foil substrate and preparation method thereof
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CN114657534B (en) * 2022-02-18 2023-06-16 华南理工大学 MoS-based 2 InN nano-pillar as well as preparation method and application thereof
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