CN115259075A - Method for preparing periodic array quantum dots by adopting droplet etching epitaxial growth technology - Google Patents
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Abstract
The invention discloses a method for preparing periodic array quantum dots by adopting a droplet etching epitaxial growth technology, which comprises the following steps: s1, arranging a substrate material, and performing surface cleaning treatment; s2, growing a buffer layer on the substrate material, and growing an epitaxial layer on the buffer layer; s3, preparing a periodic array of nano holes in the epitaxial layer through a nano patterned substrate process; s4, performing hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano-cavities; s5, depositing III-group metal liquid drops at the positions of the nanometer holes on the deoxidized epitaxial layer in a positioning mode, and etching the metal liquid drops downwards at a high temperature; s6, filling quantum dot materials on the etched epitaxial layer; and S7, growing a cover layer on the quantum dots and the epitaxial layer to finish preparation. The invention introduces the liquid drop etching into the quantum dot positioning growth technology, eliminates the defects and damages introduced in the graphic processing process by further etching the original graphic layer, is beneficial to reducing the defects introduced in the quantum dot growth process and improves the performance of the quantum dot material.
Description
Technical Field
The invention relates to the technical field of semiconductor material preparation, in particular to a method for preparing periodic array quantum dots by adopting a droplet etching epitaxial growth technology.
Background
Quantum dots are a class of semiconductor materials of nanometer scale that are confined in three dimensions. Due to their size specificity, they have discrete electronic states and discrete energy levels, and are called "artificial atoms". The method is widely applied to traditional optoelectronic devices such as transistors, light emitting diodes and lasers. Meanwhile, semiconductor quantum dots are generally considered as ideal two-level systems, exhibit unique quantum confinement effects, and as single photon sources, have also received increasing attention in solid state-based quantum optical information technology.
In order to enable large-scale integration of quantum dot devices, preparation of multiple quantum bits, and construction of scalable quantum networks, semiconductor quantum dots are inevitably required to have a periodic array of structural arrangements. Since the self-organized quantum dots are spontaneously formed in the growth process, the positions of the self-organized quantum dots are randomly distributed, and uncertainty exists, the self-organized quantum dots are difficult to be integrally processed on a large scale. Early researchers prepared quantum dot arrays by epitaxial growth on patterned substrates to control the shapes, densities and spatial positions of quantum dots within the process precision range, but the luminescent quality of quantum dots formed by the method is susceptible to defects and damages caused by process etching. How to prepare defect-free quantum dots with large area and periodic array on the premise of ensuring good photoelectric properties of the quantum dots is a problem to be solved urgently by the existing quantum dot micro-nano optical quantum device technology.
In recent years, research on quantum dots grown epitaxially by droplet etching has been hot in the preparation technology of quantum dot materials. The advantages of this epitaxy technique are: 1) The essence of the liquid drop etching epitaxy is V-W mode growth, which is different from the S-K mode driven by the traditional stress and can be compatible with a homogeneous material system such as GaAs/AlGaAs and the like; 2) The quantum dots are driven by non-stress and are not limited by the size of inherent lattice mismatch, and the size and shape of the quantum dots have large regulation and control ranges, namely the quantum dots correspond to richer single photon emission regulation and control, including fine structure splitting, wavelength and the like; 3) Due to high-temperature growth, the defects of the crystal lattice are small, and the luminescent performance of the quantum dot is good.
The prior art discloses a large-area quantum dot and an array manufacturing method thereof. Firstly, depositing a thin dielectric layer on a substrate buffer layer, and manufacturing a nanopore graphic array on the dielectric layer by adopting a soft ultraviolet nanoimprint and etching process; then, taking the prepared patterned substrate as a template, growing seed layer quantum dots in the nano holes of the pattern window area by using a selective epitaxial growth process, and removing the dielectric layer to obtain a seed layer; and growing an isolation layer on the seed layer, and vertically stacking and growing quantum dots on the isolation layer to obtain the large-area perfect quantum dots and the array thereof. The reference relates to the fabrication of quantum dot arrays, but employs conventional selective epitaxial growth and vertical stack growth processes.
Disclosure of Invention
The invention provides a method for preparing periodic array quantum dots by adopting a liquid drop etching epitaxial growth technology, which introduces liquid drop etching into a quantum dot positioning growth technology, and eliminates defects and damages introduced in the graphic processing process by further etching an original graphic layer, thereby preparing the defect-free quantum dots of a large-area high-quality periodic array.
The primary objective of the present invention is to solve the above technical problems, and the technical solution of the present invention is as follows:
a method for preparing periodic array quantum dots by adopting a droplet etching epitaxial growth technology comprises the following steps:
s1, arranging a substrate material, and cleaning the surface of the substrate material;
s2, growing a buffer layer on a substrate material, and growing an epitaxial layer on the buffer layer;
s3, preparing a periodic array of nano holes in the epitaxial layer through a nano patterned substrate process;
s4, performing hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano-cavities;
s5, positioning and depositing III-group metal liquid drops on the positions of the nanometer holes on the deoxidized epitaxial layer, and etching the metal liquid drops downwards at high temperature;
s6, filling quantum dot materials on the etched epitaxial layer;
and S7, growing a cover layer on the quantum dots and the epitaxial layer to finish the preparation.
Furthermore, when the substrate material and the buffer layer are GaAs, the epitaxial layer and the cover layer are AlGaAs; when the substrate material and the buffer layer are InP, the epitaxial layer and the cover layer are InAlGaAs; when the substrate material and the buffer layer are GaSb, the epitaxial layer and the cover layer are AlGaAsSb.
Further, the thickness of the buffer layer is 100-600nm, and the buffer layer is used for flattening the surface of the substrate.
Further, the process of patterning the substrate with the nanometer structure in step S3 includes: preparing the patterned substrate by an Atomic Force Microscope (AFM) local oxidation etching or nano-imprinting or electron beam direct writing process.
Further, the diameter of the nano-holes in the step 3 is 20-90nm, and the depth is 4-30nm.
Further, the hydrogen atom auxiliary deoxidation treatment in the step 4 specifically comprises the following steps: heating the substrate to 300-400 deg.C, heating the hydrogen cracker to 1400-1800 deg.C, opening hydrogen, and controlling the vacuum of the processing cavity to 1.0 × 10–7-2×10–7mbar, degassing for 20-40min.
Further, the step 5 of depositing group III metal droplets on the surface of the epitaxial layer in a positioning manner, the deposited metal droplets are deposited in a positioning manner at the positions of the nano holes under the driving of surface free energy, and the metal droplets are etched downwards at a high temperature to eliminate defects and damages introduced in the process of the pattern substrate, and the specific steps are as follows: adjusting the temperature of the substrate to 550-700 ℃; introducing a group III metal beam, and controlling the introduction time of the group III metal beam to be 0.5-20s; the substrate temperature is raised to 600-700 ℃.
Further, the group III metal droplet used In step 5 is one of Ga, in, and Al.
Further, the quantum dot material in step 6 is GaAs, inAs, inGaAs, inGaAsP, gaSb, or AlGaSb, and the energy band thereof is smaller than the band gaps of the epitaxial layer and the cap layer material to realize the three-dimensional confinement of the carriers, and the lattice constant thereof is close to the epitaxial layer and the cap layer to reduce the stress of filling the quantum dot.
Furthermore, the thickness of the quantum dot material is 0.3-3nm; the epitaxial growth adopts molecular beam epitaxy or metal organic compound vapor deposition.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
the invention introduces the liquid drop etching into the quantum dot positioning growth technology to eliminate the defects and damages introduced in the process of the pattern substrate, is beneficial to reducing the defects introduced in the process of the quantum dot growth and improves the performance of the quantum dot material.
The method adopts the liquid drop etching to epitaxially grow the quantum dots, can be compatible with a homogeneous material system compared with the traditional S-K mode grown quantum dots, and has the advantages of no limitation of the inherent lattice mismatch, large regulation range of the size and the shape of the quantum dots and good luminous performance of the quantum dots.
The invention is especially suitable for manufacturing large-area low-density perfect quantum dot arrays, and provides a feasible scheme for large-scale integration of quantum dot devices, preparation of multiple quantum bits and construction of scalable quantum networks.
Drawings
FIG. 1 is a flow chart of a method for preparing periodic array quantum dots by a droplet etching epitaxial growth technique according to the present invention.
FIG. 2 is a schematic structural diagram of a method for preparing a periodic array quantum dot by a droplet etching epitaxial growth technique according to the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein and, therefore, the scope of the present invention is not limited by the specific embodiments disclosed below.
Example 1
As shown in fig. 1-2, the present invention provides a method for preparing a periodic array quantum dot by using a droplet etching epitaxial growth technique, comprising:
s1: taking a substrate, wherein the substrate is GaAs, and before growing a material, performing deoxidation treatment at a certain temperature according to the properties of the substrate material;
s2: growing a buffer layer on the substrate, wherein the buffer layer is made of GaAs and has the thickness of 100-600nm, and is used for flattening the surface of the substrate; and then, continuously growing an epitaxial layer, wherein the epitaxial layer is made of AlGaAs, the composition of Al is preferably 0.2-0.4, and the thickness is preferably 30-200nm.
S3: preparing a periodic array of nano holes on the epitaxial layer by a nano patterning substrate process; the nano-patterning substrate process is preferably an AFM local oxidation etching or nano-imprinting or electron beam direct writing process; the diameter of the nano-pores is preferably 20-90nm, and the depth is 4-30nm.
S4: the method comprises the following steps of carrying out hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano holes: heating the substrate to 300-400 deg.C, heating the hydrogen cracker to 1400-1800 deg.C, opening hydrogen, and controlling the vacuum of the processing cavity to 1.0 × 10–7-2×10–7mbar, degassing 20-40min。
S5: depositing Al metal liquid drops on the deoxidized epitaxial layer, wherein the Al beam current is 0.1-1.0mL/s, the deposition time is 0.5-20s, the Al metal liquid drops are positioned and deposited in the nano holes with the lowest surface energy under the drive of surface free energy, the temperature of the substrate is controlled to be 600-700 ℃, and the Al metal liquid drops are etched downwards so as to eliminate the defects and damages caused by introducing the nano holes in the process of patterning the substrate.
S6: and filling a quantum dot material on the etched epitaxial layer, wherein the quantum dot material is GaAs, and the thickness of the quantum dot material is 0.3-3nm, preferably 1.5nm.
S7: and growing a cover layer on the quantum dots and the epitaxial layer, wherein the cover layer is made of AlGaAs, the Al component is preferably 0.2-0.4, the thickness is preferably 30-200nm, and the cover layer is used for covering the quantum dots to form three-dimensional quantum confinement and avoiding the influence of a surface state on the optoelectronic properties of the quantum dots to finish the preparation.
Example 2
S1: taking a substrate, wherein the substrate is InP, and before growing a material, deoxidation treatment is carried out at a certain temperature according to the property of the substrate material;
s2: growing a buffer layer on the substrate, wherein the buffer layer is made of InP and has the thickness of 100-600nm, and is used for flattening the surface of the substrate; and then, continuously growing an epitaxial layer, wherein the epitaxial layer is made of InGaAlAs, the composition of Al is preferably 0.15-0.2, and the thickness is preferably 30-200nm.
S3: preparing a periodic array of nano holes on the epitaxial layer by a nano patterning substrate process; the nano-patterning substrate process is preferably an AFM local oxidation etching or nano-imprinting or electron beam direct writing process; the diameter of the nano-pores is preferably 20-90nm, and the depth is 4-30nm.
S4: the method comprises the following steps of (1) carrying out hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano holes: heating the substrate to 300-400 deg.C, heating the hydrogen cracker to 1400-1800 deg.C, opening hydrogen, and controlling the vacuum of the processing cavity to 1.0 × 10–7-2×10–7mbar, degassing for 20-40min.
S5: depositing In metal liquid drops on the deoxidized epitaxial layer, wherein the In beam current is 0.1-1.0mL/s, the deposition time is 0.5-20s, the In metal liquid drops are positioned and deposited In the nano holes with the lowest surface energy under the drive of surface free energy, the substrate temperature is controlled to be 600-700 ℃, and the In metal liquid drops are etched downwards so as to eliminate the defects and damages caused by introducing the nano holes In the process of patterning the substrate.
S6: and filling a quantum dot material on the etched epitaxial layer, wherein the quantum dot material is InGaAs, and the thickness of the quantum dot material is 0.3-3nm, preferably 1.5nm.
S7: and growing a cover layer on the quantum dots and the epitaxial layer, wherein the cover layer is made of InAlGaAs, the Al component is preferably 0.15-0.2, the thickness is preferably 30-200nm, and the cover layer is used for covering the quantum dots to form three-dimensional quantum restriction and simultaneously avoiding the influence of a surface state on the optoelectronic properties of the quantum dots to finish the preparation.
Example 3
S1: taking a substrate, wherein before the substrate is a GaSb growth material, deoxidation treatment is carried out at a certain temperature according to the property of the substrate material;
s2: growing a buffer layer on the substrate, wherein the buffer layer is made of GaSb and has the thickness of 100-600nm, and the buffer layer is used for flattening the surface of the substrate; and then, continuously growing an epitaxial layer, wherein the epitaxial layer is made of AlGaAsSb, the composition of Al is preferably 0.2-0.5, and the thickness is preferably 30-200nm.
S3: preparing a periodic array of nano holes on the epitaxial layer by a nano patterning substrate process; the nano-patterning substrate process is preferably an AFM local oxidation etching or nano-imprinting or electron beam direct writing process; the diameter of the nano-pores is preferably 20-90nm, and the depth is 4-30nm.
S4: the method comprises the following steps of (1) carrying out hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano holes: heating the substrate to 300-400 deg.C, heating the hydrogen cracker to 1400-1800 deg.C, opening hydrogen, and controlling the vacuum of the processing cavity to 1.0 × 10–7-2×10–7Degassing with mbar for 20-40min.
S5: depositing Al or Ga metal liquid drops on the deoxidized epitaxial layer, wherein the beam current is 0.1-1.0mL/s, the deposition time is 0.5-20s, the Al or Ga metal liquid drops are positioned and deposited in the nano holes with the lowest surface energy under the driving of surface free energy, the substrate temperature is controlled to be 600-700 ℃, and the Al or Ga metal liquid drops are etched downwards so as to eliminate the defects and damages caused by introducing the nano holes in the process of patterning the substrate.
S6: and filling a quantum dot material on the etched epitaxial layer, wherein the quantum dot material is InGaSb, and the thickness of the quantum dot material is 0.3-3nm, preferably 1.5nm.
S7: and growing a cover layer on the quantum dots and the epitaxial layer, wherein the cover layer is made of AlGaAsSb, the Al component is preferably 0.2-0.5, the thickness is preferably 30-200nm, the cover layer is used for covering the quantum dots to form three-dimensional quantum restriction and avoiding the influence of a surface state on the optoelectronic properties of the quantum dots, and the preparation is finished.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method for preparing periodic array quantum dots by adopting a droplet etching epitaxial growth technology is characterized by comprising the following steps:
s1, arranging a substrate material, and cleaning the surface of the substrate material;
s2, growing a buffer layer on a substrate material, and growing an epitaxial layer on the buffer layer;
s3, preparing a periodic array of nano holes in the epitaxial layer through a nano patterned substrate process;
s4, performing hydrogen atom auxiliary deoxidation treatment on the epitaxial layer with the nano-cavities;
s5, positioning and depositing III-group metal liquid drops on the positions of the nanometer holes on the deoxidized epitaxial layer, and etching the metal liquid drops downwards at high temperature;
s6, filling quantum dot materials on the etched epitaxial layer;
and S7, growing a cover layer on the quantum dots and the epitaxial layer to finish the preparation.
2. The method of claim 1, wherein when the substrate material and the buffer layer are GaAs, the epitaxial layer and the cap layer are AlGaAs; when the substrate material and the buffer layer are InP, the epitaxial layer and the cover layer are InAlGaAs; when the substrate material and the buffer layer are GaSb, the epitaxial layer and the cover layer are AlGaSb.
3. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the thickness of the buffer layer is 100-600nm, and the buffer layer is used for flattening the surface of the substrate.
4. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the nanopatterned substrate process of the step S3 comprises: preparing the patterned substrate by an Atomic Force Microscope (AFM) local oxidation etching or nano-imprinting or electron beam direct writing process.
5. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the diameter of the nano-holes in step 3 is 20-90nm, and the depth is 4-30nm.
6. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the hydrogen atom assisted deoxidation treatment in the step 4 comprises the following specific steps: heating the substrate to 300-400 deg.C, heating the hydrogen cracker to 1400-1800 deg.C, opening hydrogen, and controlling the vacuum of the processing cavity to 1.0 × 10–7-2×10–7mbar, degassing for 20-40min.
7. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the step 5 of positioning and depositing the III group metal droplets on the surface of the epitaxial layer and etching the metal droplets downwards at a high temperature comprises the following specific steps: adjusting the temperature of the substrate to 550-700 ℃; introducing a group III metal beam, and controlling the introduction time of the group III metal beam to be 0.5-20s; the substrate temperature is raised to 600-700 ℃.
8. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed In claim 1, wherein the group III metal droplet adopted In the step 5 is one of Ga, in and Al.
9. The method of claim 1, wherein the quantum dot material of step 6 is GaAs, inAs, inGaAs, inGaAsP, gaSb or AlGaSb, the energy band of the quantum dot material is smaller than the band gaps of the epitaxial layer and the cap layer material, so as to realize three-dimensional confinement of carriers, and the lattice constant of the quantum dot material is close to that of the epitaxial layer and the cap layer, so as to reduce the stress for filling the quantum dot.
10. The method for preparing the periodic array quantum dots by adopting the droplet etching epitaxial growth technology as claimed in claim 1, wherein the thickness of the quantum dot material is 0.3-3nm; the epitaxial growth adopts molecular beam epitaxy or metal organic compound vapor deposition.
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