CN102254800A - Epitaxial growth method for gallium nitride (GaN)-based quantum dots - Google Patents
Epitaxial growth method for gallium nitride (GaN)-based quantum dots Download PDFInfo
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Abstract
The invention relates to an epitaxial growth method for gallium nitride (GaN)-based quantum dots. The method comprises the following steps of: sequentially epitaxially growing a buffer layer and a body material on a substrate material, introducing dislocation and/or an atom slip surface on the surface of the body material, and epitaxially growing the GaN-based quantum dots at the exposure positions of the dislocation and/or the atom slip surface. In the epitaxial growth method, an impregnation layer is not required and requirements on growth conditions and a growth process are relatively lower; and the epitaxial growth method is adapted to various substrate materials and has high application value for the preparation and utilization of the quantum dots.
Description
Technical field
The present invention relates to field of semiconductor materials, be specifically related to a kind of epitaxial growth method of GaN based quantum dot.
Background technology
When the de Broglie wavelength of the physical dimension of semi-conducting material and electronics can be compared, can produce quantum limitation effect, thereby make the band structure generation great variety of semi-conducting material.Quantum dot is a kind of semiconductor material structures that has quantum limit on three dimension scale, this makes quantum dot have the energy level and the energy state density of the separation of approximate single atom, so the quantum dot light emitting device has usually than body material and the higher radiation recombination efficient of quantum well devices.In addition, because quantum dot has the energy level and the energy state density of separation, make it be suitable for very much making single-photon source in the quantum communications.
The GaN based quantum dot can cover from ultraviolet near infrared wave-length coverage, and, make GaN radicle quanta point luminescent device have extraordinary temperature characterisitic with comparing with traditional devices based on the single-photon source of GaN based quantum dot because the GaN sill generally has than higher exciton binding energy.
Compare with the Si based quantum dot with GaAs, InP, the growth technology of GaN based quantum dot also is not very ripe.What generally adopt at present is the self assembly GaN based quantum dot that gas phase epitaxy of metal organic compound (MOCVD) or molecular beam epitaxy (MBE) are grown by the SK pattern.The SK pattern is a kind of two-dimensional growth pattern with soakage layer, growth conditions, growth technique, quality of materials all there are very harsh restriction, and can't accomplish relatively more unified and accurate control the position of the GaN based quantum dot that grows, size, density etc.
Report that local train that the place exists comes growth quantum point can to utilize material surface end of dislocation place or atom slip plane to appear in the Si/Ge system.The quantum dot that this mode is grown does not have soakage layer, and therefore better to the restriction of charge carrier, the temperature characterisitic of device is also better.
Summary of the invention
For overcoming the defective that needs soakage layer, method complexity in the prior art in the GaN based quantum dot epitaxial growth method, the purpose of this invention is to provide a kind of epitaxial growth method of GaN based quantum dot.
Said method is epitaxial growth buffer and a body material successively on backing material, introduces dislocation and/or atom slip plane on the surface of described body material, then at place's epitaxial growth GaN based quantum dot of appearing of described dislocation and/or atom slip plane.
The lateral dimension of described GaN based quantum dot is 1～200nm, and longitudinal size is 1～100nm, and density is 10
6～10
13Cm
-2Preferred widthwise measurement is 5～200nm, and longitudinal size is 2～50nm, and density is 10
8～10
10Cm
-2
The crystal structure of described quantum dot is wurtzite-type or zincblende type, can regulate by selecting suitable growth temperature, reative cell pressure and backing material structure.
Described growing method is metal-organic chemical vapor deposition equipment method (MOCVD), and growth temperature is 400～1000 ℃, and reative cell pressure is 1～1000mbar, and the preferred growth temperature is 500～800 ℃, and reative cell pressure is 10～100mbar.
Described growing method adopts alternately break-make source method or interruption of growth method.Wherein, alternately break-make source method is specially: only feed III clan source gas in a period of time, only feed group V source gas in following a period of time, alternately feed III, group V source gas so circularly, cycle period and number of times are determined by concrete growth parameter(s).The interruption of growth method is specially: feed III clan source gas and group V source gas simultaneously in a period of time, do not feed source gas in following a period of time, replace break-make source gas so circularly, cycle period and number of times are determined by concrete growth parameter(s).
Alternately break-make source method of the present invention fed nitrogenous source 5～15 seconds, repeatedly 20～80 cycles again for feeding metal organic source 1～5 second; Described interruption of growth method was interrupted 10～100 seconds for feeding metal organic source and nitrogenous source 1～3 minute, and then feeding metal organic source and nitrogenous source 1～3 minute.For above-mentioned two kinds of growing methods, in described scope, by adopting different source gas make-and-break time and make and break period, can change size, density and the emission wavelength of the quantum dot of being grown, as replacing in the method for break-make source, if the feeding time of nitrogenous source in each cycle of minimizing, then the size of Sheng Chang quantum dot is understood corresponding reducing, and density can increase; Increasing the make and break period number within the specific limits can increase the size of quantum dot, reduces the density of quantum dot.
Above-mentioned metal organic source is trimethyl gallium (TMGa), trimethyl indium (TMIn), trimethyl aluminium (TMA1), triethyl-gallium (TEGa), and nitrogenous source is ammonia (NH
3), the carrier gas of metal organic source is hydrogen (H
2) and nitrogen (N
2) mist.
The introducing method of described dislocation and/or atom slip plane is: at described body material surface deposition photoresist mask, making the body material surface form one or more areas by photoetching or electron beam exposure again is 0.1～5 μ m
2No masked areas, carry out etching in described no masked areas then and introduce dislocation and/or atom slip plane.
Described etching is inductively coupled plasma (ICP) dry etching.Described etching may introduce dislocation, atom slip plane any or its combination, dislocation kind wherein is unrestricted, comprises in helical dislocation, edge dislocation, the mixed dislocation one or more; The glide direction preferred parallel of described atom slip plane is in the direction of substrate surface, and such atom slip plane is appeared and located to be fit to more the epitaxial growth of quantum dot.
Described backing material is sapphire, SiC, InGaAlN, Si, GaAs or ZnO; Described resilient coating is GaN or AlN, and thickness is 50～200nm; Described body material is GaN or AlN, and thickness is 1～5 μ m.Backing material comprises wurtzite-type or zincblende type, selects according to the quantum-dot structure that will grow, and the epitaxial growth method of resilient coating, body material and condition adopt prior art to get final product.
Technical scheme of the present invention has been utilized GaN body material surface end of dislocation place and/or atom slip plane to appear and has been located the local train growing GaN based quantum dot of existence, appear the local train that the place exists of end of dislocation place and/or atom slip plane makes that the lattice constant of the local lattice constant of material and the quanta point material of being grown is more close, quantum dot is easier of these region growings, and described local train comprises tensile strain and compressive strain.
The introducing method of dislocation and/or atom slip plane is: at body material surface deposition one deck photoresist mask, preposition place on mask leaves the zone of similar window by photoetching or electron beam exposure, make the body material not have mask to cover at the window place, utilize etching method to introduce dislocation and/or atom slip plane by ion bombardment body material lattice, can produce the local STRESS VARIATION that helps Quantum Dots Growth at the place of appearing of these dislocations and/or atom slip plane at the body material surface at above-mentioned the window's position place.Photoetching and etching can realize the location or the introducing of semidefinite position of dislocation and/or atom slip plane.
Epitaxial growth method of the present invention need not soakage layer, utilize GaN body material surface end of dislocation place and/or atom slip plane to appear and locate the local train growing GaN based quantum dot of existence, its requirement to growth conditions and growth technique is lower, adapt to various sills, also can adopt the common molecular beam epitaxy in this area (MBE), hydride gas-phase epitaxy (HVPE) or metal-organic chemical vapor deposition equipment method (MOCVD) to carry out epitaxial growth.Utilize existing method such as photoetching or dry etching etc. can realize semidefinite position even the Quantum Dots Growth of locating fully, can accomplish better controlled position, size and the density of want Grown GaN based quantum dot.SEM (ESEM) and TEM (transmission electron microscope) test result (Fig. 1 and 2) show, the growth of the easier attraction in GaN body material surface end of dislocation place InGaN quantum dot.Epitaxial growth method of the present invention is with a wide range of applications for the utilization of quantum dot.
Description of drawings
Fig. 1 is an epitaxial growth method of the present invention at the appear schematic diagram of place's growing InGaN quantum dot of GaN body material surface edge dislocation;
Fig. 2 is an epitaxial growth method of the present invention in the appear SEM test result of place's growing InGaN quantum dot of GaN body material surface edge dislocation;
Fig. 3 is an epitaxial growth method of the present invention in the appear TEM test result of place's growing InGaN quantum dot of GaN body material surface edge dislocation.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
Adopt MOCVD epitaxial growth wurtzite-type InGaN quantum dot on Sapphire Substrate, its concrete growth course is:
1, Sapphire Substrate is put into the thick GaN resilient coating of MOCVD reative cell growth 100nm, temperature is 1150 ℃, and pressure is 50mbar.
2, growth 2 μ m GaN body materials, temperature is 1130 ℃, pressure is 400mbar.
3, from the MOCVD reative cell, take out epitaxial wafer.
4, at above-mentioned GaN body material surface deposition one deck photoresist mask, preposition place on mask leaves the square window that a length of side is about 1 μ m by photoetching, makes GaN body material not have mask to cover at the window place.
5, the GaN body material surface that utilizes ICP to be dry-etched in above-mentioned the window's position place is introduced dislocation and/or atom slip plane by ion bombardment body material lattice.
6, above-mentioned epitaxial wafer is put into the MOCVD reative cell once more.
7, adopt break-make source method alternately at the dislocation at above-mentioned window place and/or atom slip plane place's growth wurtzite-type InGaN quantum dot of appearing, temperature is 650 ℃, pressure is 50mbar, concrete growth step is as follows: the trimethyl indium and the triethyl-gallium that feed 3 seconds earlier in reative cell, in reative cell, feed 10 seconds ammonia again, so repeat 50 cycles.
8, reaction chamber temperature is reduced to room temperature, growth ending, and InGaN quantum dot lateral dimension is 100-150nm, longitudinal size is 10-20nm.Wherein, the edge dislocation of introducing is appeared the quantum dot of place growth shown in Fig. 2 and 3.
Embodiment 2
Adopt MOCVD epitaxial growth wurtzite-type InGaN quantum dot on Sapphire Substrate, its concrete growth course is:
1, Sapphire Substrate is put into the thick AlN resilient coating of MOCVD reative cell growth 100nm, temperature is 1150 ℃, and pressure is 50mbar.
2, growth 2 μ mAlN body materials, temperature is 1130 ℃, pressure is 400mbar.
3, from the MOCVD reative cell, take out epitaxial wafer.
4,,, make AlN body material not have mask to cover at the window place by photoetching preposition place on mask circular window that to leave a diameter be 1 μ m at above-mentioned AlN body material surface deposition one deck photoresist mask.
5, the AlN body material surface that utilizes ICP to be dry-etched in above-mentioned the window's position place is introduced dislocation and/or atom slip plane by ion bombardment body material lattice.
6, above-mentioned epitaxial wafer is put into the MOCVD reative cell once more.
7, adopt the interruption of growth method at the dislocation at above-mentioned window place and/or atom slip plane place's growth wurtzite-type InGaN quantum dot of appearing, temperature is 650 ℃, pressure is 50mbar, concrete growth step is as follows: the trimethyl indium, triethyl-gallium and the ammonia that feed 1 minute earlier in reative cell, wait for 20 seconds, in reative cell, feed 1 minute trimethyl indium, triethyl-gallium and ammonia again.
8, reaction chamber temperature is reduced to room temperature, and growth ending, quantum dot lateral dimension are 50-100nm, and longitudinal size is 20-40nm.
Embodiment 3
Adopt MOCVD epitaxial growth wurtzite-type AlGaN quantum dot on Sapphire Substrate, its concrete growth course is:
1, Sapphire Substrate is put into the thick AlN resilient coating of MOCVD reative cell growth 100nm, temperature is 1150 ℃, and pressure is 50mbar.
2, growth 2 μ m AlN body materials, temperature is 1130 ℃, pressure is 400mbar.
3, from the MOCVD reative cell, take out epitaxial wafer.
4,,, make AlN body material not have mask to cover at the window place by electron beam exposure preposition place on mask square window that to leave a length of side be 1 μ m at above-mentioned AlN body material surface deposition one deck photoresist mask.
5, the AlN body material surface that utilizes ICP to be dry-etched in above-mentioned the window's position place is introduced dislocation and/or atom slip plane by ion bombardment body material lattice.
6, above-mentioned epitaxial wafer is put into the MOCVD reative cell once more.
7, adopt break-make source method alternately at the dislocation at above-mentioned window place and/or atom slip plane place's growth wurtzite-type AlGaN quantum dot of appearing, temperature is 650 ℃, pressure is 50mbar, concrete growth step is as follows: the trimethyl aluminium and the triethyl-gallium that feed 3 seconds earlier in reative cell, in reative cell, feed 10 seconds ammonia again, so repeat 50 cycles.
8, reaction chamber temperature is reduced to room temperature, and growth ending, quantum dot lateral dimension are 150-200nm, and longitudinal size is 10-40nm.
Embodiment 4
Adopt MOCVD epitaxial growth wurtzite-type InGaN quantum dot on wurtzite-type ZnO substrate, its concrete growth course is:
1, the ZnO substrate is put into the thick GaN resilient coating of MOCVD reative cell growth 50nm, temperature is 1200 ℃, and pressure is 50mbar.
2, growth 5 μ m GaN body materials, temperature is 1130 ℃, pressure is 400mbar.
3, from the MOCVD reative cell, take out epitaxial wafer.
4, at above-mentioned GaN body material surface deposition one deck photoresist mask, preposition place on mask leaves the square window that some length of sides are 1-1.5 μ m by photoetching, makes GaN body material not have mask to cover at the window place.
5, the GaN body material surface that utilizes ICP to be dry-etched in above-mentioned the window's position place is introduced dislocation and/or atom slip plane by ion bombardment body material lattice.
6, above-mentioned epitaxial wafer is put into the MOCVD reative cell once more.
7, adopt break-make source method alternately at the dislocation at above-mentioned window place and/or the atom slip plane place's growing InGaN quantum dot of appearing, temperature is 750 ℃, pressure is 20mbar, concrete growth step is as follows: the trimethyl indium and the triethyl-gallium that feed 3 seconds earlier in reative cell, in reative cell, feed 10 seconds ammonia again, so repeat 50 cycles.
8, reaction chamber temperature is reduced to room temperature, and growth ending, quantum dot lateral dimension are 80-150nm, and longitudinal size is 10-30nm, and averag density is about 10
8Cm
-2
Embodiment 5
Adopt MOCVD epitaxial growth zincblende type InGaN quantum dot on zincblende type GaAs substrate, its concrete growth course is:
1, the GaAs substrate is put into the thick AlN resilient coating of MOCVD reative cell growth 150nm, temperature is 1150 ℃, and pressure is 50mbar.
2, growth 2 μ m A1N body materials, temperature is 1130 ℃, pressure is 400mbar.
3, from the MOCVD reative cell, take out epitaxial wafer.
4, at above-mentioned AlN body material surface deposition one deck photoresist mask, leaving some diameters at preposition place on the mask by photoetching is circular window between the 0.1-2 μ m, makes AlN body material not have mask to cover at the window place.
5, the AlN body material surface that utilizes ICP to be dry-etched in above-mentioned the window's position place is introduced dislocation and/or atom slip plane by ion bombardment body material lattice.
6, above-mentioned epitaxial wafer is put into the MOCVD reative cell once more.
7, adopt the interruption of growth method at the dislocation at above-mentioned window place and/or atom slip plane place's growth zincblende type InGaN quantum dot of appearing, temperature is 500 ℃, pressure is 100mbar, concrete growth step is as follows: the trimethyl indium, triethyl-gallium and the ammonia that feed 2 minutes earlier in reative cell, wait for 90 seconds, in reative cell, feed 2 minutes trimethyl indium, triethyl-gallium and ammonia again.
8, reaction chamber temperature is reduced to room temperature, and growth ending, quantum dot lateral dimension are 30-100nm, and longitudinal size is 10-40nm, and averag density is about 10
10Cm
-2
Embodiment 6
Step 1-6 is with embodiment 1.
7, adopt break-make source method alternately at the dislocation at above-mentioned window place and/or atom slip plane place's growth wurtzite-type InGaN quantum dot of appearing, temperature is 650 ℃, pressure is 50mbar, concrete growth step is as follows: the trimethyl indium and the triethyl-gallium that feed 3 seconds earlier in reative cell, in reative cell, feed 8 seconds ammonia again, so repeat 50 cycles.
8, reaction chamber temperature is reduced to room temperature, growth ending, and InGaN quantum dot lateral dimension is 60-100nm, longitudinal size is 10-15nm.
Embodiment 7
Step 1-6 is with embodiment 4.
7, adopt break-make source method alternately at the dislocation at above-mentioned window place and/or the atom slip plane place's growing InGaN quantum dot of appearing, temperature is 750 ℃, pressure is 20mbar, concrete growth step is as follows: the trimethyl indium and the triethyl-gallium that feed 5 seconds earlier in reative cell, in reative cell, feed 10 seconds ammonia again, so repeat 80 cycles.
8, reaction chamber temperature is reduced to room temperature, and growth ending, quantum dot lateral dimension are 120-160nm, and longitudinal size is 20-50nm, and averag density is about 10
7Cm
-2
Though above used general explanation, embodiment and experiment, the present invention is described in detail, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the epitaxial growth method of a GaN based quantum dot, epitaxial growth buffer and body material successively on backing material, it is characterized in that, dislocation and/or atom slip plane are introduced in surface at described body material, locate epitaxial growth GaN based quantum dot appearing of described dislocation and/or atom slip plane then.
2. growing method according to claim 1 is characterized in that, the lateral dimension of described GaN based quantum dot is 1～200nm, and longitudinal size is 1～100nm, and density is 10
6～10
13Cm
-2Preferred widthwise measurement is 5～200nm, and longitudinal size is 2～50nm, and density is 10
8～10
10Cm
-2
3. growing method according to claim 2 is characterized in that, described GaN based quantum dot is wurtzite-type quantum dot or zincblende type quantum dot.
4. growing method according to claim 1, it is characterized in that, described epitaxial growth method is the metal-organic chemical vapor deposition equipment method, growth temperature is 400～1000 ℃, reative cell pressure is 1～1000mbar, the preferred growth temperature is 500～800 ℃, and reative cell pressure is 10～100mbar.
5. growing method according to claim 4 is characterized in that, described epitaxial growth method adopts alternately break-make source method or interruption of growth method; Described alternately break-make source method fed nitrogenous source 5～15 seconds, repeatedly 20～80 cycles again for feeding metal organic source 1～5 second; Described interruption of growth method was interrupted 10～100 seconds for feeding metal organic source and nitrogenous source 1～3 minute, and then feeding metal organic source and nitrogenous source 1～3 minute.
6. according to claim 4 or 5 described growing methods, it is characterized in that described metal organic source is trimethyl gallium, trimethyl indium, trimethyl aluminium, triethyl-gallium, described nitrogenous source is an ammonia, and the carrier gas of described metal organic source is the mist of hydrogen and nitrogen.
7. growing method according to claim 1, it is characterized in that, the introducing method of described dislocation and/or atom slip plane is: at described body material surface deposition photoresist mask, making the body material surface form one or more areas by photoetching or electron beam exposure again is 0.1～5 μ m
2No masked areas, carry out etching in described no masked areas then and introduce dislocation and/or atom slip plane.
8. growing method according to claim 7 is characterized in that, described etching is the inductively coupled plasma dry etching.
9. according to claim 7 or 8 described growing methods, it is characterized in that described dislocation is one or more in helical dislocation, edge dislocation, the mixed dislocation; The glide direction of described atom slip plane is parallel to the direction of substrate surface.
10. growing method according to claim 1 is characterized in that, described backing material is sapphire, SiC, InGaAlN, Si, GaAs or ZnO; Described resilient coating is GaN or AlN, and thickness is 50～200nm; Described body material is GaN or AlN, and thickness is 1～5 μ m.
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| CN103187498A (en) * | 2011-12-29 | 2013-07-03 | 比亚迪股份有限公司 | Semiconductor structure and forming method thereof |
| CN111188027A (en) * | 2020-02-12 | 2020-05-22 | 南京大学 | Chemical vapor deposition equipment and film forming method |
| CN112530791A (en) * | 2020-12-03 | 2021-03-19 | 清华大学 | Method for growing high-density indium gallium nitrogen quantum dots |
| CN113113287A (en) * | 2021-03-29 | 2021-07-13 | 清华大学 | Indium gallium nitrogen quantum dot and preparation method and application thereof |
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Cited By (6)
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| CN111188027B (en) * | 2020-02-12 | 2021-08-03 | 南京大学 | Chemical vapor deposition equipment and film forming method |
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| CN113113287A (en) * | 2021-03-29 | 2021-07-13 | 清华大学 | Indium gallium nitrogen quantum dot and preparation method and application thereof |
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Application publication date: 20111123 |