CN106384762A - Nano-pillar LED grown on strontium tantalum lanthanum aluminate substrate and preparation method thereof - Google Patents
Nano-pillar LED grown on strontium tantalum lanthanum aluminate substrate and preparation method thereof Download PDFInfo
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- CN106384762A CN106384762A CN201610931958.1A CN201610931958A CN106384762A CN 106384762 A CN106384762 A CN 106384762A CN 201610931958 A CN201610931958 A CN 201610931958A CN 106384762 A CN106384762 A CN 106384762A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
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- H—ELECTRICITY
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- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/04—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier 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
- H01L33/12—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 stress relaxation structure, e.g. buffer layer
Abstract
The invention belongs to the technical field of nano-pillar LED preparation, and discloses a nano-pillar LED grown on a strontium tantalum lanthanum aluminate substrate and a preparation method thereof. The nano-pillar LED grown on a strontium tantalum lanthanum aluminate substrate comprises a strontium tantalum lanthanum aluminate substrate, an AlN nucleation layer grown on the strontium tantalum lanthanum aluminate substrate, a GaN nano-pillar template grown on the AlN nucleation layer, an AlN/GaN super lattice layer grown on the GaN nano-pillar template, a non-doped GaN layer grown on the AlN/GaN super lattice layer, an n-type doped GaN layer grown on the non-doped GaN layer, an InGaN/GaN quantum well grown on the n-type doped GaN layer, and a p-type doped GaN layer grown on the InGaN/GaN quantum well. The substrate material is of low cost. A nano-pillar array prepared is size-controllable and of uniform orientation. The obtained nano-pillar LED has low defect density and excellent electrical and optical properties.
Description
Technical field
The present invention relates to nano-array LED growth and preparation field, particularly to being grown in strontium aluminate tantalum lanthanum
(La0.3Sr1.7AlTaO6) nano-pillar LED on substrate and preparation method thereof.
Background technology
The group III-nitride of GaN and its correlation has extremely excellent property in electricity, optics and acoustically,
It is widely used in and prepare the devices such as light emitting diode (LEDs), laser diode (LDs) and field-effect transistor.In recent years
Come, GaN base nano-pillar LED has potential LED structure and receives much concern as a kind of, this be due to planar structure LED phase
Nano-pillar LED first has high surface to volume ratio (area/volume) to ratio, can significantly reduce threading dislocation density；Secondly, nanometer
Post LED can increase substantially the light extraction efficiency of LED, realizes the coupling outgoing of light；Finally can be by controlling the chi of nano-pillar LED
Very little, change the emission wavelength of nano-pillar LED, prepare multicolor luminous nano-pillar LED of single-chip, for realizing inexpensive white light
The preparation of LED opens new road.
The growing method of GaN nano-pillar mainly has catalyst method, no catalyst method, selective area growth method at present.Catalyst method
Vapor liquid solid (VLS) growth mechanism with Au, Pt, Ni etc. for catalyst inducement GaN, makes gas reactant dissolve in
In the catalytic metal drop of nano-scale, grow into nano crystal post or line because of supersaturation.But catalyst method is difficult to control to
The nucleation density of GaN nano-pillar, arrangement situation and crystal mass.Meanwhile, catalyst can during extension as impurity simultaneously
Enter in epitaxial material, substantially reduce the electrical and optical properties of device.No catalyst method passes through to control suitable growth conditionss, bag
Include the application homepitaxy growth GaN nano-pillar of V/III and cushion.Although the self assembly GaN nano-pillar of this method growth
No catalyst contamination, crystal mass is high, but due to lacking positioning and the induction of catalyst, nano-pillar distribution lacks rule and chi
Very little difficult control, lack of homogeneity.Selective area growth method is to be turned the homogeneous reticle pattern of artificial design by ripe etching technics
Move to epitaxial layer, the growth for nano-pillar provides the nucleation site being evenly distributed, and is conducive to manufactured size controlled and is uniformly distributed
Nano-pillar LED.Therefore, size is controlled to select suitable growing technology to prepare, and the homogeneous nano column array of orientation has important
Meaning.
To improve the performance of nano-pillar LED further, another severe challenge being also faced with is that business-like LED is main
It is epitaxially grown on a sapphire substrate, sapphire is high with the lattice mismatch of GaN and thermal mismatching, leads to shape in GaN nano-pillar
Becoming very high dislocation density, thus reducing the carrier mobility of material, finally have impact on the performance of device.
La0.3Sr1.7AlTaO6Substrate is only 0.1% and 3.6% respectively with the lattice mismatch of GaN and thermal mismatching, is that extension GaN most preferably serves as a contrast
One of bottom.But La0.3Sr1.7AlTaO6Unstable chemcial property under substrate high temperature, La therefore to be made0.3Sr1.7AlTaO6Receive on substrate
Rice post LED really can realize large-scale application, needs to find La0.3Sr1.7AlTaO6The new side of Grown nano-pillar LED
Method and technique.
Content of the invention
In order to overcome disadvantages mentioned above and the deficiency of prior art, it is an object of the invention to provide one kind is grown in strontium aluminate
Nano-pillar LED on tantalum lanthanum substrate and preparation method, selected strontium aluminate tantalum lanthanum backing material is with low cost, and prepared receives
Rice post array sizes are controlled, and orientation is homogeneous, and the defect concentration of nano-pillar LED being obtained is low, electrical and optical function admirable.
The purpose of the present invention is achieved through the following technical solutions：
It is grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate, including La0.3Sr1.7AlTaO6Substrate, is grown in
La0.3Sr1.7AlTaO6AlN nucleating layer on substrate, is grown in the GaN nanometer column template on AlN nucleating layer, is grown in GaN and receives
AlN/GaN superlattice layer on rice column template, is grown in the undoped GaN layer on AlN/GaN superlattice layer, is grown in undoped
N-shaped doped gan layer in GaN layer, is grown in the InGaN/GaN SQW in N-shaped doped gan layer, is grown in InGaN/GaN amount
P-type doped gan layer on sub- trap.
Described GaN nanometer column template is GaN nano column array, and described GaN nanometer column template is by being grown in AlN nucleating layer
On GaN cushion pass through TracePro software optimization nano-pillar arrange, then using nanometer embossing and lithographic technique preparation
Form.
Described La0.3Sr1.7AlTaO6Substrate is with (111) face 0.5～1 ° of (100) direction partially as epitaxial surface；Crystalline epitaxial takes
To relation it is：(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111) face.
The thickness of described AlN nucleating layer is 100～200nm；The height of described GaN nanometer column template is 500～1000nm,
A diameter of 100～200nm, adjacent spacing is 150～250nm.
Described AlN/GaN superlattice layer is the AlN layer/GaN layer in 15～25 cycles, and gross thickness is 30～100nm, its
The thickness of middle AlN layer is 1～2nm, and the thickness of GaN layer is 1～2nm.
The thickness of undoped GaN layer is 200～300nm；The thickness of N-shaped doped gan layer is 2～4 μm；InGaN/GaN measures
Sub- trap is the InGaN well layer/GaN barrier layer in 8～13 cycles, and wherein the thickness of InGaN well layer is 3～5nm, the thickness of GaN barrier layer
Spend for 10～15nm；The thickness of p-type doped gan layer is 300～350nm.
Described AlN nucleating layer is to realize low temperature (temperature is 450～550 DEG C) using pulsed laser deposition (PLD) technology
Lower epitaxial growth, can effectively alleviate La0.3Sr1.7AlTaO6Unstable under substrate high temperature, there is serious boundary and cushion between
The problem of face reaction.
Described nanometer column template passes through using the arrangement of TracePro software optimization nano-pillar, using nanometer embossing slow
Rush preparation, the nano column array size uniform being obtained on layer, then prepared nanometer column template is transferred to metal organic
Carry out the preparation of nano-pillar LED by selective area growth in Vapor Deposition reaction chamber (MOCVD).
Described nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate, also includes sealing coat, described isolation is deposited upon
The side wall of GaN nanometer column template and not by the AlN nucleating layer of GaN nanometer column template.Described separation layer thickness is 10～50nm.
The material of described sealing coat is SiNx、SiO2Or Al2O3.
The preparation method of described nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate, comprises the following steps：
(1) selection of substrate and its crystal orientation：Using La0.3Sr1.7AlTaO6Substrate, with (111) face (100) direction partially
0.5～1 ° is epitaxial surface, and crystalline epitaxial orientation relationship is：(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111)
Face；
(2) substrate surface polishes, cleans and makes annealing treatment, and the detailed process of described annealing is：Place the substrate into annealing
Interior, to La in air atmosphere at 800～900 DEG C0.3Sr1.7AlTaO6Substrate carries out making annealing treatment 3～5 hours and then air cooling
To room temperature；
(3) AlN nucleation layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 450～550 DEG C, in the pressure of reative cell
Power is 6.0 × 10-3Torr, the speed of growth are growth 100～200nm thickness AlN nucleating layer under conditions of 0.2～0.3ML/s；
(4) GaN buffering layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 650～850 DEG C, in the pressure of reative cell
Power is 6.0 × 10-3Torr, the speed of growth, for growing GaN cushion on AlN nucleating layer under conditions of 0.4～0.6ML/s, are delayed
Rushing thickness degree is 500～1000nm；
(5) nanometer embossing etching GaN nanometer column template：By being arranged using TracePro software optimization nano-pillar,
Using nanometer embossing and dry etch process, GaN cushion is etched downwards, obtaining GaN nano column array is GaN
Nanometer column template, the height of nano-pillar is 500～1000nm, a diameter of 100～200nm, and adjacent spacing is 150～250nm；
(6) layer deposited isolating：Using chemical vapor deposition, ald or magnetron sputtering technique in GaN nano-pillar mould
Layer deposited isolating on the side wall of plate and the AIN nucleating layer that do not covered by nano-pillar, the material of described sealing coat is SiNx、SiO2Or
Person Al2O3, thickness is 10～50nm；
(7) epitaxial growth of AlN/GaN superlattice layer：GaN nanometer column template is transferred in MOCVD, room temperature will be reacted
Degree be maintained at 650～850 DEG C, reative cell pressure be 150～200Torr under the conditions of, on GaN nanometer column template (not by
The nanometer column top of sealing coat deposition) 15～25 cycle AlN/GaN superlattice layers of growth, 30～100nm's, wherein AlN layer
Thickness is 1～2nm, and the thickness of GaN layer is 1～2nm；
(8) epitaxial growth of undoped GaN layer：Reaction chamber temperature is maintained at 1000～1300 DEG C, in the pressure of reative cell
Under the conditions of power is 150～200Torr, undoped GaN layer is grown on the AlN/GaN superlattice layer that step (7) obtains, thickness is
200～300nm；
(9) epitaxial growth of N-shaped doped gan layer：Reaction chamber temperature is risen to 1000～1500 DEG C, in chamber pressure is
Under the conditions of 150～200Torr, growing n-type doped gan layer in the undoped GaN layer that step (8) obtains, doping content be 3 ×
1018～9 × 1018cm-3, thickness be 2～4 μm；
(10) epitaxial growth of InGaN/GaN MQW：Reaction chamber temperature is reduced to 700～780 DEG C, in reative cell
Under the conditions of pressure is 150～200Torr, it is passed through ammonia, nitrogen, trimethyl gallium and trimethyl indium, the N-shaped obtaining in step (9)
InGaN/GaN MQW is grown, InGaN/GaN SQW is the InGaN well layer/GaN in 8～13 cycles in doped gan layer
Barrier layer, the wherein thickness of InGaN well layer are 3～5nm, and the thickness of GaN barrier layer is 10～15nm；
(11) epitaxial growth of p-type doped gan layer：Reaction chamber temperature is increased to 900～1100 DEG C, in the pressure of reative cell
Under the conditions of 150～200Torr, it is passed through two luxuriant magnesium, ammonia, nitrogen and trimethyl gallium, the InGaN/GaN obtaining in step (10)
P-type doped gan layer is grown on MQW, doping content is 3 × 1017～9 × 1017cm-3, thickness is 300～350nm.
In the epitaxial growth of the described AlN/GaN superlattice layer of step (7), Al source is TMAl；Nitrogen source is NH3；Ga source is
TMGa；Nitrogen source is NH3；The flow in each source is silicon source 150～300sccm, gallium source 125～175sccm, nitrogen source 25～35slm；
In the epitaxial growth of the described undoped GaN layer of step (8), Ga source is TMGa；Nitrogen source is NH3；
In the epitaxial growth of the described N-shaped doped gan layer of step (9), doped source is silane；Ga source is TMGa；Nitrogen source is NH3；
The flow in each source is Ga source 350～450sccm, nitrogen source 50～65slm, doped source 100～200sccm；
In step (10) flow in each source be indium source 450～550sccm, gallium source 100～150sccm, nitrogen source 25～
35slm；In step (11) flow in each source be Ga source 350～450sccm, nitrogen source 50～65slm, doped source 150～
250sccm.
Described substrate surface polishing, specially：First by La0.3Sr1.7AlTaO6Substrate surface is carried out with diamond mud
Polishing, coordinates observation by light microscope substrate surface, after not having cut, then is thrown using the method for chemically mechanical polishing
Optical processing.
Described cleaning, specially：By La0.3Sr1.7AlTaO6Substrate is put into and is cleaned by ultrasonic 3～5 under room temperature in deionized water
Minute, remove La0.3Sr1.7AlTaO6Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface
Organic substance, is dried up with drying nitrogen.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) present invention uses La0.3Sr1.7AlTaO6As substrate, La0.3Sr1.7AlTaO6Substrate is readily available, and price is just
Preferably, advantageously reduce production cost.
(2) present invention adopts nanometer embossing to obtain high-quality nanometer column template, is then transferred to nanometer column template
MOCVD carries out the preparation of nano-pillar LED epitaxial material by selective area growth.Both reduced the growth difficulty of nano-pillar LED, disappeared again
Except introducing the harmful effect of impurity using catalyst, be conducive to acquisition size controlled, be orientated homogeneous high-quality nano-pillar
LED.
(3) present invention takes full advantage of the respective advantage of PLD and MOCVD：Exist first by PLD technology
La0.3Sr1.7AlTaO6The first epitaxial growth of nucleation layers of (450-550 DEG C) of low temperature is adopted on substrate, successfully suppresses interfacial reaction, under being
The nano column array that one step prepares high-quality low defect carries out place mat；It is subsequently transferred to MOCVD high temperature extension u-GaN, n-
GaN, P-GaN and SQW etc., have given full play to the advantage of MOCVD, improve growth rate and production capacity.
(4) present invention is using the La low with GaN lattice mismatch and thermal mismatching degree0.3Sr1.7AlTaO6(111) as substrate,
Thermal stress can be efficiently reduced, reduce the formation of dislocation, prepare high-quality nano-pillar LED epitaxial material, favorably improve
The radiation recombination efficiency of carrier, can increase substantially nitride device such as semiconductor laser, light emitting diode and solar energy
The luminous efficiency of battery.
Brief description
Fig. 1 is the sectional view of nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate of the present invention；
Fig. 2 is the structural representation that GaN nano column array prepared by embodiment 1 is GaN nanometer column template；
Fig. 3 is luminescence generated by light (PL) collection of illustrative plates of nano-pillar LED of embodiment 1 preparation.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
The sectional view of nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate of the present invention is as shown in figure 1, include
La0.3Sr1.7AlTaO6Substrate, is grown in La0.3Sr1.7AlTaO6AlN nucleating layer 11 on substrate 10, is grown in AlN nucleating layer 11
On GaN nanometer column template 12 (i.e. GaN nano column array is will to be grown on AlN nucleating layer through nanometer embossing
GaN cushion etching forms), be deposited on GaN nanometer column template 12 side wall and the AlN nucleating layer 11 that do not covered by nano-pillar every
Absciss layer 13, is grown in the AlN/GaN superlattices 14 on GaN nanometer column template 12, and be grown on AlN/GaN superlattices 14 non-mixes
Miscellaneous GaN layer 15, is grown in the N-shaped doped gan layer 16 in undoped GaN layer 15, is grown in N-shaped doped gan layer 16
InGaN/GaN SQW 17, is grown in the p-type doped gan layer 18 on InGaN/GaN SQW 17.
The thickness of described AlN nucleating layer is 100～200nm；The height of described GaN nanometer column template is 500～1000nm,
A diameter of 100～200nm, adjacent spacing is 150～250nm.
Described AlN/GaN superlattice layer is the AlN layer/GaN layer in 15～25 cycles, and gross thickness is 30～100nm, its
The thickness of middle AlN layer is 1～2nm, and the thickness of GaN layer is 1～2nm.
The thickness of undoped GaN layer is 200～300nm；The thickness of N-shaped doped gan layer is 2～4 μm；InGaN/GaN measures
Sub- trap is the InGaN well layer/GaN barrier layer in 8～13 cycles, and wherein the thickness of InGaN well layer is 3～5nm, the thickness of GaN barrier layer
Spend for 10～15nm；The thickness of p-type doped gan layer is 300～350nm.Described separation layer thickness is 10～50nm.
Embodiment 1
The preparation method of nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate of the present embodiment, comprises the following steps：
(1) selection of substrate and its crystal orientation：Using La0.3Sr1.7AlTaO6Substrate, with (111) face (100) direction partially
0.5～1 ° is epitaxial surface, and crystalline epitaxial orientation relationship is：(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111)
Face；
(2) substrate surface polishes, cleans and makes annealing treatment, and the detailed process of described annealing is：Place the substrate into annealing
Interior, to La in air atmosphere at 850 DEG C0.3Sr1.7AlTaO6Substrate carries out making annealing treatment 3 hours and then being air cooled to room temperature；
Described substrate surface polishing, specially：First by La0.3Sr1.7AlTaO6Substrate surface is carried out with diamond mud
Polishing, coordinates observation by light microscope substrate surface, after not having cut, then is thrown using the method for chemically mechanical polishing
Optical processing；
Described cleaning, specially：By La0.3Sr1.7AlTaO6Substrate is put into and is cleaned by ultrasonic 3 points under room temperature in deionized water
Clock, removes La0.3Sr1.7AlTaO6Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, removing surface has
Machine thing, is dried up with drying nitrogen；
(3) AlN nucleation layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 500 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth are growth 100nm thickness AlN nucleating layer under conditions of 0.3ML/s；Al source is AlN target, nitrogen source
For high-purity plasma nitrogen, substrate rotating speed is 5Rad/s, and target-substrate distance is 5cm, laser wave in pulsed laser deposition (PLD) simultaneously
A length of 248nm, laser energy is 220mJ, and frequency is 10Hz, and the plasma flow of nitrogen is 5sccm；
(4) GaN buffering layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 700 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth for growing GaN cushion, buffer layer thickness under conditions of 0.6ML/s on AlN nucleating layer are
1000nm；Ga source is GaN target, and nitrogen source is high-purity plasma nitrogen, and substrate rotating speed is 5Rad/s, and target-substrate distance is 5cm, simultaneously
In pulsed laser deposition (PLD), optical maser wavelength is 248nm, and laser energy is 220mJ, and frequency is 10Hz, the plasma stream of nitrogen
Measure as 5sccm；
(5) nanometer embossing etching nanometer column template：By using the arrangement of TracePro software optimization nano-pillar, utilizing
Nanometer embossing and dry etch process are to La0.3Sr1.7AlTaO6On substrate, GaN cushion is etched downwards, and etching is high
Spend the GaN nano column array for 1000nm, its a diameter of 200nm, adjacent spacing is 250nm；
(6) nano-pillar sidewall spacers are deposited：Existed using chemical vapor deposition, ald or magnetron sputtering technique
Layer deposited isolating on GaN nano column array side wall and the AlN nucleating layer that do not covered by nano-pillar, described nano-pillar sidewall spacers
Material be SiNx, thickness is 10nm；
(7) epitaxial growth of AlN/GaN superlattice layer：The GaN preparing nano column array is transferred in MOCVD, will
Reaction chamber temperature is maintained at 750 DEG C, under the conditions of the pressure of reative cell is 150Torr, the GaN nano-pillar that obtains in step (6)
20 cycle AlN/GaN superlattice layers, AlN thickness degree 1nm are grown on array；GaN layer thickness 1nm, gross thickness is 40nm；Al source
For TMAl；Nitrogen source is NH3；Ga source is TMGa；Nitrogen source is NH3；The flow in each source is silicon source 150～300sccm, gallium source 125～
175sccm, nitrogen source 25～35slm；
(8) epitaxial growth of undoped GaN layer：Reaction chamber temperature is maintained at 1100 DEG C, in the pressure of reative cell is
Under the conditions of 150Torr, undoped GaN layer is grown on the AlN/GaN superlattice structure that step (7) obtains, thickness is 200nm；
Ga source is TMGa；Nitrogen source is NH3；
(9) epitaxial growth of N-shaped doped gan layer：Reaction chamber temperature is risen to 1400 DEG C, in chamber pressure is
Under the conditions of 150Torr, growing n-type doped gan layer in the undoped GaN layer that step (8) obtains, doping content be 3 ×
1018cm-3, thickness be 2 μm；Doped source is silane；Ga source is TMGa；Nitrogen source is NH3；The flow in each source be Ga source 350～
450sccm, nitrogen source 50～65slm, doped source 100～200sccm；
(10) epitaxial growth of InGaN/GaN MQW：Reaction chamber temperature is reduced to 720 DEG C, in the pressure of reative cell
Under the conditions of 150Torr, it is passed through ammonia, nitrogen, trimethyl gallium and trimethyl indium, the N-shaped doped gan layer obtaining in step (9)
Upper growth InGaN/GaN MQW, InGaN/GaN SQW is the InGaN well layer/GaN barrier layer, wherein InGaN in 8 cycles
The thickness of well layer is 3nm, and the thickness of GaN barrier layer is 10nm；The flow in each source is indium source 450～550sccm, gallium source 100～
150sccm, nitrogen source 25～35slm；
(11) epitaxial growth of p-type doped gan layer：Reaction chamber temperature is increased to 900 DEG C, in the pressure of reative cell is
Under the conditions of 150Torr, it is passed through two luxuriant magnesium, ammonia, nitrogen, trimethyl gallium, the InGaN/GaN MQW obtaining in step (10)
Upper growth p-type doped gan layer, doping content is 3 × 1017cm-3, thickness is 300nm；The flow in each source be Ga source 350～
450sccm, nitrogen source 50～65slm, doped source 150～250sccm.
The structural representation of the GaN nano-array being etched on GaN cushion in the present embodiment is as shown in Figure 2.
The PL spectrum of nano-pillar LED that the present embodiment is prepared is as shown in figure 3, test shows the luminescence generated by light of SQW
Peak position in 450nm, a width of 23.0nm of half-peak, show that this LED has preferable photoelectric properties, be the reason preparing efficient LED devices
Think material.
Embodiment 2
The preparation method of nano-pillar LED being grown on strontium aluminate tantalum lanthanum substrate of the present embodiment, comprises the following steps：
(1) selection of substrate and its crystal orientation：Using La0.3Sr1.7AlTaO6Substrate, with (111) face (100) direction partially
0.5～1 ° is epitaxial surface, and crystalline epitaxial orientation relationship is：(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111)
Face；
(2) substrate surface polishes, cleans and makes annealing treatment, and the detailed process of described annealing is：Place the substrate into annealing
Interior, to La in air atmosphere at 800 DEG C0.3Sr1.7AlTaO6Substrate carries out making annealing treatment 5 hours and then being air cooled to room temperature；
Described substrate surface polishing, specially：First by La0.3Sr1.7AlTaO6Substrate surface is carried out with diamond mud
Polishing, coordinates observation by light microscope substrate surface, after not having cut, then is thrown using the method for chemically mechanical polishing
Optical processing；
Described cleaning, specially：By La0.3Sr1.7AlTaO6Substrate is put into and is cleaned by ultrasonic 5 points under room temperature in deionized water
Clock, removes La0.3Sr1.7AlTaO6Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, removing surface has
Machine thing, is dried up with drying nitrogen；
(3) AlN nucleation layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 450 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth are growth 200nm thickness AlN nucleating layer under conditions of 0.2ML/s；Al source is AlN target, nitrogen source
For high-purity plasma nitrogen, substrate rotating speed is 8Rad/s, and target-substrate distance is 10cm, laser in pulsed laser deposition (PLD) simultaneously
Wavelength is 248nm, and laser energy is 250mJ, and frequency is 20Hz, and the plasma flow of nitrogen is 10sccm；
(4) GaN buffering layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 800 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth for growing GaN cushion, buffer layer thickness under conditions of 0.5ML/s on AlN nucleating layer are
1000nm；Ga source is GaN target, and nitrogen source is high-purity plasma nitrogen, and substrate rotating speed is 8Rad/s, and target-substrate distance is 10cm, with
When pulsed laser deposition (PLD) in optical maser wavelength be 248nm, laser energy is 250mJ, and frequency is 20Hz, the plasma of nitrogen
Flow is 10sccm；
(5) nanometer embossing etching nanometer column template：By using the arrangement of TracePro software optimization nano-pillar, utilizing
Nanometer embossing and dry etch process are etched downwards to GaN cushion on AlN nucleating layer, and etching height is 1000nm
GaN nano column array, its a diameter of 100nm, spacing be 150nm；
(6) nano-pillar sidewall spacers are deposited：Existed using chemical vapor deposition, ald or magnetron sputtering technique
One layer of nano-pillar sidewall spacers of AlN nano column array surrounding growth, the material of described nano-pillar sidewall spacers is SiO2, thick
Spend for 50nm；
(7) epitaxial growth of AlN/GaN superlattice layer：The GaN preparing nano column array is transferred in MOCVD, will
Reaction chamber temperature is maintained at 750 DEG C, under the conditions of the pressure of reative cell is 200Torr, the GaN nano-pillar that obtains in step (6)
20 cycle AlN/GaN superlattice layers, AlN thickness degree 1nm are grown on array；GaN layer thickness 1nm, gross thickness is 40nm；Al source
For TMAl；Nitrogen source is NH3；Ga source is TMGa；Nitrogen source is NH3；The flow in each source is silicon source 150～300sccm, gallium source 125～
175sccm, nitrogen source 25～35slm；
(8) epitaxial growth of undoped GaN layer：Reaction chamber temperature is maintained at 1100 DEG C, in the pressure of reative cell is
Under the conditions of 200Torr, undoped GaN layer is grown on the AlN/GaN superlattice structure that step (7) obtains, thickness is 300nm；
(9) epitaxial growth of N-shaped doped gan layer：Reaction chamber temperature is risen to 1500 DEG C, in chamber pressure is
Under the conditions of 200Torr, growing n-type doped gan layer in the undoped GaN layer that step (8) obtains, doping content be 9 ×
1018cm-3, thickness be 4 μm；Doped source is silane；Ga source is TMGa；Nitrogen source is NH3；The flow in each source be Ga source 350～
450sccm, nitrogen source 50～65slm, doped source 100～200sccm；
(10) epitaxial growth of InGaN/GaN MQW：Reaction chamber temperature is reduced to 720 DEG C, in the pressure of reative cell
Under the conditions of 200Torr, it is passed through ammonia, nitrogen, trimethyl gallium and trimethyl indium, the N-shaped doped gan layer obtaining in step (9)
Upper growth InGaN/GaN MQW, InGaN/GaN SQW is the InGaN well layer/GaN barrier layer in 13 cycles, wherein
The thickness of InGaN well layer is 5nm, and the thickness of GaN barrier layer is 15nm；The flow in each source is indium source 450～550sccm, gallium source 100
～150sccm, nitrogen source 25～35slm；
(11) epitaxial growth of p-type doped gan layer：Reaction chamber temperature is increased to 1000 DEG C, in the pressure of reative cell is
Under the conditions of 200Torr, it is passed through two luxuriant magnesium, ammonia, nitrogen, trimethyl gallium, the InGaN/GaN MQW obtaining in step (10)
Upper growth p-type doped gan layer, doping content is 9 × 1017cm-3, thickness is 350nm；The flow in each source be Ga source 350～
450sccm, nitrogen source 50～65slm, doped source 150～250sccm.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate it is characterised in that：Including La0.3Sr1.7AlTaO6Substrate, growth
In La0.3Sr1.7AlTaO6AlN nucleating layer on substrate, is grown in the GaN nanometer column template on AlN nucleating layer, is grown in GaN
AlN/GaN superlattice layer on nanometer column template, is grown in the undoped GaN layer on AlN/GaN superlattice layer, is grown in non-mixing
N-shaped doped gan layer in miscellaneous GaN layer, is grown in the InGaN/GaN SQW in N-shaped doped gan layer, is grown in InGaN/GaN
P-type doped gan layer on SQW.
2. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：Described
La0.3Sr1.7AlTaO6Substrate is with (111) face 0.5～1 ° of (100) direction partially as epitaxial surface；Crystalline epitaxial orientation relationship is：GaN
(0001) face parallel to La0.3Sr1.7AlTaO6(111) face.
3. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：Described GaN receives
Rice column template is GaN nano column array, and the height of described GaN nanometer column template is 500～1000nm, a diameter of 100～
200nm, adjacent spacing is 150～250nm；(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111) face.
4. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：Described AlN becomes
The thickness of stratum nucleare is 100～200nm；The thickness of undoped GaN layer is 200～300nm；The thickness of N-shaped doped gan layer is 2～4
μm；The thickness of p-type doped gan layer is 300～350nm.
5. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：Described AlN/
GaN superlattice layer is the AlN layer/GaN layer in 15～25 cycles, and gross thickness is 30～100nm, and wherein the thickness of AlN layer is 1
～2nm, the thickness of GaN layer is 1～2nm.
6. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：InGaN/GaN
SQW is the InGaN well layer/GaN barrier layer in 8～13 cycles, and wherein the thickness of InGaN well layer is 3～5nm, GaN barrier layer
Thickness is 10～15nm.
7. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 1 it is characterised in that：Described growth
Nano-pillar LED on strontium aluminate tantalum lanthanum substrate, also includes sealing coat, and described isolation is deposited upon the side of GaN nanometer column template
Wall and not by the AlN nucleating layer of GaN nanometer column template.
8. be grown in nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 7 it is characterised in that：Described isolation
Thickness degree is 10～50nm；The material of described sealing coat is SiNx、SiO2Or Al2O3.
9. it is grown in the preparation method of nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to any one of claim 1～8,
It is characterized in that：Comprise the following steps：
(1) selection of substrate and its crystal orientation：Using La0.3Sr1.7AlTaO6Substrate, with (111) face 0.5～1 ° of (100) direction partially
For epitaxial surface, crystalline epitaxial orientation relationship is：(0001) face of GaN is parallel to La0.3Sr1.7AlTaO6(111) face；
(2) substrate surface polishes, cleans and makes annealing treatment, and the detailed process of described annealing is：Place the substrate into annealing indoor,
To La in air atmosphere at 800～900 DEG C0.3Sr1.7AlTaO6Substrate carries out making annealing treatment 3～5 hours and then being air cooled to room
Temperature；
(3) AlN nucleation layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 450～550 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth are growth 100～200nm thickness AlN nucleating layer under conditions of 0.2～0.3ML/s；
(4) GaN buffering layer epitaxially grown：Using PLD technology, underlayer temperature is adjusted to 650～850 DEG C, in the pressure of reative cell is
6.0×10-3Torr, the speed of growth are for growing GaN cushion, cushion on AlN nucleating layer under conditions of 0.4～0.6ML/s
Thickness is 500～1000nm；
(5) nanometer embossing etching GaN nanometer column template：By using the arrangement of TracePro software optimization nano-pillar, utilizing
Nanometer embossing and dry etch process are etched downwards to GaN cushion, and obtaining GaN nano column array is GaN nanometer
Column template, the height of nano-pillar is 500～1000nm, a diameter of 100～200nm, and adjacent spacing is 150～250nm；
(6) layer deposited isolating：Using chemical vapor deposition, ald or magnetron sputtering technique in GaN nanometer column template
Layer deposited isolating on side wall and the AIN nucleating layer that do not covered by nano-pillar, the material of described sealing coat is SiNx、SiO2Or
Al2O3, thickness is 10～50nm；
(7) epitaxial growth of AlN/GaN superlattice layer：GaN nanometer column template is transferred in MOCVD, reaction chamber temperature is protected
Hold at 650～850 DEG C, under the conditions of the pressure of reative cell is 150～200Torr, GaN nanometer column template is not isolated
15～25 cycle AlN/GaN superlattice layers of nano-pillar grown on top of layer deposition, gross thickness 30～100nm's, wherein AlN layer
Thickness is 1～2nm, and the thickness of GaN layer is 1～2nm；
(8) epitaxial growth of undoped GaN layer：Reaction chamber temperature is maintained at 1000～1300 DEG C, in the pressure of reative cell is
Under the conditions of 150～200Torr, undoped GaN layer is grown on the AlN/GaN superlattice layer that step (7) obtains, thickness is 200
～300nm；
(9) epitaxial growth of N-shaped doped gan layer：Reaction chamber temperature is risen to 1000～1500 DEG C, is 150 in chamber pressure
Under the conditions of～200Torr, growing n-type doped gan layer in the undoped GaN layer that step (8) obtains, doping content is 3 × 1018
～9 × 1018cm-3, thickness be 2～4 μm；
(10) epitaxial growth of InGaN/GaN MQW：Reaction chamber temperature is reduced to 700～780 DEG C, in the pressure of reative cell
Under the conditions of 150～200Torr, it is passed through ammonia, nitrogen, trimethyl gallium and trimethyl indium, the N-shaped obtaining in step (9) adulterates
InGaN/GaN MQW is grown, InGaN/GaN SQW is the InGaN well layer/GaN barrier layer in 8～13 cycles in GaN layer,
The thickness of wherein InGaN well layer is 3～5nm, and the thickness of GaN barrier layer is 10～15nm；
(11) epitaxial growth of p-type doped gan layer：Reaction chamber temperature is increased to 900～1100 DEG C, in the pressure of reative cell is
Under the conditions of 150～200Torr, it is passed through two luxuriant magnesium, ammonia, nitrogen, trimethyl gallium and trimethyl indium, obtains in step (10)
P-type doped gan layer is grown on InGaN/GaN MQW, doping content is 3 × 1017～9 × 1017cm-3, thickness be 300～
350nm.
10. it is grown in the preparation method of nano-pillar LED on strontium aluminate tantalum lanthanum substrate according to claim 9, its feature exists
In：Described substrate surface polishing, specially：First by La0.3Sr1.7AlTaO6Substrate surface diamond mud is polished,
Cooperation observation by light microscope substrate surface, after not having cut, then is polished locating using the method for chemically mechanical polishing
Reason；
Described cleaning, specially：By La0.3Sr1.7AlTaO6Substrate is put into and is cleaned by ultrasonic 3～5 minutes under room temperature in deionized water,
Remove La0.3Sr1.7AlTaO6Substrate surface pickup granule, then sequentially pass through hydrochloric acid, acetone, washing with alcohol, remove surface organic
Thing, is dried up with drying nitrogen.
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