CN100495750C - Gallium nitride based LED epitaxial slice structure and method for preparing the same - Google Patents
Gallium nitride based LED epitaxial slice structure and method for preparing the same Download PDFInfo
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- 229910002601 GaN Inorganic materials 0.000 title claims description 146
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims description 117
- 238000000034 method Methods 0.000 title claims description 8
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 229910002704 AlGaN Inorganic materials 0.000 claims abstract description 21
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 15
- 239000010980 sapphire Substances 0.000 claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims description 49
- 229910052710 silicon Inorganic materials 0.000 claims description 49
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 47
- 239000010703 silicon Substances 0.000 claims description 47
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 42
- 229910052749 magnesium Inorganic materials 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 38
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 28
- 239000011248 coating agent Substances 0.000 claims description 21
- 238000000576 coating method Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000012159 carrier gas Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
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- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 230000004907 flux Effects 0.000 claims description 8
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 claims description 8
- 238000001259 photo etching Methods 0.000 claims description 6
- 241000826860 Trapezium Species 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 230000026267 regulation of growth Effects 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 150000004767 nitrides Chemical class 0.000 abstract description 4
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Abstract
The invention relates to a nitride-based LED epitaxial wafer structure and a processing method, belonging to the LED field. The nitride-based LED epitaxial wafer structure has high light extraction efficiency and good crystal quality. A GaN buffer layer, a first si-doped GaN layer, a dielectric layer, a second si-doped GaN layer, an InGaN/GaN multiple quantum well, a mg-doped AlGaN layer and a mg-doped GaN layer are arranged on the substrate of the nitride-based LED epitaxial wafer structure in a bottom-up order. A sapphire substrate with (0001) face is put into the reaction chamber and heat treated under the atmosphere of H2; the temperature is lowered to grow the GaN buffer layer, on which the first si-doped GaN layer grows; then the temperature is lowered and the sample is taken out.
Description
Technical field
The present invention relates to a kind of light-emitting diode, especially relate to gallium nitride based LED epitaxial slice structure of growth technology-horizontal extension outgrowth technology (ELOG) of using gallium nitride (GaN) base and compound film thereof in a kind of third generation semiconductor photoelectronic device field and preparation method thereof.
Background technology
The GaN based light-emitting diode has that volume is little, the life-span is long, can realize the large tracts of land array; LED uses the DC power supply that is lower than 5V to drive, and radiation area mainly concentrates on visible region.Have low pressure, power saving, cold light source, the response time is short, luminous efficiency is high, explosion-proof and energy-conservation advantage such as reliable, its market potential is huge.It is except being applied in stop-light, outside the large tracts of land display screen, also reaches its maturity in the application of energy-conservation normal lighting light source.LED does not contain harmful lead and mercury, has avoided the pollution to environment simultaneously, for the recovery problem of discarded object, lacks than existing sight lamp yet, and it is safe and environmentally friendly to say so, and the title of " green illumination light source " is arranged.Many experts think that LED is the first generation incandescent light source that continues, second generation fluorescent light, after the third generation high-intensity gas discharge lamp light source the 4th generation lighting source.Produce the numerous and confused and old brand bulbmaker of the semiconductor company of blue light diode in the world and form an alliance, seize the illumination market that this can be described as following maximum.
III family-nitride semi-conductor material is because its good photoelectric characteristic, at the preparation ultraviolet detector, light-emitting diode, laser diode and high temperature, photoelectric device field extensive application such as high frequency have also obtained breakthrough progress ([1] Shuji Nakamura.Recent Developments in InGaN-Based Blue LEDs and LDs.Department ofResearch and Development in recent years, Nichia Chemical Industries, Ltd; [2] Takashi MUKAI, MotokazuYAMADA and Shuji NAKAMURA.Characteristics of InGaN-Based UV/Blue/Green/Amber/RedLight-Emitting Diodes.Jpn.J.Appl.Phys, 1999; 38:3976).Its ternary compound InGaN, by regulating the component of In in the alloy, energy gap can vary continuously to 3.4eV (GaN) from 0.6eV (InN) in theory, emission wavelength has covered whole visible light wave range and part ultraviolet light wave band, be widely used in active layer ([3] Chin-Hsiang CHEN of opto-electronic device LED and LD, Shoou-Jinn CHANG and Yan-Kuin SU.High-Indium-Content InGaN/GaNMultiple-Quantum-Well Light-Emitting Diodes.Jpn.J.Appl.Phys, 2003; 42:2281; [4] Horng-Shyang Chen, Dong-Ming Yeh, Chih-Feng Lu, etal.White light generation with CdSe-ZnSnanocrystals coated on an InGaN-GaN quantum-well blue/Green two-wavelength light-emittingdiode.IEEE PHOTONICS TECHNOLOGY LETTERS, 2006; 18:NO.13.)。
Nineteen ninety-five, people such as Nakamura have developed InGaN single quantum LED, and then the multi-quantum pit structure external quantum efficiency that can make LED up to 20% ([5] Mukai T.Recent progress in grou mixes magnesium III nitride Light-emittingdiodes[J] .IEEE J.Select.Topics Quantum electron, 2002,8 (2): 264-270), because quantum well plays good restriction to charge carrier, and the InGaN ternary-alloy material has its intrinsic characteristic: in the growth course of InGaN, there is fluctuation in the spatial distribution of In, thereby in quantum well, form the rich In district of the nano-scale of similar quantum-dot structure, charge carrier is played three-dimensional restriction, make charge carrier more difficult moving to before radiation recombination takes place because the non-radiative recombination center that defective etc. cause, thereby improve radiation recombination luminous efficiency ([6] S.Nakamura greatly, M.Senoh and T.Mukai. mixes magnesium GaN/N-InGaN/N-GaN Double-Heterostructure Blue-Light-Emitting Diodes Jpn.Jpn.J.Appl.Phys., 1993; 32:L8; [7] S.Nakamura, T.Mukai, M.Senoh, etal.In
xGa
(1-x)N/In
yGa
(1-y)N superlattices grownon GaN films J.Appl.Phys., 1993; 74:3911).So GaN base LED main flow structure adopts InGaN/GaN, InGaN/AlGaN single quantum well or multi-quantum pit structure exactly at present.Existing traditional GaN base LED (referring to Fig. 1) is a low temperature GaN resilient coating of using the non-doping of metal organic chemical vapor deposition (MOCVD) method growth one deck on Sapphire Substrate 1, what the L temperature grew at high temperature that one deck mixes Si then mixes silicon GaN layer 2, then mixing growing InGaN on the silicon GaN layer/GaN multiple quantum well active layer 3, growing on active layer at last, one deck is mixed magnesium AlGaN layer and one deck is mixed magnesium GaN layer 4.Form the LED device epitaxial slice on plane.
Generally speaking, the luminosity of LED strengthens along with the increase of injection current, but the pn surplus is a maximum operating temperature, big electric current injection can produce a large amount of heat and damage crystal and sealed in unit, thereby cause shorten device lifetime, be only crucial technology so improve the energy conversion efficiency of injection current.We weigh the efficient that electric energy is converted to luminous energy at external quantum efficiency commonly used, and its size equals the amassing of escapement ratio of internal quantum efficiency and photon.Raising along with epitaxy technology, the crystal mass of GaN base semiconductor material is greatly improved, so in general, the internal quantum efficiency of high performance LED is all very high, just because lattice defect, substrate causes the photon escapement ratio very low to the absorption of light and the total reflection problem of traditional LED rectangular cavity structure, and actual external quantum efficiency is not high.Since the refractive index ratio air of GaN refractive index big, so as θ＜θ
cWhen (angle of total reflection of light when the GaN layer shines air), light can be overflowed from the front, works as θ〉90 °-θ
cThe time, less than the angle of total reflection, overflow from the side by light in the side incidence angle for light, and work as θ
c＜θ＜90 °-θ
cThe time, light, can not be overflowed all less than the angle of total reflection in positive and side.As calculated, for the LED of rectangular cavity structure, has only 40% luminous energy overflow from the surface (referring to Fig. 2).
Round the escapement ratio that improves photon, a lot of researchs have been done both at home and abroad.Nineteen ninety-five, people such as Yoshida defective from reduce crystal set about proposing the LEO growing technology has reduced the dislocation density (4-5 orders of magnitude) of GaN epitaxial loayer effectively in addition at pterion GaN near dislocation-free ([8] Usui A, Sunakawa H, Sakai A etal.Jpn.J.Appl.Phys, Part2,1997,36 (7B): thus the luminous efficiency of LED L899) improved greatly.A kind of method at the U.S.'s business-like raising photon escapement ratio adopts transparent substrates exactly, reduce the absorption of substrate, after LED has grown, opaque substrate etching is fallen photon, again transparent substrate and epitaxial wafer are bonded together, make the photon can be from each face outgoing.A kind of LED that adopts inverted structure, earlier substrate etching is got very thin, fine and improve light extraction efficiency in the reflectivity of utilizing electrode.Lumileds company adopts transparent substrates, and the cross section is trapezoidal, and stereochemical structure is the chip structure of inverted pyramid shape, destroys the traditional die cube shaped, solves the total reflection problem and improves light extraction efficiency.The eighties in last century, people such as Burnham proposed growth distribution Bragg reflecting layer structure ([9] QiYun, Dai Ying, Li Anyi.Enhancement of the external quantum efficiency of light-emitting-diodes[J] .Electronic Components and Materials, 2003,22 (4): 43-45 (in Chinese)), reduce substrate to the absorption of light and improve the escapement ratio of photon greatly.Also there is research to adopt and on the epitaxial wafer of having grown, carries out surface coarsening, the laser lift-off substrate is transparent substrates and substrate changed into the metal that heat conduction is good and reflectivity is good on the bonding again, adopt photonic crystal or the like, all these researchs all are in order to improve the external quantum efficiency of LED device.
Summary of the invention
To the objective of the invention is to that the light extraction efficiency that adopts conventional LED device architecture to exist is low to be waited not enoughly in order overcoming, a kind of light extraction efficiency height, gallium nitride based LED epitaxial slice structure that crystal mass is good and preparation method thereof to be provided.
Technical scheme of the present invention is to utilize the characteristics of horizontal extension outgrowth technology to destroy traditional rectangular optical resonant cavity, adopts LP-MOCVD (low pressure metal organic chemical vapor deposition system) equipment, utilizes high-purity H
2, N
2As carrier gas, carry out the preparation of LED epitaxial wafer, growth pressure is controlled between the 50-780Torr in the whole growth process.
Gallium nitride based LED epitaxial slice structure of the present invention is provided with Sapphire Substrate, unadulterated GaN resilient coating, the 1st mixes silicon GaN layer, dielectric layer, the 2nd mixes silicon GaN layer, the InGaN/GaN Multiple Quantum Well in 3～5 cycles, mix magnesium AlGaN layer and mix magnesium GaN layer, unadulterated from bottom to up GaN resilient coating, the 1st mixes silicon GaN layer, dielectric layer, the 2nd mixes silicon GaN layer, the InGaN/GaN Multiple Quantum Well in 3～5 cycles, mix magnesium AlGaN layer and mix magnesium GaN layer and be located at successively on the Sapphire Substrate, finally its cross section forms side by side little triangle or trapezium structure on the direction of growth; The thickness of unadulterated GaN resilient coating is 10～40nm, the 1st thickness of mixing silicon GaN layer is 2～3 μ m, the thickness of dielectric layer is 100～200nm, the 2nd thickness of mixing silicon GaN layer is 2～3 μ m, the thickness in each cycle of the InGaN/GaN Multiple Quantum Well in 3～5 cycles is 3～5nm, the thickness of mixing magnesium AlGaN layer is 0.1～0.2 μ m, and the thickness of mixing magnesium GaN layer is 0.2～0.3 μ m; Dielectric layer is SiO
2Layer or SiN layer.
The preparation method of gallium nitride based LED epitaxial slice structure of the present invention, concrete steps are as follows:
1) Sapphire Substrate of (0001) face is packed into reative cell is at H
2Be heated to 1050～1200 ℃ under the atmosphere substrate is heat-treated 10～20min; Then cooling is at the GaN of 500～600 ℃ of growth thickness 10～40nm resilient coating;
2) mix silicon GaN layer at 0.5～2 μ m the 1st that grows under 950～1100 ℃ on the GaN resilient coating, sample is taken out in cooling;
3) under 200～300 ℃, on sample, deposit the thick SiO of 100～200nm with PE-CVD sedimentation
2Layer or SiN layer, respectively along the 1st mix silicon GaN layer＜1100 or＜1120〉direction carve the wide window of 2～10 μ m as graph substrate with traditional photoetching process, the sample that must have graph substrate, the figure of window can be bar shaped, hexagon, rhombus or circle etc., wherein the width of marking shape window is 2～8 μ m, and the cycle is 8～20 μ m, and length is 1～3cm, the external diameter of a circle of hexagonal window openings is 5～10 μ m, cycle is 10～20 μ m, and the diameter of the inscribed circle of diamond-shaped windows is 4～10 μ m, and the cycle is 10～20 μ m, the diameter of circular window is 5～10 μ m, and the cycle is 10～20 μ m;
4) put into metal organic chemical vapor deposition (MOCVD) system after sample cleans and carry out epitaxial growth: at first mix silicon GaN layer, then at N at 950～1100 ℃ of the 2nd of one deck 2～3 μ m that grow down
2Grow under the atmosphere InGaN/GaN Multiple Quantum Well in 3～5 cycles, 0.1～0.2 μ m that grows at last is thick mix magnesium AlGaN layer and 0.2～0.3 μ m thick mix magnesium GaN layer, after whole epitaxial growth is finished, with the N of epitaxial wafer at 700～850 ℃
210～the 20min that anneals under the atmosphere, gallium nitride based LED epitaxial slice.
Ga of the present invention, In, Mg, N, Si source are respectively high-purity trimethyl gallium (TMGa), trimethyl indium (TMIn), two luxuriant magnesium (Cp
2Mg), NH
3And silane (SiH
4).
The pressure of growing GaN resilient coating is 500～600Torr, and carrier gas flux is 10～30L/min, and the TMGa flow is 20～120 μ mol/min, NH
3Flow is 80～120mol/min.
The pressure of growing InGaN/GaN Multiple Quantum Well is 50～500Torr, and carrier gas flux is 5～20L/min, NH
3Flow is 120～500mol/min.The thickness of trap layer is 2.0～5.0nm, and the growth temperature of trap layer is 700～900 ℃, and the TMGa flow is 1.0～4.0 μ mol/min, the TMIn flow is 10～40 μ mol/min, the thickness of building layer is 5～20nm, and the growth temperature of building layer is 700～900 ℃, and the TMGa flow is 10～40 μ mol/min.
It is 76～200Torr with the pressure of mixing magnesium GaN layer that magnesium AlGaN layer is mixed in growth, and carrier gas flux is 5～20L/min, and growth temperature is 1000～1100 ℃, the flow of TMGa is 20～50 μ mol/min, the flow of TMAl is 2.0～5.0 μ mol/min, and the NH3 flow is 120～500mol/min, Cp
2The flow of Mg is 0.5～5.0 μ mol/min.
In horizontal extension outgrowth process, epitaxy layer thickness that it is generally acknowledged window region begins epitaxial lateral overgrowth when surpassing mask regions thickness, although the dislocation density of resilient coating is relatively very high, the GaN dislocation density of epitaxial lateral overgrowth is but well below window region on the pterion.And horizontal and vertical growth rate is than controlling by the growth conditions of reative cell.Make cross growth speed less than longitudinal growth speed by parameters such as control growing temperature, growth pressure and V/III.When adjacent two window region epitaxial lateral overgrowths partly combine, epitaxially grown Multiple Quantum Well LED device architecture on different graph substrate, final its cross section forms little triangle or trapezium structure side by side on the direction of growth, be different from traditional rectangular cavity structure.
Compare with existing LED device, outstanding advantage of the present invention is:
1, utilizes controlled non-planar LED device architecture, destroy traditional rectangular optical cavity resonator structure, solve the total reflection problem (referring to Fig. 2) of light, thereby improve light extraction efficiency.
2, need to consider from practice, because lateral growth speed is very slow, its cross section forms side by side little triangle or trapezoidal on the direction of growth, must select little mask layer width, certainly as long as the time long enough of growth, its epitaxial structure can form big triangle or big trapezium structure, but this scheme is infeasible, because consider and be the exponential relationship decay in the process that light propagates in crystal, big triangle and big trapezoidal escapement ratio to the raising photon have little significance, so very little mask layer width is selected in the pterion of lateral growth, final its cross section forms side by side little triangle or little trapezoidal on the direction of growth, help light from material surface effusion (referring to Fig. 4 and Fig. 6).
3, LED device architecture material is grown directly upon on the GaN of the low dislocation in pterion, helps obtaining high-quality active layer material, thereby can improve its luminous efficiency greatly.
4, well-known, as long as light extraction efficiency is improved and just can correspondingly reduces the problem that the led chip internal heat effect brings, i.e. the characteristic sublinear problem of P-I.Under the condition of injecting identical electric current, its thermal effect of LED that light extraction efficiency is high is lower, and the pn knot just is not easy to reach its maximum operating temperature, therefore can prolong its working life, makes that also the various aspects of performance of LED device is well improved.
Description of drawings
Fig. 1 is traditional LED epitaxial slice structure schematic diagram.
Fig. 2 is traditional LED rectangular cavity structure light path schematic diagram.
Fig. 3 is LED epitaxial slice structure (cross section the is little triangle) schematic diagram of the embodiment of the invention 1.
Fig. 4 obtains the LED structure light path schematic diagram of little triangular-section for the laterally overgrown of the embodiment of the invention 1.
Fig. 5 is LED epitaxial slice structure (cross section the is little trapezoidal) schematic diagram of the embodiment of the invention 2.
Fig. 6 obtains the LED structure light path schematic diagram of little trapezoid cross section for the laterally overgrown of the embodiment of the invention 2.
In Fig. 1～6,1. Sapphire Substrate, 2. the 1st mixes silicon GaN layer, and the InGaN/GaN Multiple Quantum Well in 3.3～5 cycles is 4. mixed magnesium AlGaN layer and is mixed magnesium GaN layer, 5. dielectric layer, 6. the 2nd mixes silicon GaN layer.
Embodiment
Following examples all adopt 3 * 2CCS LP-MOCVD equipment to carry out the epitaxial wafer growth.
Referring to Fig. 3, gallium nitride based LED epitaxial slice structure of the present invention is provided with that Sapphire Substrate 1, unadulterated GaN resilient coating (not drawing), the 1st are mixed silicon GaN layer 2, dielectric layer the 5, the 2nd is mixed silicon GaN layer 6 in Fig. 3, the InGaN/GaN Multiple Quantum Well 3 in 3～5 cycles, mix magnesium AlGaN layer and mix magnesium GaN layer 4, unadulterated from bottom to up GaN resilient coating, the 1st is mixed silicon GaN layer 2, dielectric layer the 5, the 2nd and is mixed the InGaN/GaN Multiple Quantum Well 7 in 6,3～5 cycle of silicon GaN layer, mixes magnesium AlGaN layer and mix magnesium GaN layer 4 and be located at successively on the Sapphire Substrate 1; The thickness of unadulterated GaN resilient coating is 10～40nm, the 1st thickness of mixing silicon GaN layer is 2～3 μ m, the thickness of dielectric layer is 100～200nm, the 2nd thickness of mixing silicon GaN layer is 2～3 μ m, the thickness in each cycle of the InGaN/GaN Multiple Quantum Well in 3～5 cycles is 3～5nm, the thickness of mixing magnesium AlGaN layer is 0.1～0.2 μ m, and the thickness of mixing magnesium GaN layer is 0.2～0.3 μ m; Dielectric layer 5 is SiO
2Layer or SiN layer.
Below provide its preparation method.
(1) (0001) orientation Sapphire Substrate of exempting to clean is packed into reative cell is at H
2Be heated to 1060 ℃ of baking 15min under the atmosphere, chamber pressure is 500Torr.
(2) the GaN resilient coating that is 25nm at 530 ℃ of following growth thickness, growth pressure is 500Torr, the TMGa flow is 40 μ mol/min, NH
3Flow is 110 μ mol/min.
(3) mix silicon GaN layer at 1030 ℃ of following growth regulations 1, growth pressure is 200Torr.
(4) deposit SiO with PE-CVD sedimentation down at 300 ℃
2Layer, thickness is 200nm, with traditional photoetching skill edge mix silicon GaN layer＜1120〉direction carve the window region of different graphic and size.
(5) after being cleaned up, the sample that is carved with figure puts into metal organic chemical vapor deposition (MOCVD) system epitaxial growth once more (secondary epitaxy) once more.
(6) secondary epitaxy: earlier at H
2Growth regulation 2 is mixed silicon GaN layer under the atmosphere, and growth temperature is 1050 ℃, and growth pressure is 200Torr, and the TMGa flow is 100 μ mol/min, NH
3Flow is 250mol/min.Because the difference of horizontal and vertical growth rate, the 2nd of adjacent windows oral region are mixed silicon GaN layer after healing on the mask layer zone, forming the cross section is leg-of-mutton epitaxial slice structure, then at N
2The InGaN/GaN quantum well in 5 cycles of growth under the atmosphere.The trap layer is InGaN, and thickness is 3nm, and growth pressure is 300Torr, and the flow of TMGa is 4.0 μ mol/min, and the flow of TMIn is 12.0 μ mol/min, NH
3Flow is 250.0mol/min, and growth temperature is 750 ℃; Building layer is GaN, and thickness is 15nm, and the flow of TMGa is 20.0 μ mol/min, NH
3Flow is 250mol/min, and growth temperature is 850 ℃.Grow down at 950 ℃ at last and mix magnesium AlGaN layer and mix magnesium GaN layer, growth pressure is 100Torr, and the flow of TMGa is 50 μ mol/min, NH
3Flow is 180.0mol/min, Cp
2The flow of Mg is 0.5 μ mol/min.
(7) the sample that obtains after the epitaxial growth at 700 ℃ of N
2The 20min that anneals under the atmosphere, N
2Flow is 2.0L/min (referring to Fig. 3).
(1) (0001) orientation Sapphire Substrate of exempting to clean is packed into reative cell is at H
2Be heated to 1080 ℃ of baking 10min under the atmosphere, chamber pressure is 500Torr.
(2) the GaN resilient coating that is 30nm at 530 ℃ of following growth thickness, growth pressure is 500Torr, the TMGa flow is 50 μ mol/min, NH
3Flow is 150 μ mol/min.
(3) mix silicon GaN layer at 1050 ℃ of following growing GaN layers and the 1st, growth pressure is respectively 200Torr and 100Torr.
(4) under 300 ℃, deposit SiO with PE-CVD
2Layer, thickness is 200nm, with traditional photoetching skill carve the edge mix silicon GaN layer＜1100〉direction carve out the window region of different graphic and size.
(5) after being cleaned up, the sample that is carved with figure puts into metal organic chemical vapor deposition system (MOCV system) epitaxial growth (secondary epitaxy) once more.
(6) secondary epitaxy: earlier at H
2Growth regulation 2 is mixed silicon GaN layer under the atmosphere, and growth temperature is 1030 ℃, and growth pressure is 200Torr, and the TMGa flow is 100 μ mol/min, NH
3Flow is 250mol/min.Because the difference of horizontal and vertical growth rate makes the 2nd of adjacent windows oral region mix silicon GaN layer and heals on the mask layer zone, forming the cross section is trapezoidal epitaxial slice structure, then at N
2The InGaN/GaN quantum well in 5 cycles of growth under the atmosphere.The trap layer is InGaN, and thickness is 3nm, and growth pressure is 300Torr, and the flow of TMGa is 4.0 μ mol/min, and the flow of TMIn is 12.0 μ mol/min, NH
3Flow is 250.0mol/min; Building layer is GaN, and thickness is 15nm, and the flow of TMGa is 30.0 μ mol/min, NH
3Flow is 230mol/min, and growth temperature is 850 ℃.Grow down at 950 ℃ at last and mix magnesium AlGaN layer and mix magnesium GaN layer, growth pressure is 100Torr, and the flow of TMGa is 50 μ mol/min, NH
3Flow is 180.0mol/min, Cp
2The flow of Mg is 0.5 μ mol/min.
(7) the sample that obtains after the epitaxial growth at 800 ℃ of N
2The 10min that anneals under the atmosphere, N
2Flow is 2.0L/min (referring to Fig. 5, the code name implication among Fig. 5 is identical with Fig. 3).
(1) (0001) orientation Sapphire Substrate of exempting to clean is packed into reative cell is at H
2Be heated to 1060 ℃ of baking 15min under the atmosphere, chamber pressure is 500Torr.
(2) the GaN resilient coating that is 25nm at 550 ℃ of following growth thickness, growth pressure is 500Torr, the TMGa flow is 65 μ mol/min, NH
3Flow is 180 μ mol/min.
(3) mix silicon GaN layer at 1030 ℃ of following growing GaN layers and the 1st, growth pressure is respectively 200Torr and 100Torr.
(4) under 300 ℃, deposit SiO with PE-CVD
2, thickness is 150nm, with traditional photoetching skill along n-GaN＜1120〉direction carve the window region of different graphic and size.
(5) after being cleaned up, the sample that is carved with figure puts into metal organic chemical vapor deposition system (MOCV system) epitaxial growth (secondary epitaxy) once more
(6) secondary epitaxy: earlier at H
2Growth regulation 2 is mixed silicon GaN layer under the atmosphere, and growth temperature is 1080 ℃, and growth pressure is 200Torr, and the TMGa flow is 50 μ mol/min, NH
3Flow is 120mol/min.Because the difference of horizontal and vertical growth rate, the 2nd of adjacent windows oral region is mixed silicon GaN and is healed on the mask layer zone, and forming the cross section is leg-of-mutton epitaxial slice structure, then at N
2The InGaN/GaN quantum well in 3 cycles of growth under the atmosphere.The trap layer is InGaN, and thickness is 4nm, and growth pressure is 300Torr, and the flow of TMGa is 3.0 μ mol/min, and the flow of TMIn is 10.0 μ mol/min, NH
3Flow is 220.0mol/min; Building layer is GaN, and thickness is 12nm, and the flow of TMGa is 20.0 μ mol/min, NH
3Flow is 250mol/min, and growth temperature is 900 ℃.Grow down at 950 ℃ at last and mix magnesium AlGaN layer and mix magnesium GaN layer, growth pressure is 100Torr, and the flow of TMGa is 50 μ mol/min, NH
3Flow is 180.0mol/min, Cp
2The flow of Mg is 0.5 μ mol/min.
(7) the sample that obtains after the epitaxial growth at 800 ℃ of N
2The 10min that anneals under the atmosphere, N
2Flow is 2.0L/min.
(1) (0001) orientation Sapphire Substrate of exempting to clean is packed into reative cell is at H
2Be heated to 1080 ℃ of baking 10min under the atmosphere, chamber pressure is 500Torr.
(2) the GaN resilient coating that is 30nm at 530 ℃ of following growth thickness, growth pressure is 500Torr, the TMGa flow is 80 μ mol/min, NH
3Flow is 220 μ mol/min.
(3) mix silicon GaN layer at 1050 ℃ of following growing GaN layers and the 1st, growth pressure is 200Torr.
(4) under 300 ℃, deposit SiO with PE-CVD
2Layer, thickness is 150nm, with traditional photoetching skill carve the edge mix silicon GaN layer＜1100〉direction carve out the window region of different graphic and size.
(5) after being cleaned up, the sample that is carved with figure puts into metal organic chemical vapor deposition system (MOCV system) epitaxial growth (secondary epitaxy) once more.
(6) secondary epitaxy: earlier at H
2Growth regulation 2 is mixed silicon GaN layer under the atmosphere, and growth temperature is 1050 ℃, and growth pressure is 200Torr, and the TMGa flow is 50 μ mol/min, NH
3Flow is 120mol/min.Heal on the mask layer zone because the difference of horizontal and vertical growth rate makes the 2nd of adjacent windows oral region mix silicon GaN layer, forming the cross section is trapezoidal epitaxial slice structure, then at N
2The InGaN/GaN quantum well in 3 cycles of growth under the atmosphere.The trap layer is InGaN, and thickness is 4nm, and growth pressure is 300Torr, and the flow of TMGa is 3 μ mol/min, and the flow of TMIn is 10.0 μ mol/min, NH
3Flow is 220.0mol/min; Building layer is GaN, and thickness is 15nm, and the flow of TMGa is 30.0 μ mol/min, NH
3Flow is 280mol/min, and growth temperature is 900 ℃.Grow down at 950 ℃ at last and mix magnesium AlGaN layer and mix magnesium GaN layer, growth pressure is 100Torr, and the flow of TMGa is 50 μ mol/min, NH
3Flow is 180.0mol/min, Cp
2The flow of Mg is 0.5 μ mol/min.
(7) the sample that obtains after the epitaxial growth at 800 ℃ of N
2The 10min that anneals under the atmosphere, N
2Flow is 2.0L/min.
Claims (8)
1. gallium nitride based LED epitaxial slice structure, it is characterized in that being provided with Sapphire Substrate, unadulterated GaN resilient coating, the 1st mixes silicon GaN layer, dielectric layer, the 2nd mixes silicon GaN layer, the InGaN/GaN Multiple Quantum Well in 3～5 cycles, mix magnesium AlGaN layer and mix magnesium GaN layer, unadulterated from bottom to up GaN resilient coating, the 1st mixes silicon GaN layer, dielectric layer, the 2nd mixes silicon GaN layer, the InGaN/GaN Multiple Quantum Well in 3～5 cycles, mix magnesium AlGaN layer and mix magnesium GaN layer and be located at successively on the Sapphire Substrate, finally its cross section forms side by side little triangle or trapezium structure on the direction of growth;
The thickness of unadulterated GaN resilient coating is 10～40nm, the 1st thickness of mixing silicon GaN layer is 2～3 μ m, the thickness of dielectric layer is 100～200nm, the 2nd thickness of mixing silicon GaN layer is 2～3 μ m, the thickness in each cycle of the InGaN/GaN Multiple Quantum Well in 3～5 cycles is 3～5nm, the thickness of mixing magnesium AlGaN layer is 0.1～0.2 μ m, and the thickness of mixing magnesium GaN layer is 0.2～0.3 μ m;
Dielectric layer is SiO
2Layer or SiN layer.
2. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 1 is characterized in that concrete steps are as follows:
1) Sapphire Substrate of (0001) face is packed into reative cell is at H
2Be heated to 1050～1200 ℃ under the atmosphere substrate is heat-treated 10～20min; Then cooling is at the GaN of 500～600 ℃ of growth thickness 10～40nm resilient coating;
2) mix silicon GaN layer at 0.5～2 μ m the 1st that grows under 950～1100 ℃ on the GaN resilient coating, sample is taken out in cooling;
3) under 200～300 ℃, on sample, deposit the thick SiO of 100～200nm with the PE-CVD sedimentation
2Layer or SiN layer, respectively along the 1st mix silicon GaN layer＜1100 or＜1120〉direction carve the wide window of 2～10 μ m as graph substrate with traditional photoetching process, must have the sample of graph substrate;
4) put into metal organic chemical vapor deposition (MOCVD) system after sample cleans and carry out epitaxial growth: at first mix silicon GaN layer, then at N at 950～1100 ℃ of the 2nd of one deck 2～3 μ m that grow down
2Grow under the atmosphere InGaN/GaN Multiple Quantum Well in 3～5 cycles, 0.1～0.2 μ m that grows at last is thick mix magnesium AlGaN layer and 0.2～0.3 μ m thick mix magnesium GaN layer, after whole epitaxial growth is finished, with the N of epitaxial wafer at 700～850 ℃
210～the 20min that anneals under the atmosphere, gallium nitride based LED epitaxial slice.
3. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2 is characterized in that Ga, In, Mg, N, Si source are respectively trimethyl gallium, trimethyl indium, two luxuriant magnesium, NH
3And silane.
4. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2, the pressure that it is characterized in that the growing GaN resilient coating is 500～600Torr, and carrier gas flux is 10～30L/min, and the TMGa flow is 20～120 μ mol/min, NH
3Flow is 80～120mol/min.
5. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2, it is characterized in that mixing silicon GaN layer and the 2nd by growth regulation 1, to mix the pressure of silicon GaN layer be 100～300Torr, carrier gas flux is 5～20L/min, and the TMGa flow is 80～400 μ mol/min, NH
3Flow is 120～500mol/min, SiH
4Flow is 0.2～2.0nmol/min.
6. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2, the pressure that it is characterized in that growing InGaN/GaN Multiple Quantum Well is 50～500Torr, and carrier gas flux is 5～20L/min, and the NH3 flow is 120～500mol/min; The thickness of trap layer is 2.0～5.0nm, and the growth temperature of trap layer is 700～900 ℃, and the TMGa flow is 1.0～4.0 μ mol/min, the TMIn flow is 10～40 μ mol/min, the thickness of building layer is 5～20nm, and the growth temperature of building layer is 700～900 ℃, and the TMGa flow is 10～40 μ mol/min.
7. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2, the pressure of mixing magnesium AlGaN layer and mixing magnesium GaN layer that it is characterized in that growing is 76～200Torr, carrier gas flux is 5～20L/min, growth temperature is 1000～1100 ℃, the flow of TMGa is 20～50 μ mol/min, the flow of TMA1 is 2.0～5.0 μ mol/min, and the NH3 flow is 120～500mol/min, Cp
2The flow of Mg is 0.5～5.0 μ mol/min.
8. the preparation method of gallium nitride based LED epitaxial slice structure as claimed in claim 2, the figure that it is characterized in that window is bar shaped, hexagon, rhombus or circle, wherein the width of marking shape window is 2～8 μ m, cycle is 8～20 μ m, length is 1～3cm, the external diameter of a circle of hexagonal window openings is 5～10 μ m, cycle is 10～20 μ m, and the diameter of the inscribed circle of diamond-shaped windows is 4～10 μ m, and the cycle is 10～20 μ m, the diameter of circular window is 5～10 μ m, and the cycle is 10～20 μ m.
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| CN103928578A (en) * | 2014-04-22 | 2014-07-16 | 湘能华磊光电股份有限公司 | LED epitaxial layer, growth method thereof and LED chip |
| CN104241464B (en) * | 2014-09-05 | 2017-12-22 | 西安神光皓瑞光电科技有限公司 | A kind of epitaxial growth method for improving p-type gallium nitride doping concentration |
| CN108346752A (en) * | 2018-01-18 | 2018-07-31 | 南方科技大学 | A kind of preparation method and application of light emitting diode with quantum dots |
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