CN104037287B - LED epitaxial wafer grown on Si substrate and preparation method thereof - Google Patents

LED epitaxial wafer grown on Si substrate and preparation method thereof Download PDF

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CN104037287B
CN104037287B CN201410256386.2A CN201410256386A CN104037287B CN 104037287 B CN104037287 B CN 104037287B CN 201410256386 A CN201410256386 A CN 201410256386A CN 104037287 B CN104037287 B CN 104037287B
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CN104037287A (en
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李国强
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Guangzhou Zhongtuo Optoelectrical Technology Co Ltd
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Abstract

The invention discloses an LED epitaxial wafer grown on an Si substrate and a preparation method thereof. The LED epitaxial wafer grown on the Si substrate is prepared through the following preparation method: using the Si substrate, enabling the surface (111) of the Si substrate to deviate from (100) by 0.5 to 1 degree, growing a first AlN buffer layer, and growing a second AlN buffer layer, an AlGaN step buffer layer, a u-GaN layer, an n-GaN layer, an InGaN/GaN quantum well layer and a p-GaN layer in sequence. The LED epitaxial wafer grown on the Si substrate uses Si as the substrate, the preparation method combines a metal organic chemical vapor deposition technique and a pulsed laser deposition technique, a procedure of pre-paving Al for using the metal organic chemical vapor deposition technique to grow the AlN is omitted, the problem that Si is diffused to the AlN buffer layer under a high temperature to damage the surface shape is avoided, and the LED epitaxial wafer is good in performance, high in crystal quality and suitable for LED devices.

Description

Growth LED on a si substrate and preparation method thereof
Technical field
The present invention relates to LED, particularly to growth LED extension on a si substrate Sheet and preparation method thereof.
Background technology
LED is the product under the social background advocating energy-saving and emission-reduction, its environmental protection, energy-conservation, antidetonation Performance is good, has a extensive future, be described as forth generation green illumination light source in following illumination market.
GaN as one of third generation semi-conducting material representative, have direct band gap, broad stopband, The excellent properties such as high saturated electron drift velocity, high breakdown electric field and high heat conductance, at microelectronics Application aspect has obtained paying close attention to widely.P-GaN it is successfully obtained first from I.Akasaki, After realizing the new breakthrough of blue-ray LED, GaN base compound always prepares the main of LED component Material, has a wide range of applications in fields such as room lighting, commercial lighting, engineering illuminations.
High-quality GaN material is the most all made by heteroepitaxy method.As being usually used in growth The substrate of GaN, sapphire has stable physicochemical properties, but exists the biggest between it and GaN Lattice mismatch (16%) and thermal mismatching (25%), the GaN film causing growth is second-rate； Although the lattice mismatch of SiC with GaN only 3.5%, thermal conductivity is higher, but its thermal mismatching with Sapphire is quite (25.6%), poor with the wettability of GaN, expensive, and extension Technology is monopolized by Creat Company of the U.S., the most also cannot commonly use.Under comparing relatively, Si Substrate has low cost, monocrystalline size is big and quality is high, thermal conductivity is high, electric conductivity is good Various features, and the microelectric technique of Si is the most ripe, and growth GaN is thin on a si substrate Film is expected to realize photoelectron and microelectronic integrated.
Exactly because the above-mentioned plurality of advantages of Si substrate, Si Grown GaN film and then Preparation LED increasingly receives much concern.But, prepare GaN the most on a si substrate The quality of monocrystal thin films is not so good as Sapphire Substrate, mainly due to: Si Yu GaN thermal mismatching is far away Higher than sapphire, epitaxial wafer is caused to be easier to be full of cracks；It is easy in interface that Si substrate meets activity N Form unbodied SixNy, affect the growth quality of GaN；The Si Absorption to visible ray Also LED luminous efficiency can be substantially reduced.
As can be seen here, even if Si substrate has the advantage such as low cost, good heat dissipation, have very Good development prospect, but to grow high-quality GaN thin film and then preparation LED on a si substrate Epitaxial wafer, needs to find new method and the technique of Si Grown LED.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, an object of the present invention is to carry For a kind of growth LED on a si substrate, have that performance is good, crystal mass is high Feature.
The two of the purpose of the present invention are to provide the preparation method of above-mentioned LED, use this The LED that method obtains has the advantages that performance is good, crystal mass is high, is suitably applied in In LED component.
Realize the purpose of the present invention to reach by adopting the following technical scheme that:
A kind of growth LED on a si substrate, it is characterised in that: it includes that Si serves as a contrast The end, a growth AlN cushion on a si substrate, on an AlN cushion successively Grow the 2nd AlN cushion, AlGaN stepping cushion, u-GaN layer, n-GaN layer, InGaN/GaN quantum well layer and p-GaN layer；The crystal orientation of described Si substrate is that (111) are brilliant Facing inclined 0.5-1 ° of (100) direction, this angle of chamfer can be effectively improved the table of GaN epitaxial film Face pattern, reduce dislocation density and improve the crystal mass of GaN.
Preferably, the thickness of a described AlN cushion is 10-100nm；Described 2nd AlN The thickness of cushion is 10-50nm.
Preferably, described AlGaN stepping cushion comprises three layers, is from bottom to top followed successively by: the One AlGaN layer, the second AlGaN layer and the 3rd AlGaN layer；Wherein, first AlGaN layer Thickness is 80-150nm；The thickness of the second AlGaN layer is 100-200nm；3rd AlGaN The thickness of layer is 200-300nm；First AlGaN layer, the second AlGaN layer and the 3rd AlGaN In Ceng, the doping of Al reduces successively.
A kind of preparation method of growth LED on a si substrate, it is characterised in that: Use Si substrate, choose (111) crystal face crystalline substance towards inclined 0.5-1 ° of (100) direction of Si substrate Body is orientated, and first grows an AlN cushion, then grow successively the 2nd AlN cushion, AlGaN stepping cushion, u-GaN layer, n-GaN layer, InGaN/GaN quantum well layer and p-GaN Layer.
Preferably, pulse laser deposition process growth the oneth AlN cushion, process conditions are used For: underlayer temperature is 650-850 DEG C, and chamber pressure is 1-10m Torr, and V/III ratio is 30-50, the speed of growth is 0.5-0.7ML/s.
Preferably, use metal organic chemical vapor deposition technique growth the 2nd AlN cushion, Process conditions are: underlayer temperature is 860-960 DEG C, and chamber pressure is 50-100Torr, V / III ratio is 1000-2500, and the speed of growth is 0.1-0.2 μm/h.
Preferably, metal organic chemical vapor deposition technique growth AlGaN stepping buffering is used Layer, process conditions are: keeping substrate to be 960-1060 DEG C, chamber pressure is 50-100Torr, NH3Flow is under the conditions of 10-15slm, TMAl flow is 200-250sccm, by changing TMGa flow and growth rate, obtain: the first AlGaN layer, the 2nd AlGaN the most successively Layer and the 3rd AlGaN layer；Wherein, the thickness of the first AlGaN layer is 80-150nm；Second The thickness of AlGaN layer is 100-200nm；The thickness of the 3rd AlGaN layer is 200-300nm； In first AlGaN layer, the second AlGaN layer and the 3rd AlGaN layer, the doping of Al drops successively Low.
Preferably, changing TMGa flow and growth rate, specific practice is as follows: TMGa flow For 5-10sccm, growth rate is 0.2-0.3 μm/h, grows the first AlGaN layer, Al Doping be 70-85%；TMGa flow is 20-30sccm, and growth rate is 0.3-0.4 μm/h, grows the second AlGaN layer, and the doping of Al is 50-65%；TMGa flow is 65-75 Sccm, growth rate is 0.5-0.7 μm/h, grows the i.e. the 3rd AlGaN layer, and Al mixes Miscellaneous amount is 20-35%.
Preferably, metal organic chemical vapor deposition technique growth u-GaN layer, technique bar are used Part is: underlayer temperature is 1000-1060 DEG C, and chamber pressure is 150-220Torr, V/ III ratio is 2500-3000, and the speed of growth is 3.0-3.5 μm/h.
Preferably, metal organic chemical vapor deposition technique growth n-GaN layer, technique bar are used Part is: underlayer temperature is 1000-1100 DEG C, and chamber pressure is 150-220Torr, V/ III ratio is 2000-4000, and the speed of growth is 3.0-4.0 μm/h.
Preferably, before growing AIN cushion, Si substrate is carried out successively surface clean, Annealing process step, to remove oxide and the impurity particle of Si substrate surface.
The concrete grammar of surface clean is: Si substrate is firstly placed on ultrasonic cleaning in acetone soln, Put ultrasonic cleaning in deionized water the most again；Then ultrasonic cleaning in isopropyl acetone solution；So After ultrasonic cleaning in a solution of hydrofluoric acid, then soak in deionized water；Again Si substrate is put The mixed solution of sulphuric acid and hydrogen peroxide soaks；Finally Si substrate is put in Fluohydric acid. and soak Bubble, with deionized water rinsing, nitrogen dries up.
The concrete grammar of annealing is: by Si substrate high-temperature baking at 900-1000 DEG C 3-5h。
Preferably, the thickness of an AlN cushion is 10-100nm；2nd AlN cushion Thickness be 10-50nm.
The beneficial effects of the present invention is:
(1) present invention uses pulse laser deposition process to grow an AlN cushion in advance, Needed for avoiding using metal organic chemical vapor deposition technique growing AIN, process overlays Al work Sequence, prevents because overlaying the uneven AlN Quality Down caused of Al.The AlN of the method growth Buffer-layer surface is smooth, and the metal organic chemical vapor deposition offer for the next stage well grows mould Plate.
(2) present invention is on a prefabricated AlN cushion, continues to use Organometallic Learn gas-phase deposition growth the 2nd AlN cushion, reach the smooth transition of technique conversion.
(3) three layers of AlGaN stepping cushion that the present invention uses, it is possible to effectively alleviate because of GaN And the tensile stress that lattice mismatch huge between Si and thermal mismatching cause, extends outward flawless GaN film, reduces leakage current, improves the electric property of LED.
(4) present invention adopts pulse laser deposition process metal organic chemical vapor deposition work Skill with combine, first low-temperature epitaxy AlN cushion, prevent Si from high temperature diffusing to AlN Cushion destroys surface topography, then high growth temperature LED epitaxial layer, to improve the equal of GaN film Even property and the speed of growth.
In sum, the present invention uses Si to be substrate, in combination with Metallo-Organic Chemical Vapor Depositing operation and pulse laser deposition process, avoid using metal organic chemical vapor deposition technique Needed for growing AIN process overlay Al operation, prevent Si under high temperature from diffusing to AlN cushion Destroy surface topography, it is thus achieved that LED performance good, crystal mass is high, be suitably applied in In LED component.
Accompanying drawing explanation
Fig. 1 is the growth LED schematic cross-section on a si substrate of the present invention.
Fig. 2 is the growth LED X-ray on a si substrate of the embodiment of the present invention 1 Swing curve figure.
Fig. 3 is the growth LED X-ray on a si substrate of the embodiment of the present invention 2 Swing curve figure.
Fig. 4 is the growth LED X-ray on a si substrate of the embodiment of the present invention 3 Swing curve figure.
Fig. 5 is the PL spectrum of the growth LED on a si substrate of the embodiment of the present invention 3 Test figure.
Detailed description of the invention
Below, in conjunction with detailed description of the invention, the present invention is described further:
Embodiment 1:
Refer to Fig. 1, the growth of present invention LED on a si substrate includes that Si serves as a contrast The end the 11, the oneth AlN cushion the 12, the 2nd AlN cushion 13, AlGaN stepping cushion 14, u-GaN layer 15, n-GaN layer 16, InGaN/GaN quantum well layer 17 and p-GaN layer 18；
Above-mentioned growth LED on a si substrate is adopted and is obtained with the following method:
(1) the choosing of substrate and its crystal orientation: use Si substrate, choose (111) face inclined (100) crystal orientation in 0.5 ° of direction.
(2) using pulse laser deposition process growth the oneth AlN cushion, process conditions are: Underlayer temperature is 650 DEG C, and chamber pressure is 1mTorr, and V/III ratio is 30, the speed of growth For 0.5ML/s, the thickness of an AlN cushion is 20nm.
(3) metal organic chemical vapor deposition technique growth the 2nd AlN cushion, work are used Skill condition is: underlayer temperature is 860 DEG C, and chamber pressure is 50Torr, and V/III ratio is 2000, The speed of growth is 0.2 μm/h, and the thickness of the 2nd AlN cushion is 30nm.
(4) metal organic chemical vapor deposition technique growth AlGaN stepping cushion is used, Process conditions are: keeping substrate is 960 DEG C, and chamber pressure is 50Torr, NH3Flow is Under the conditions of 10slm, TMAl flow is 200sccm, change TMGa flow and the speed of growth, Ground floor is 5sccm, and the speed of growth is 0.2 μm/h, grows 90nm thickness AlGaN thin film, The doping of Al is 85%；The second layer is 20sccm, and the speed of growth is 0.4 μm/h, growth 120nm thickness AlGaN thin film, the doping of Al is 65%；Third layer is 65sccm, growth Speed is 0.5 μm/h, grows 200nm thickness AlGaN thin film, and the doping of Al is 35%.
(5) metal organic chemical vapor deposition technique growth u-GaN layer, process conditions are used For: underlayer temperature is 1000 DEG C, and chamber pressure is 150Torr, and V/III ratio is 3000, The speed of growth is 3.0 μm/h, and the thickness of u-GaN layer is 1 μm.
(6) metal organic chemical vapor deposition technique growth n-GaN layer, process conditions are used For: underlayer temperature is 1000 DEG C, and chamber pressure is 150Torr, and V/III ratio is 3000, The speed of growth is 3.5 μm/h, and the thickness of n-GaN layer is 2 μm.
(7) metal organic chemical vapor deposition technique growth InGaN/GaN quantum well layer is used, Process conditions are: underlayer temperature is 1000 DEG C, and chamber pressure is 150Torr, V/III ratio Being 2500, the speed of growth is 0.6 μm/h, and the thickness of InGaN/GaN quantum well layer is 75nm.
(8) metal organic chemical vapor deposition technique growth p-GaN layer, process conditions are used For: underlayer temperature is 1000 DEG C, and chamber pressure is 150Torr, and V/III ratio is 3500, The speed of growth is 0.5 μm/h, and the thickness of p-GaN layer is 200nm.
Refer to Fig. 2, from X-ray swing curve figure it will be seen that in LED Half-peak breadth (FWHM) value of GaN (002) is 391arcsec, outside showing on Si (111) face Epitaxial growth has gone out the high-quality LED of fabricating low-defect-density.
Embodiment 2:
The feature of the present embodiment is:
Described growth LED on a si substrate is adopted and is obtained with the following method:
(1) the choosing of substrate and its crystal orientation: use Si substrate, choose (111) face inclined (100) crystal orientation in 1 ° of direction.
(2) using pulse laser deposition process growth the oneth AlN cushion, process conditions are: Underlayer temperature is 850 DEG C, and chamber pressure is 10mTorr, and V/III ratio is 45, the speed of growth For 0.6ML/s, the thickness of an AlN cushion is 10nm.
(3) metal organic chemical vapor deposition technique growth the 2nd AlN cushion, work are used Skill condition is: underlayer temperature is 960 DEG C, and chamber pressure is 100Torr, and V/III ratio is 2500, the speed of growth is 0.1 μm/h, and the thickness of the 2nd AlN cushion is 40nm.
(4) metal organic chemical vapor deposition technique growth AlGaN stepping cushion is used, Process conditions are: keeping substrate is 1060 DEG C, and chamber pressure is 100Torr, NH3Flow Under the conditions of being 250sccm for 15slm, TMAl flow, change TMGa flow and the speed of growth, Ground floor is 10sccm, and the speed of growth is 0.3 μm/h, and growth 120nm thickness AlGaN is thin Film, the doping of Al is 80%；The second layer is 25sccm, and the speed of growth is 0.3 μm/h, Growth 150nm thickness AlGaN thin film, the doping of Al is 60%；Third layer is 70sccm, The speed of growth is 0.6 μm/h, grows 250nm thickness AlGaN, and the doping of Al is 30%.
(5) metal organic chemical vapor deposition technique growth u-GaN layer, process conditions are used For: underlayer temperature is 1060 DEG C, and chamber pressure is 220Torr, and V/III ratio is 2500, The speed of growth is 3.5 μm/h, and the thickness of u-GaN layer is 1.5 μm.
(6) metal organic chemical vapor deposition technique growth n-GaN layer, process conditions are used For: underlayer temperature is 1100 DEG C, and chamber pressure is 220Torr, and V/III ratio is 4000, The speed of growth is 3.0 μm/h, and the thickness of n-GaN layer is 2.5 μm.
(7) metal organic chemical vapor deposition technique growth InGaN/GaN quantum well layer is used, Process conditions are: underlayer temperature is 1060 DEG C, and chamber pressure is 220Torr, V/III ratio Being 3000, the speed of growth is 0.7 μm/h, and the thickness of InGaN/GaN quantum well layer is 85nm.
(8) metal organic chemical vapor deposition technique growth p-GaN layer, process conditions are used For: underlayer temperature is 1060 DEG C, and chamber pressure is 220Torr, and V/III ratio is 3000, The speed of growth is 0.4 μm/h, and the thickness of p-GaN layer is 250nm.
Refer to Fig. 3, from X-ray swing curve figure it will be seen that in LED Half-peak breadth (FWHM) value of GaN (002) is 388arcsec, outside showing on Si (111) face Epitaxial growth has gone out the high-quality LED of fabricating low-defect-density.
Embodiment 3:
The present embodiment is changed one's profession on the basis of embodiment 1, and difference is: Before growing AIN cushion, substrate is carried out successively surface clean, annealing process step, specifically Method is as follows:
Surface cleaning processing: Si substrate is firstly placed on ultrasonic cleaning in acetone soln, the most again Put ultrasonic cleaning in deionized water；Then ultrasonic cleaning in isopropyl acetone solution；Then at hydrogen Ultrasonic cleaning in fluorspar acid solution, then soak in deionized water；Again Si substrate is placed on sulphuric acid Soak with in the mixed solution of hydrogen peroxide；Finally Si substrate is put in Fluohydric acid. and soak, use Deionized water rinsing, nitrogen dries up.
Annealing: by substrate high-temperature baking 3-5h at 900-1000 DEG C.
Refer to Fig. 4, from X-ray swing curve figure it will be seen that in LED Half-peak breadth (FWHM) value of GaN (002) is 375arcsec, outside showing on Si (111) face Epitaxial growth has gone out the high-quality LED of fabricating low-defect-density.
Refer to Fig. 5, from PL spectrum test figure it will be seen that the emission wavelength of LED is 438nm, PL half-peak breadth (FWHM) value is 19nm, shows that extension is raw on Si (111) face Long LED has the optical property of excellence.
For a person skilled in the art, can technical scheme as described above and structure Think, make other various corresponding changes and deformation, and all these changes and deformation Within all should belonging to the protection domain of the claims in the present invention.

Claims (8)

1. growth LED on a si substrate, it is characterised in that: it includes that Si serves as a contrast The end, a growth AlN cushion on a si substrate, on an AlN cushion successively Grow the 2nd AlN cushion, AlGaN stepping cushion, u-GaN layer, n-GaN layer, InGaN/GaN quantum well layer and p-GaN layer；The crystal orientation of described Si substrate is that (111) are brilliant Face inclined 0.5-1 ° of (100) direction；
Wherein, using pulse laser deposition process growth the oneth AlN cushion, process conditions are: Underlayer temperature is 650-850 DEG C, and chamber pressure is 1-10m Torr, and V/III ratio is 30-50, The speed of growth is 0.5-0.7ML/s；
Use metal organic chemical vapor deposition technique growth the 2nd AlN cushion, process conditions For: underlayer temperature is 860-960 DEG C, and chamber pressure is 50-100Torr, and V/III ratio is 1000-2500, the speed of growth is 0.1-0.2 μm/h.
Growth the most according to claim 1 LED on a si substrate, it is special Levy and be: described AlGaN stepping cushion comprises three layers, is from bottom to top followed successively by: first AlGaN layer, the second AlGaN layer and the 3rd AlGaN layer；Wherein, the thickness of the first AlGaN layer Degree is 80-150nm；The thickness of the second AlGaN layer is 100-200nm；3rd AlGaN layer Thickness be 200-300nm；First AlGaN layer, the second AlGaN layer and the 3rd AlGaN In Ceng, the doping of Al reduces successively.
3. the preparation method growing LED on a si substrate, it is characterised in that: Use Si substrate, choose (111) crystal face crystalline substance towards inclined 0.5-1 ° of (100) direction of Si substrate Body is orientated, and first grows an AlN cushion, then grow successively the 2nd AlN cushion, AlGaN stepping cushion, u-GaN layer, n-GaN layer, InGaN/GaN quantum well layer and p-GaN Layer；
Wherein, using pulse laser deposition process growth the oneth AlN cushion, process conditions are: Underlayer temperature is 650-850 DEG C, and chamber pressure is 1-10m Torr, and V/III ratio is 30-50, The speed of growth is 0.5-0.7ML/s；
Use metal organic chemical vapor deposition technique growth the 2nd AlN cushion, process conditions For: underlayer temperature is 860-960 DEG C, and chamber pressure is 50-100Torr, and V/III ratio is 1000-2500, the speed of growth is 0.1-0.2 μm/h.
The preparation of growth the most according to claim 3 LED on a si substrate Method, it is characterised in that: use the growth AlGaN stepping of metal organic chemical vapor deposition technique Cushion, process conditions are: keeping substrate to be 960-1060 DEG C, chamber pressure is 50-100 Torr, NH3Flow is under the conditions of 10-15slm, TMAl flow is 200-250sccm, logical Cross change TMGa flow and growth rate, obtain the most successively: the first AlGaN layer, Second AlGaN layer and the 3rd AlGaN layer；Wherein, the thickness of the first AlGaN layer is 80-150 nm；The thickness of the second AlGaN layer is 100-200nm；The thickness of the 3rd AlGaN layer is 200-300nm；Al in first AlGaN layer, the second AlGaN layer and the 3rd AlGaN layer Doping reduces successively.
The preparation of growth the most according to claim 4 LED on a si substrate Method, it is characterised in that: changing TMGa flow and growth rate, specific practice is as follows: TMGa Flow is 5-10sccm, and growth rate is 0.2-0.3 μm/h, grows the first AlGaN layer. Doping 70-85% of Al；TMGa flow is 20-30sccm, and growth rate is 0.3-0.4 μm/h, grows the second AlGaN layer, doping 50-65% of Al；TMGa flow is 65-75 Sccm, growth rate is 0.5-0.7 μm/h, grows the 3rd AlGaN layer, the doping of Al Amount 20-35%.
The preparation of growth the most according to claim 3 LED on a si substrate Method, it is characterised in that: use metal organic chemical vapor deposition technique growth u-GaN layer, Process conditions are: underlayer temperature is 1000-1060 DEG C, and chamber pressure is 150-220Torr, V/III ratio is 2500-3000, and the speed of growth is 3.0-3.5 μm/h.
The preparation of growth the most according to claim 3 LED on a si substrate Method, it is characterised in that: use metal organic chemical vapor deposition technique growth n-GaN layer, Process conditions are: underlayer temperature is 1000-1100 DEG C, and chamber pressure is 150-220Torr, V/III ratio is 2000-4000, and the speed of growth is 3.0-4.0 μm/h.
The preparation of growth the most according to claim 3 LED on a si substrate Method, it is characterised in that: before growing AIN cushion, Si substrate is carried out successively table Face is cleaned, annealing process step；
The concrete grammar of surface clean is: Si substrate is firstly placed on ultrasonic cleaning in acetone soln, Put ultrasonic cleaning in deionized water the most again；Then ultrasonic cleaning in isopropyl acetone solution；So After ultrasonic cleaning in a solution of hydrofluoric acid, then soak in deionized water；Again Si substrate is put The mixed solution of sulphuric acid and hydrogen peroxide soaks；Finally Si substrate is put in Fluohydric acid. and soak Bubble, with deionized water rinsing, nitrogen dries up；
The concrete grammar of annealing is: by Si substrate high-temperature baking at 900-1000 DEG C 3-5h。
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