CN105576096B - A kind of preparation method of the LED epitaxial wafer grown on a si substrate using SiN insert layers - Google Patents
A kind of preparation method of the LED epitaxial wafer grown on a si substrate using SiN insert layers Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000012010 growth Effects 0.000 claims description 78
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 2
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- 238000011065 in-situ storage Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
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- 238000002017 high-resolution X-ray diffraction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
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- 238000003780 insertion Methods 0.000 description 1
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers 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 having potential barriers 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 having potential barriers 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- 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
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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Abstract
The present invention discloses a kind of LED epitaxial wafer and preparation method thereof grown on a si substrate using SiN insert layers, LED epitaxial wafer is specifically grown using Metal Organic Vapor extension on a si substrate, structure includes Si substrate layers, is grown in the AlN buffer layers of Si substrate layers successively, stepping AlxGa1‑xN buffer layers, AlN insert layers, the islands lower layer three-dimensional GaN layer, original position SiN insert layers, the upper layer islands three-dimensional GaN layer, n GaN layers, InGaN/GaN multiple quantum well layers and p GaN layers.The features such as LED epitaxial wafer has residual stress low on the Si substrates of the present invention, and defect concentration is small, and crystal quality is good, and photoelectric properties are excellent.
Description
Technical field
The invention belongs to technical field of semiconductors, and in particular to a kind of to be existed using Metal Organic Vapor epitaxy technology
Si Grown LED epitaxial wafer.
Background technology
It is common technology at this stage to prepare light emitting diode (LED) using GaN and its relevant III group semi-conducting material
Means, however cost problem is always an important factor for hindering LED technology extension.Nowadays, the growth technique of Si monocrystalline body maturation
Large-area high-quality Si substrates can be obtained with lower cost, the manufacturing cost of LED is effectively reduced in Si substrate growths LED, and
And suitable for the preparation of high power LED device.
Although Si tools have many advantages, the GaN single crystal film quality prepared on a si substrate is precious not as good as traditional indigo plant
Stone lining bottom, and the lattice mismatch of Si and GaN is larger (about 16%), the GaN epitaxial layer defect grown on Si is difficult to realize count
Magnitude is reduced.Meanwhile Si is up to 114% with GaN thermal mismatchings, and epitaxial layer is caused to generate huge tensile stress, it is outer to easily cause
Prolong layer cracking.
Currently, existing multiple technologies realize growth high-quality GaN film on a si substrate both at home and abroad.SiN insert layers in situ
Technology can realize three-dimensional GaN island growths, inhibits dislocation defects and improve the crystal quality of GaN film on Si substrates, improve LED
Device performance and reliability, become the LED technologies of preparing of mainstream.However, traditional SiN insert layers in situ are usually sunk
For product on the GaN masterplates that two dimensional surface is grown, this depositional mode easilys lead to the remnants of the LED films of extension on Si substrates
Stress increases, and film surface is caused to form micro-crack.The reliability and applicability of the technology in order to further increase, needs to seek
A kind of method overcomes traditional original position SiN insert layers defect present in Stress Control.
Invention content
In view of the deficiencies of the prior art, a kind of use original position SiN insert layers provided by the invention are grown on a si substrate
LED epitaxial wafer provides that a kind of residual stress is low, defect concentration is small, crystal by introducing a kind of novel SiN insert layer structures
LED epitaxial wafer high-quality, photoelectric properties are excellent.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of LED epitaxial wafer grown on a si substrate using SiN insert layers, it is characterised in that：Including Si substrate layers, according to
AlN buffer layer, stepping Al of the secondary growth on Si substrate layersxGa1-xN buffer layers, AlN insert layers, the islands lower layer three-dimensional GaN layer, original
Position SiN insert layers, the upper layer islands three-dimensional GaN layer, n-GaN layers, InGaN/GaN multiple quantum well layers and p-GaN layer.
Preferably, the thickness of the AlN buffer layers is 90-110nm.
Preferably, the stepping AlxGa1-xN buffer layers include the Al grown successively0.2Ga0.8N buffer layers, Al0.5Ga0.5N
Buffer layer, Al0.8Ga0.2N buffer layers, wherein Al0.2Ga0.8N buffer layer thicknesses are 95-105nm, the Al0.5Ga0.5N buffer layers
Thickness is 140-155nm, the Al0.8Ga0.2N buffer layer thicknesses are 185-210nm.
Preferably, the thickness of the AlN insert layers is 30-45nm.
Preferably, the islands the lower layer's three-dimensional GaN layer is made of several consistency of thickness and mutually independent island, wherein mutually
The thickness on independent island is 30-200nm, and the average thickness of the islands the lower layer three-dimensional GaN layer formed by mutually independent island is 145-
155nm。
Preferably, the islands the lower layer's three-dimensional GaN layer, original position SiN insert layers, the overall thickness of the upper layer islands three-dimensional GaN layer are
500-1500nm。
A method of the LED epitaxial wafer grown on a si substrate using SiN insert layers is prepared, it is characterized in that：Packet
Include following steps：
(1) Si substrates are prepared：Single crystal Si substrate is put into room temperature in 15%HF solution to be cleaned by ultrasonic 15-20 seconds, removes table
Face pickup particle, then ethyl alcohol, deionized water is used to be cleaned by ultrasonic successively, it is finally dried up with high-purity drying nitrogen spare；
(2) growing AIN buffer layer：Take step (1) prepare Si substrates in temperature be 1000-1100 DEG C, air pressure 50-
Under the conditions of 60Torr, it is passed through the NH that flow is the trimethyl aluminium of 240-260 μm of ol/min, flow is 7.5-9slm3, then AlN
Buffer layer is that 3-4nm/s grows to thickness as 90-110nm with the speed of growth；
(3) Al is grownxGa1-xN buffer layers：Described in step (2) under the conditions of AlN buffer growths, trimethyl aluminium is maintained
Flow is constant, then passes to flow as 18-25 μm of ol/min trimethyl gallium to Al0.2Ga0.8N buffer layer thicknesses are grown to 95-
105nm；The flow of trimethyl gallium is increased into 50-60 μm of ol/min to Al again0.5Ga0.5N buffer layer thicknesses are grown to 140-
155nm；The flow of trimethyl gallium is finally increased into 80-90 μm of ol/min to Al0.8Ga0.2N buffer layer thicknesses are grown to 185-
210nm；
(4) growing AIN insert layer：By step (3) AlxOn the basis of Ga1-xN buffer layers, adjusting growth temperature is
800-850 DEG C, reative cell air pressure be 50-60Torr, it is 145-160 μm of ol/min trimethyl aluminium, flow 7- to be passed through flow
9slm NH3, then AlN insert layers with the speed of growth be 4-6nm/min in AlxGa1-x30-45nm is grown on N buffer layers；
(5) islands growth lower layer three-dimensional GaN layer：On the basis of step (4) the AlN insert layers, it is passed through trimethyl gallium, NH3,
Then mutually independent island is 30-200nm with certain growth to thickness, and mutually independent island forms average thickness
The islands the lower layer three-dimensional GaN layer that degree is 145-155nm；
(6) original position SiN insert layers are deposited：On the basis of step (5) islands the lower layer's three-dimensional GaN layer, it is passed through SiH4、NH3,
Deposit 30-180s；
(7) the growth upper layer islands three-dimensional GaN layer：On the basis of step (6) the original position SiN insert layers, be passed through trimethyl aluminium,
NH3, then the islands lower layer's three-dimensional GaN are with certain growth speed to the islands lower layer three-dimensional GaN, original position SiN insert layers and upper layer three-dimensional GaN
The overall thickness of island layer is 500-1500nm；
(8) on the layer of step (7) islands upper layer three-dimensional GaN successively growth thickness be 2-4 μm, Si mix it is a concentration of
5x1018cm-3N-GaN layers, the GaN that the InGaN and thickness that staggered thickness is 3-4nm are 11-13nm, staggered 10
A period-producer InGaN/GaN multiple quantum well layers and thickness are 200-210nm p-GaN layers.
Preferably, the detailed process of the islands growth lower layer three-dimensional GaN layer is in the step (5), in step (4) AlN
On the basis of insert layer, adjusting growth temperature is 800-1050 DEG C, reative cell air pressure is 300-600Torr, and it is 280- to be passed through flow
320 μm of ol/min trimethyl galliums, flow are 50-70slm NH3, then mutually independent island is with the growth speed of 45-55nm/min
It is 30-200nm that degree, which grows to thickness, and mutually independent island forms the islands lower layer three-dimensional GaN that average thickness is 145-155nm
Layer.
Preferably, the detailed process of deposition original position SiN insert layers is in the step (6), in step (5) lower layer three
On the basis of tieing up the islands GaN layer, adjusting growth temperature is 1000-1100 DEG C, reative cell air pressure is 500-550Torr, is passed through flow and is
190-215μmol/min SiH4, flow be 45-60slm NH3, deposit 30-180s.
Preferably, the detailed process of the growth upper layer islands three-dimensional GaN layer is in the step (7), in step (6) original position
On the basis of SiN insert layers, it is 800-1050 DEG C to adjust growth temperature, and reative cell air pressure is 300-600Torr, and being passed through flow is
140-160 μm of ol/min trimethyl aluminium, flow are 7-9slm NH3, then the islands lower layer's three-dimensional GaN are with the 4-6nm/min speeds of growth
Overall thickness to the islands lower layer three-dimensional GaN, original position SiN insert layers and the upper layer islands three-dimensional GaN layer is 500-1500nm.
The method have the benefit that：
The present invention, which uses, is initially formed the mutually independent islands lower layer's three-dimensional GaN layer, then deposits original on the layer of the islands lower layer three-dimensional GaN
Position SiN insert layers can further strengthen the localization growth of the islands lower layer three-dimensional GaN layer, raw to enhance the islands lower layer three-dimensional GaN layer
It is long, the defect that can effectively inhibit defect concentration big.Compared to traditional SiN deposition methods in situ, original position of the present invention
The mode of the SiN insertion three-dimensionals islands GaN layer can effectively reduce the residual stress of LED epitaxial wafer, inhibit the formation of crackle, overcome
Stress Control defect existing for traditional original position SiN technologies.
Description of the drawings
Fig. 1 is the schematic diagram of the LED epitaxial wafer of present invention growth on a si substrate.
Fig. 2 is the Raman spectrogram of LED epitaxial wafer prepared by embodiment 4.
Fig. 3 is high-resolution X-ray diffraction (HRXRD) collection of illustrative plates of LED epitaxial wafer prepared by embodiment 4.
Fig. 4 is the electric current and luminous power, electric current and voltage curve of blue-light LED chip prepared by Application Example 1.
Wherein, 11, Si substrate layers；12, AlN buffer layers；13, stepping AlxGa1-xN buffer layers；14, AlN insert layers；15、
The islands lower layer three-dimensional GaN layer；16, original position SiN insert layers；17, the islands upper layer three-dimensional GaN layer；18, n-GaN layers；19, InGaN/GaN is more
Quantum well layer；20, p-GaN layer.
Specific implementation mode
As shown in Figure 1, the LED epitaxial wafer disclosed by the invention grown on a si substrate using SiN insert layers comprising Si
Substrate layer 11, AlN buffer layers 12, the stepping Al being grown in successively on Si substrate layers 11xGa1-xN buffer layers 13, AlN insert layers
14, the islands lower layer three-dimensional GaN layer 15, original position SiN insert layers 16, the upper layer islands the three-dimensional GaN layer 17 being made of mutually independent island, with
And n-GaN layers 18, InGaN/GaN multiple quantum well layers 19 and the p-GaN layer 20 grown on the upper layer islands three-dimensional GaN layer 17.
Invention is further described in detail for son in the following with reference to the drawings and specific embodiments.
Embodiment 1
The disclosed LED epitaxial wafer grown on a si substrate using SiN insert layers of the present embodiment comprising Si substrate layers
11, thickness is 90nm AlN buffer layers 12, is 95nmAl by thickness0.2Ga0.8N buffer layers, thickness are 140nm Al0.5Ga0.5N is slow
Rush layer, thickness 185nmAl0.8Ga0.2The stepping Al of N buffer layers compositionxGa1-xN buffer layers 13, thickness are that 30nm AlN are inserted into
Layer 14, be made of mutually independent island the islands lower layer three-dimensional GaN layer 15 that average thickness is 145nm, original position SiN insert layers 16, on
The total thickness of the layer three-dimensional islands GaN layer 17, the wherein islands lower layer's three-dimensional GaN layer 15, original position SiN insert layers 16, the upper layer islands three-dimensional GaN layer 17
Degree is 500, further includes that growth thickness is 2 μm of n-GaN layers 18, thickness 140nm on the upper layer islands three-dimensional GaN layer 17 successively
InGaN/GaN multiple quantum well layers 19 and thickness are 200nm p-GaN layers 20, wherein InGaN/GaN multiple quantum well layers 19 are by thickness
Degree is 3nmGaN and thickness is 11nm InGaN staggered formation successively, is arranged altogether ten periods.
The preparation method of the LED epitaxial wafer of the growth on a si substrate is as follows：
(1) Si substrate layers 11 are prepared：Single crystalline Si (111) substrate is put into room temperature in 15%HF solution and is cleaned by ultrasonic 15-20
Second, surface pickup particle is removed, then ethyl alcohol, deionized water is used to be cleaned by ultrasonic successively, is finally dried up with high-purity drying nitrogen spare；
(2) growing AIN buffer layer 12：Take Si substrate layers 11 prepared by step (1) in temperature is 1000 DEG C, air pressure is
Under the conditions of 50Torr, it is passed through the NH that flow is the trimethyl aluminium of 240 μm of ol/min, flow is 7.5slm3, then AlN buffer layers
12 with the speed of growth be that 3nm/s grows to thickness as 90nm；
(3) Al is grownxGa1-xN buffer layers 12：Under 12 growth conditions of AlN buffer layers described in step (2), front three is maintained
Base aluminum flux is constant, then passes to flow as 18 μm of ol/min trimethyl galliums to Al0.2Ga0.8N buffer layer thicknesses are grown to 95nm；
The flow of trimethyl gallium is increased into 50 μm of ol/min to Al again0.5Ga0.5N buffer layer thicknesses are grown to 140nm；Finally by front three
The flow of base gallium increases to 80 μm of ol/min to Al0.8Ga0.213 grown in thickness of N buffer layers is 185nm；
(4) growing AIN insert layer 14：In step (3) the stepping AlxOn the basis of Ga1-xN buffer layers 13, growth is adjusted
Temperature is 800 DEG C, reative cell air pressure is 50Torr, is passed through that flow is 145 μm of ol/min trimethyl aluminiums, flow is 7slm NH3,
Then AlN insert layers 14 with the speed of growth be 4nm/min in AlxGa1-x30nm is grown on N buffer layers 13；
(5) islands growth lower layer three-dimensional GaN layer 15：On the basis of step (4) AlN insert layers 14,800 are adjusted the temperature to
DEG C, reative cell air pressure be 300Torr, be passed through that flow is 280 μm of ol/min trimethyl galliums, flow is 50slm NH3, then mutually
Independent island grows to thickness as 30-200nm with speed of growth 45nm/min, the lower layer three-dimensional GaN that mutually independent island is formed
The average thickness of island layer 15 is 145nm；
(6) original position SiN insert layers 16 are deposited：On the basis of step (5) islands lower layer's three-dimensional GaN layer 15, growth is adjusted
Temperature is 1000 DEG C, reative cell air pressure is 500Torr, and it is 190 μm of ol/min SiH to be passed through flow4, flow be 545slm NH3,
Deposit 180s；
(7) the growth upper layer islands three-dimensional GaN layer 17：On the basis of step (6) original position insert layer 16 SiN, growth is adjusted
Temperature is 800 DEG C, and reative cell air pressure is 300Torr, is passed through that flow is 140 μm of ol/min trimethyl aluminiums, flow is 7slm NH3,
Then the islands upper layer three-dimensional GaN layer 17 with the 4nm/min speeds of growth to the islands lower layer three-dimensional GaN layer 15, original position SiN insert layers 16 and on
The overall thickness of the layer three-dimensional islands GaN layer 17 is 500nm；
(8) on step (7) islands upper layer three-dimensional GaN layer 17 successively growth thickness be 2 μm, Si mix it is a concentration of
5x1018cm-3N-GaN layers 18, the GaN that the InGaN and thickness that staggered thickness is 3nm are 11nm, and staggered ten
Period-producer InGaN/GaN multiple quantum well layers 19 and thickness are 200nm p-GaN layers 20.
Embodiment 2
The disclosed LED epitaxial wafer grown on a si substrate using SiN insert layers of the present embodiment comprising Si substrate layers
11, thickness is 100nm AlN buffer layers 12, is 55nmAl by thickness0.2Ga0.8N buffer layers, thickness are 150nm Al0.5Ga0.5N
Buffer layer, thickness 200nmAl0.8Ga0.2The stepping Al of N buffer layers compositionxGa1-xN buffer layers 13, thickness are inserted for 40nm AlN
Enter layer 14, average thickness is made of mutually independent island for 150nm the islands lower layer three-dimensional GaN layer 15, original position SiN insert layers 16,
The upper layer islands three-dimensional GaN layer 17, the wherein islands lower layer's three-dimensional GaN layer 15, original position SiN insert layers 16, the upper layer islands three-dimensional GaN layers 17 it is total
Thickness is 1000nm, further includes that growth thickness is that 3 μm of n-GaN layers 18, thickness are on the upper layer islands three-dimensional GaN layer 17 successively
155nm InGaN/GaN multiple quantum well layers 19 and thickness are 205nm p-GaN layers 20, wherein InGaN/GaN multiple quantum well layers 19
It is 3.5nm GaN to be by thickness and thickness is 12nm InGaN staggered formation successively, is arranged altogether ten periods.
The preparation method of the LED epitaxial wafer of the growth on a si substrate is as follows：
(1) Si substrate layers 11 are prepared：Single crystalline Si (111) substrate is put into room temperature in 15%HF solution and is cleaned by ultrasonic 15-20
Second, surface pickup particle is removed, then ethyl alcohol, deionized water is used to be cleaned by ultrasonic successively, is finally dried up with high-purity drying nitrogen spare；
(2) growing AIN buffer layer 12：Take Si substrate layers 11 prepared by step (1) in temperature is 1050 DEG C, air pressure is
Under the conditions of 55Torr, it is passed through that flow is the trimethyl aluminium of 250 μm of ol/min, flow is 8slm NH3, then AlN buffer layers 12 with
The speed of growth is that grow to thickness be 100nm to 3.5nm/s；
(3) Al is grownxGa1-xN buffer layers 13：Under 12 growth conditions of AlN buffer layers described in step (2), front three is maintained
Base aluminum flux is constant, then passes to flow as 20 μm of ol/min trimethyl galliums to Al0.2Ga0.8N buffer layer thicknesses are grown to
100nm；The flow of trimethyl gallium is increased into 55 μm of ol/min to Al again0.5Ga0.5N buffer layer thicknesses are grown to 150nm；Finally
The flow of trimethyl gallium is increased into 85 μm of ol/min to Al0.8Ga0.2N buffer layer thicknesses are grown to 200nm；
(4) growing AIN insert layer 14：In step (3) the stepping AlxOn the basis of Ga1-xN buffer layers 13, growth is adjusted
Temperature is 825 DEG C, reative cell air pressure is 55Torr, is passed through that flow is 150 μm of ol/min trimethyl aluminiums, flow is 8slm NH3,
Then AlN insert layers 14 with the speed of growth be 5nm/min in AlxGa1-x40nm is grown on N buffer layers 13；
(5) islands growth lower layer three-dimensional GaN layer 15：On the basis of step (4) the AlN insert layers, 950 are adjusted the temperature to
DEG C, reative cell air pressure be 450Torr, be passed through that flow is 300 μm of ol/min trimethyl galliums, flow is 56slm NH3, then mutually
Independent island grows to thickness as 30-200nm with speed of growth 50nm/min, the lower layer three-dimensional GaN that mutually independent island is formed
The average thickness of island layer 15 is 150nm；
(6) original position SiN insert layers 16 are deposited：On the basis of step (5) islands lower layer's three-dimensional GaN layer 15, growth is adjusted
Temperature is 1050 DEG C, reative cell air pressure is 525Torr, and it is 200 μm of ol/min SiH to be passed through flow4, flow be 50slm NH3, sink
Product 90s；
(7) the growth upper layer islands three-dimensional GaN layer 17：On the basis of step (6) the original position SiN insert layers, growth temperature is adjusted
Degree is 900 DEG C, and reative cell air pressure is 450Torr, is passed through that flow is 150 μm of ol/min trimethyl aluminiums, flow is 8slm NH3, so
The islands upper layer three-dimensional GaN layer 17 is with the 5nm/min speeds of growth to the islands lower layer three-dimensional GaN layer 15, original position SiN insert layers 16 and upper layer afterwards
The overall thickness of the three-dimensional islands GaN layer 17 is 1000nm；
(8) growth thickness is 3 μm, Si mixes a concentration of 5x10 successively on step (7) islands the upper layer three-dimensional GaN layer18cm-3N-GaN layers 18, the InGaN and thickness that staggered thickness is 3.5nm are 12nm GaN layers, staggered ten period shapes
It is 205nm p-GaN layers 20 at InGaN/GaN multiple quantum well layers 19 and thickness.
Embodiment 3
The disclosed LED epitaxial wafer grown on a si substrate using SiN insert layers of the present embodiment comprising Si substrate layers
11, thickness is 110nm AlN buffer layers 12, is 105nm Al by thickness0.2Ga0.8N buffer layers, thickness 155nm
Al0.5Ga0.5N buffer layers, thickness are 210nm Al0.8Ga0.2The stepping Al of N buffer layers compositionxGa1-xN buffer layers 13, thickness are
45nm AlN insert layers 14 are made of the islands the lower layer three-dimensional GaN layer 15 that average thickness is 155nm, original position SiN mutually independent island
Insert layer 16, the upper layer islands three-dimensional GaN layer 17, the wherein islands lower layer's three-dimensional GaN layer 15, original position SiN insert layers 16, upper layer three-dimensional GaN
The overall thickness of island layer 17 is 1500nm, further includes that growth thickness is 4 μm n-GaN layers on the upper layer islands three-dimensional GaN layer 17 successively
18, thickness is 170nm InGaN/GaN multiple quantum well layers 19 and thickness is 210nm p-GaN layers 20, wherein InGaN/GaN is more
It is 4nm GaN that quantum well layer 19, which is by thickness, and thickness is 13nm InGaN staggered formation successively, is arranged altogether ten periods.
The preparation method of the LED epitaxial wafer of the growth on a si substrate is as follows：
(1) Si substrate layers 11 are prepared：Single crystalline Si (111) substrate is put into room temperature in 15%HF solution and is cleaned by ultrasonic 15-20
Second, surface pickup particle is removed, then ethyl alcohol, deionized water is used to be cleaned by ultrasonic successively, is finally dried up with high-purity drying nitrogen spare；
(2) growing AIN buffer layer 12：Take Si substrate layers 11 prepared by step (1) in temperature is 1100 DEG C, air pressure is
Under the conditions of 60Torr, it is passed through that flow is the trimethyl aluminium of 260 μm of ol/min, flow is 9slm NH3, then AlN buffer layers 12 with
The speed of growth is that grow to thickness be 110nm to 4nm/s；
(3) Al is grownxGa1-xN buffer layers 13：Under 12 growth conditions of AlN buffer layers described in step (2), front three is maintained
Base aluminum flux is constant, then passes to flow as 25 μm of ol/min trimethyl galliums to Al0.2Ga0.8N buffer layer thicknesses are grown to
105nm；The flow of trimethyl gallium is increased into 60 μm of ol/min to Al again0.5Ga0.5N buffer layer thicknesses are grown to 155nm；Finally
The flow of trimethyl gallium is increased into 90 μm of ol/min to Al0.8Ga0.2N buffer layer thicknesses are grown to 210nm；
(4) growing AIN insert layer 14：In step (3) the stepping AlxOn the basis of Ga1-xN buffer layers 13, growth is adjusted
Temperature is 850 DEG C, reative cell air pressure is 60Torr, is passed through that flow is 160 μm of ol/min trimethyl aluminiums, flow is 9slm NH3,
Then AlN insert layers 14 with the speed of growth be 6nm/min in AlxGa1-x45nm is grown on N buffer layers 13；
(5) islands growth lower layer three-dimensional GaN layer 15：On the basis of step (4) AlN insert layers 14,105 are adjusted the temperature to
DEG C, reative cell air pressure be 600Torr, be passed through that flow is 320 μm of ol/min trimethyl galliums, flow is 70slm NH3, then mutually
Independent island grows to thickness as 30-200nm with speed of growth 70nm/min, the lower layer three-dimensional GaN that mutually independent island is formed
The average thickness of island layer 15 is 155nm；
(6) original position SiN insert layers 16 are deposited：On the basis of step (5) islands lower layer's three-dimensional GaN layer 15, growth is adjusted
Temperature is 1100 DEG C, reative cell air pressure is 550Torr, and it is 215 μm of ol/min SiH to be passed through flow4, flow be 60slm NH3, sink
Product 30s；
(7) the growth upper layer islands three-dimensional GaN layer 17：On the basis of step (6) original position insert layer 16 SiN, growth is adjusted
Temperature is 1050 DEG C, and reative cell air pressure is 600Torr, and it is 160 μm of ol/min trimethyl aluminiums, flow 9slm to be passed through flow
NH3, then the islands upper layer three-dimensional GaN layer 17 is with the 6nm/min speeds of growth to the islands lower layer three-dimensional GaN layer 15, original position SiN insert layers 16
Overall thickness with the upper layer islands three-dimensional GaN layer 17 is 1500nm；
(8) on step (7) islands upper layer three-dimensional GaN layer 17 successively growth thickness be 4 μm, Si mix it is a concentration of
5x1018cm-3N-GaN layers 18, the InGaN and thickness that staggered thickness is 4nm are 13nm GaN layers, staggered ten
Period-producer InGaN/GaN multiple quantum well layers 19 and thickness are 210nm p-GaN layers 20.
Embodiment 4
The present embodiment is improved on the basis of embodiment 3, and difference is：In the preparation process of LED epitaxial wafer,
The sedimentation time of SiN insert layers 16 in situ is 35s, and under the conditions of not changing the islands lower layer three-dimensional GaN 15 average thickness of layer, lower layer
The overall thickness of the three-dimensional islands GaN layer 15, original position SiN insert layers 16 and the upper layer islands three-dimensional GaN layer 17 is 1100nm.
LED epitaxial wafer has lower residual stress and excellent crystal quality, Fig. 2 on Si substrates manufactured in the present embodiment
It is the Raman spectrogram of LED epitaxial wafer manufactured in the present embodiment, wherein GaN E2(high) wave crest at peak is 567.02cm-1With nothing
Stress GaN E2(high) 567.5cm-1Peak position is very close, illustrates that the residual stress of this sample is smaller.Fig. 3 is the present embodiment
The X-ray swing curve of the LED epitaxial wafer of preparation, half-peak breadth (FWHM) value of the X-ray swing curve of GaN (0002) down to
Half-peak breadth (FWHM) value of the X-ray swing curve of 339arcsec, GaN (10-12) shows down to 386arcsec in Si substrates
On, the LED epitaxial wafer of growth has the characteristics that residual stress is low, defect concentration is small, crystal quality is good, photoelectric properties are excellent.
Application Example 1
LED epitaxial wafer prepared by Example 3, light emitting diode (LED) chip with vertical structure is prepared by the LED epitaxial wafer in embodiment 3, is had
Body process is as follows：First epitaxial wafer is cleaned, Ti/Ag/Ti/Au is then deposited successively on p-GaN layer surface, then by another piece
It is bonded with p-GaN layer surface after the upper same metal of N-shaped (100) face surfaces Si vapor deposition, the method for then using chemical attack
Removal is outer to adopt Si substrates, obtains the surfaces AlN, then ICP is used to etch, expose n-GaN layer surfaces, and in n-GaN layers of table
Cr/Pt/Au electrodes are deposited in face successively, are finally packaged using epoxy resin.As shown in figure 4, the blue-ray LED after encapsulation exists
Under the operating current of 350mA, optical output power 483mW, working voltage 3.1V.
For those skilled in the art, technical solution that can be as described above and design are made other each
Kind is corresponding to be changed and deforms, and all these change and deform the protection model that should all belong to the claims in the present invention
Within enclosing.
Claims (4)
1. a kind of preparation method of the LED epitaxial wafer grown on a si substrate using SiN insert layers, it is characterised in that：It is described to adopt
The LED epitaxial wafer grown on a si substrate with SiN insert layers includes：Si substrate layers, the AlN being grown in successively on Si substrate layers are slow
Rush layer, stepping AlxGa1-xN buffer layers, AlN insert layers, the islands lower layer three-dimensional GaN layer, original position SiN insert layers, the upper layer islands three-dimensional GaN
Layer, n-GaN layers, InGaN/GaN multiple quantum well layers and p-GaN layer；
The preparation method comprises the following steps：
(1) Si substrates are prepared：Single crystal Si substrate is put into room temperature in 15%HF solution to be cleaned by ultrasonic 15-20 seconds, removal surface is viscous
Dirty particle, then ethyl alcohol, deionized water is used to be cleaned by ultrasonic successively, it is finally dried up with high-purity drying nitrogen spare；
(2) growing AIN buffer layer：Take step (1) prepare Si substrates in temperature be 1000-1100 DEG C, air pressure 50-60Torr
Under the conditions of, it is passed through the NH that flow is the trimethyl aluminium of 240-260 μm of ol/min, flow is 7.5-9slm3, then AlN buffer layers
It is that 3-4nm/s grows to thickness as 90-110nm with the speed of growth；
(3) Al is grownxGa1-xN buffer layers：Described in step (2) under the conditions of AlN buffer growths, trimethyl aluminium flow is maintained
It is constant, flow is then passed to as 18-25 μm of ol/min trimethyl gallium to Al0.2Ga0.8N buffer layer thicknesses are grown to 95-105nm；
The flow of trimethyl gallium is increased into 50-60 μm of ol/min to Al again0.5Ga0.5N buffer layer thicknesses are grown to 140-155nm；Most
The flow of trimethyl gallium is increased into 80-90 μm of ol/min to Al afterwards0.8Ga0.2N buffer layer thicknesses are grown to 185-210nm；
(4) growing AIN insert layer：By step (3) AlxOn the basis of Ga1-xN buffer layers, adjusting growth temperature is 800-850
DEG C, reative cell air pressure be 50-60Torr, be passed through that flow is 145-160 μm of ol/min trimethyl aluminium, flow is 7-9slm NH3,
Then AlN insert layers with the speed of growth be 4-6nm/min in AlxGa1-x30-45nm is grown on N buffer layers；
(5) islands growth lower layer three-dimensional GaN layer：On the basis of step (4) the AlN insert layers, it is passed through trimethyl gallium, NH3, then
Mutually independent island is 30-200nm with certain growth to thickness, and mutually independent island formation average thickness is
The islands the lower layer three-dimensional GaN layer of 145-155nm；
(6) original position SiN insert layers are deposited：On the basis of step (5) islands the lower layer's three-dimensional GaN layer, it is passed through SiH4、NH3, deposition
30-180s；
(7) the growth upper layer islands three-dimensional GaN layer：On the basis of step (6) the original position SiN insert layers, it is passed through trimethyl aluminium, NH3,
Then the islands lower layer's three-dimensional GaN are with certain growth speed to the islands lower layer three-dimensional GaN, original position SiN insert layers and the upper layer islands three-dimensional GaN layer
Overall thickness be 500-1500nm；
(8) growth thickness is 2-4 μm, Si mixes a concentration of 5x10 successively on step (7) islands the upper layer three-dimensional GaN layer18cm-3's
N-GaN layers, the GaN that the InGaN and thickness that staggered thickness is 3-4nm are 11-13nm, staggered 10 period-producers
InGaN/GaN multiple quantum well layers and thickness are 200-210nm p-GaN layers.
2. the preparation method of the LED epitaxial wafer according to claim 1 grown on a si substrate using SiN insert layers,
It is characterized in that：The detailed process of the islands growth lower layer three-dimensional GaN layer is in the step (5), in step (4) the AlN insert layers
On the basis of, adjusting growth temperature is 800-1050 DEG C, reative cell air pressure is 300-600Torr, and it is 280-320 μ to be passed through flow
Mol/min trimethyl galliums, flow are 50-70slm NH3, then mutually independent island is with the speed of growth life of 45-55nm/min
Length to thickness is 30-200nm, and mutually independent island forms the islands the lower layer three-dimensional GaN layer that average thickness is 145-155nm.
3. the preparation method of the LED epitaxial wafer according to claim 1 grown on a si substrate using SiN insert layers,
It is characterized in that：The detailed process of deposition original position SiN insert layers is in the step (6), in step (5) lower layer's three-dimensional GaN
On the basis of the layer of island, adjusting growth temperature is 1000-1100 DEG C, reative cell air pressure is 500-550Torr, and it is 190- to be passed through flow
215μmol/min SiH4, flow be 45-60slm NH3, deposit 30-180s.
4. the preparation method of the LED epitaxial wafer according to claim 1 grown on a si substrate using SiN insert layers,
It is characterized in that：The detailed process of the growth upper layer islands three-dimensional GaN layer is inserted in step (6) the original position SiN in the step (7)
On the basis of entering layer, it is 800-1050 DEG C to adjust growth temperature, and reative cell air pressure is 300-600Torr, and it is 140-160 to be passed through flow
μm ol/min trimethyl aluminiums, flow are 7-9slm NH3, then the islands lower layer's three-dimensional GaN are with the 4-6nm/min speeds of growth to lower layer
The overall thickness on the three-dimensional islands GaN, original position SiN insert layers and the upper layer islands three-dimensional GaN layer is 500-1500nm.
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| CN107492480A (en) * | 2017-03-08 | 2017-12-19 | 大连民族大学 | A kind of Si bases GaN film and preparation method with AlN pressure modulation cushions |
| CN108598234A (en) * | 2018-04-26 | 2018-09-28 | 吉林大学 | In a kind of reduction SiC substrate in GaN film tensile stress epitaxial structure and preparation method thereof |
| CN109560172B (en) * | 2018-10-26 | 2020-01-10 | 复旦大学 | Semi-polar gallium-nitrogen epitaxial wafer and preparation method thereof |
| CN109524293B (en) * | 2018-10-30 | 2021-10-19 | 江苏晶曌半导体有限公司 | Method for growing high-quality GaN epitaxial film on SiC substrate |
| CN114335267B (en) * | 2022-03-14 | 2023-02-28 | 江西兆驰半导体有限公司 | Epitaxial wafer preparation method, epitaxial wafer and light emitting diode |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002043233A (en) * | 2000-07-28 | 2002-02-08 | Shiro Sakai | Manufacturing method for semiconductor of gallium nitride group compound |
| KR20080022684A (en) * | 2006-09-07 | 2008-03-12 | 엘지전자 주식회사 | Nitride based led and method of manufacturing the same |
| KR20090016051A (en) * | 2007-08-10 | 2009-02-13 | 엘지이노텍 주식회사 | Semiconductor light emitting device and fabrication method thereof |
| CN104037287A (en) * | 2014-06-10 | 2014-09-10 | 广州市众拓光电科技有限公司 | LED epitaxial wafer grown on Si substrate and preparation method thereof |
| CN105355738A (en) * | 2015-11-30 | 2016-02-24 | 天津三安光电有限公司 | LED epitaxial wafer structure and preparation method |
| CN205508855U (en) * | 2016-03-15 | 2016-08-24 | 河源市众拓光电科技有限公司 | LED epitaxial wafer that adoption siN interposed layer is grown on si substrate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7071494B2 (en) * | 2002-12-11 | 2006-07-04 | Lumileds Lighting U.S. Llc | Light emitting device with enhanced optical scattering |
-
2016
- 2016-03-15 CN CN201610147686.6A patent/CN105576096B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002043233A (en) * | 2000-07-28 | 2002-02-08 | Shiro Sakai | Manufacturing method for semiconductor of gallium nitride group compound |
| KR20080022684A (en) * | 2006-09-07 | 2008-03-12 | 엘지전자 주식회사 | Nitride based led and method of manufacturing the same |
| KR20090016051A (en) * | 2007-08-10 | 2009-02-13 | 엘지이노텍 주식회사 | Semiconductor light emitting device and fabrication method thereof |
| CN104037287A (en) * | 2014-06-10 | 2014-09-10 | 广州市众拓光电科技有限公司 | LED epitaxial wafer grown on Si substrate and preparation method thereof |
| CN105355738A (en) * | 2015-11-30 | 2016-02-24 | 天津三安光电有限公司 | LED epitaxial wafer structure and preparation method |
| CN205508855U (en) * | 2016-03-15 | 2016-08-24 | 河源市众拓光电科技有限公司 | LED epitaxial wafer that adoption siN interposed layer is grown on si substrate |
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