CN104393136A - Preparation method of GaN-based LED epitaxial wafer enhancing luminescence efficiency - Google Patents
Preparation method of GaN-based LED epitaxial wafer enhancing luminescence efficiency Download PDFInfo
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- CN104393136A CN104393136A CN201410599879.6A CN201410599879A CN104393136A CN 104393136 A CN104393136 A CN 104393136A CN 201410599879 A CN201410599879 A CN 201410599879A CN 104393136 A CN104393136 A CN 104393136A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/20—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
- H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/26—Materials of the light emitting region
- H01L33/30—Materials of the light emitting region containing only elements of group III and group V of the periodic system
- H01L33/32—Materials of the light emitting region containing only elements of group III and group V of the periodic system containing nitrogen
Abstract
The invention discloses a preparation method of a GaN-based LED epitaxial wafer enhancing luminescence efficiency. The preparation method comprises the following steps that a buffer layer, an unintentional doping layer, a first N-type doping layer, a second N-type doping layer, a InGaN/GaN multi-quantum well active layer, an electron blocking layer, a P-type doping layer and a contact layer are grown on a substrate in turn; after the first N-type doping layer is grown completely, an organic source is closed, piping of NH3 into a reaction chamber is reduced or stopped and growing is stopped for 10-200s under the atmosphere of H2 or N2 so that the first N-type doping layer with a rough surface is acquired. LED internal quantum efficiency and external quantum efficiency can be enhanced simultaneously. Besides, the preparation method is simple and preparation cost is relatively low.
Description
Technical field
The present invention relates to GaN base LED preparing technical field, refer in particular to a kind of GaN base LED preparation method improving luminous efficiency.
Background technology
GaN base LED has that volume is little, the life-span long, low in energy consumption, brightness is high and the advantage such as easy of integrationization, has entered general illumination field, along with GaN base LED is in the extensive use of lighting field, more and more higher to the requirement of its luminous efficiency.Therefore, the brightness promoting GaN base LED becomes the key issue needing solution badly.
In prior art, the brightness promoting GaN base LED is mainly the raising of internal quantum efficiency and the raising of external quantum efficiency, comprises the optimization of epitaxial structure, the lifting of crystal mass, the processing of graph substrate, alligatoring, the optimization etc. of chip structure.
Because GaN material refractive index and air refraction differ greatly, the light that luminous zone sends is not easy outgoing, makes external quantum efficiency low.Coarsening technique and graph substrate are often used as the means that GaN base LED external quantum efficiency promotes.Current roughening process and graph substrate major part utilize dry method or wet etching, need through special processing, complex process, and cost are high.
GaN base LED film is along the growth of polarity c direction, and the quantum well structure of described c plane suppresses electricity and spontaneous polarization and the Stark effect (QCSE) that produces quantum limit because existing.Strong internal electric field along c direction causes electronics and hole being separated spatially, reduces rate of radiative recombination.
In order to slow down or eliminate the adverse effect of described polarity effect, the GaN template of semi-polarity face or non-polar plane can be selected, utilize horizontal extension technology to grow InGaN/GaN multi-quantum pit structure.The preparation of semi-polarity face or nonpolar face GaN template and transversal epitaxial growth technology add the complexity of technique.
In sum, in prior art, still there is more technical difficulty in the GaN base LED of preparation low cost, high-luminous-efficiency.
In MOCVD reative cell, the epitaxial growth of GaN is the moment process of decomposing along with GaN also, and this decomposable process, mainly by the flow rate effect of temperature, pressure and gas, in order to slow down the decomposition of GaN as far as possible, in whole epitaxial process, all there is NH
3pass into reative cell.We utilize this decomposing phenomenon of GaN, by the adjustment of epitaxy technique condition, can obtain the GaN epitaxial layer surface that roughness is controlled.
By utilizing the decomposing phenomenon of GaN, obtain the N-type doped layer that surface is suitably coarse, through the optimization of process conditions, can promote internal quantum efficiency and the external quantum efficiency of LED, this case produces thus simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of GaN base LED preparation method improving luminous efficiency, to improve LED internal quantum efficiency and external quantum efficiency simultaneously, and preparation method is simple, and preparation cost is lower.
For reaching above-mentioned purpose, solution of the present invention is:
Improve a GaN base LED preparation method for luminous efficiency, comprise the following steps: grown buffer layer, involuntary doped layer, the first N-type doped layer, the second N-type doped layer, InGaN/GaN multiple quantum well active layer, electronic barrier layer, P type doped layer and contact layer successively on substrate; After having grown the first N-type doped layer, close organic source, reduced or stop NH
3pass into reative cell, at H
2or N
2pause under atmosphere growth 10-200s, obtains shaggy first N-type doped layer.
Further, during pause growth, the temperature of reative cell is 800-1250 DEG C, and pressure is 100-600mbar.
Further, reduce or stop NH
3the mode passing into reative cell is that staged changes NH
3intake, gradual change type change NH
3intake, pulsed close NH
3pass into the one in reative cell or combination.
Further, the first N-type doped layer is GaN material; First N-type doped layer growth temperature is 950-1150 DEG C, and pressure is 100-600mbar, and the ratio of V/III is 500-5000, and growth thickness is 1-4 μm, and N-type doping content is 1 × 10
18-1 × 10
19.
Further, the surface roughness of the first N-type doped layer is 5-50 nm, and the average height of alligatoring is 20-200nm.The control of surface roughness is particularly important, and degree of roughness is too little, not obvious to the lifting of LED light effect, and degree of roughness is too large, and make follow-up epitaxial growth difficulty, epitaxial wafer surface irregularity, is unfavorable for the lifting of light efficiency on the contrary.
Further, the second N-type doped layer is In
xga
1-xn material, wherein x gets any one numerical value in 0-0.2; Second N-type doped layer growth temperature is 800-1150 DEG C, and pressure is 100-600mbar, and the ratio of V/III is 500-10000, and growth thickness is 10-200nm, and N-type doping content is 1 × 10
18-1 × 10
19.
Further, the material of resilient coating and involuntary doped layer is GaN, and growth pressure is 100-600mbar, and the ratio of V/III is 500-5000; Wherein, the growth temperature of resilient coating is 500-700 DEG C, and thickness is 10-50nm, and the growth temperature of involuntary doped layer is 950-1150 DEG C, and thickness is 1-3 μm.
Further, in InGaN/GaN multiple quantum well active layer, the growth temperature of GaN barrier layer is 750-900 DEG C, and growth pressure is 100-600mbar, and V/III is 3000-50000, and growth thickness is 8-15nm; The growth temperature of InGaN well layer is 650-800 DEG C, and growth pressure is 100-600mbar, and V/III is 3000-50000, and growth thickness is 2-5nm, In component is 0.15-0.25.
Further, the material of electronic barrier layer is AlGaN, and wherein Al component is 0.1-0.3, and growth temperature is 950 DEG C-1150 DEG C, and pressure is 100-600mbar, and V/III is 1000-30000, and growth thickness is 15-50nm, and carry out P type Mg and adulterate, doping content is 1 × 10
17-5 × 10
18.
Further, the material of P type doped layer is GaN, and growth temperature is 950-1150 DEG C, and pressure is 100-600mbar, and the ratio of V/III is 1000-30000, and growth thickness is 100-300nm, and doping content is 1 × 10
17-5 × 10
18; The material of contact layer is the InGaN/GaN superlattice layer of P type doping, and doping content is 1 × 10
18-5 × 10
19, growth temperature is 600-900 DEG C, and pressure is 100-600mbar, and the ratio of V/III is the In component of 3000-50000, InGaN is 0.02-0.12, and thickness is the thickness of 1-3nm, GaN is 1-3nm.
After adopting such scheme, the present invention, after having grown the first N-type doped layer, closes organic source, reduces or stops NH
3pass into reative cell, at H
2or N
2pause under atmosphere growth 10-200s, obtains the first N-type doped layer that surface is suitably coarse.The epitaxial structure that shaggy first N-type doped layer grows, not only active area light-emitting area is large, and there is more semi-polarity face in active area, reduce the impact of piezoelectric effect, improve rate of radiative recombination, and the first coarse N-type doped layer surface, the inner light path of epitaxial loayer can be changed, be more conducive to the outgoing of light, improve light emission rate.
After having grown the first N-type doped layer, process without the need to taking out epitaxial wafer, directly by epitaxy technique alligatoring, method is simple, need not increase production cost, can significantly promote LED light power.Compared with prior art, it has following beneficial effect:
One, through the first N-type doped layer surface of alligatoring, the multi-quantum well active region light-emitting area of growth after making increases, and can increase substantially luminosity.
Two, through the first N-type doped layer surface of this epitaxy technique alligatoring, expose more semi-polarity face, the InGaN/GaN Multiple Quantum Well that this semi-polarity face grows, reduce the impact of piezoelectric effect, improve radiation recombination efficiency, reduce the impact of quantum limit Stark effect, the stability of wavelength is better.
Three, the first N-type doped layer surface of alligatoring, can change the light path of epitaxial loayer inside, promote the exit probability of light, and then improve LED external quantum efficiency.
Simultaneously, described preparation method is without the need to passing through the additional process such as etching, method is simple, production cost need not be increased, and the GaN base LED grown by described method, internal quantum efficiency and external quantum efficiency are all improved, and luminous efficiency is compared conventional epitaxial growth method and promoted more than 20%, and wavelength stability is better.
Accompanying drawing explanation
Fig. 1 is the shape appearance figure on the present invention first N-type doped layer surface after alligatoring;
Fig. 2 is that the present invention's MOCVD device in-situ monitoring used obtains part epitaxial loayer reflectance curves in real time;
Fig. 3 is the LED epitaxial structure schematic diagram that the present invention is formed;
NH when Fig. 4 is the embodiment of the present invention one extension interruption of growth
3flow schematic diagram;
NH when Fig. 5 is the embodiment of the present invention two extension interruption of growth
3flow schematic diagram;
NH when Fig. 6 is the embodiment of the present invention three extension interruption of growth
3flow schematic diagram;
Fig. 7 is embodiment of the present invention NH when prolonging interruption of growth all round
3flow schematic diagram.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in detail.
Embodiment one
Utilize MOCVD device growing GaN base LED, adopt the Sapphire Substrate of 2 inches of C face No clean, epitaxial step mainly comprises:
1, reaction chamber temperature is elevated to 1200 DEG C, reative cell pressure is 100mbar, at H
2sapphire Substrate 300s is cured under atmosphere.
2, reduce reaction chamber temperature to 560 DEG C, pass into NH
3, nitride deposition 120s.
3, adjusting reative cell pressure is 600 mbar, passes into Ga source and NH
3, the ratio of V/III is 1200, grows 25nm GaN resilient coating at 560 DEG C.
4, raise reaction chamber temperature to 1100 DEG C, adjustment reative cell pressure is 250mbar, passes into Ga source and NH
3, the ratio of V/III is 1500, the involuntary doped gan layer of growth 2000nm.
5, Ga source is passed into, NH
3and silane, the ratio of V/III is 1500, and growth 2500nm N-type doped gan layer, N-type doping content is 1 × 10
18-1 × 10
19.
6, keep reaction chamber temperature and pressure constant, close Ga source, adjustment NH
3flow, as shown in Figure 4, is specially: at 0-25s by NH
3flow is gradient to 0,25-50s and closes NH
3, again by NH in the time of 50-75s
3flow gradual change is adjusted to original numerical value.
7, keep reaction chamber temperature and pressure constant, pass into Ga source, NH
3and silane, the ratio of V/III is 1500, and growth 100nm N-type doped gan layer, N-type doping content is 1 × 10
18-1 × 10
19.
8, main carrier gas is switched to N
2, adjustment reative cell pressure is 400 mbar, the InGaN/GaN multiple quantum well active layer in 6 cycles of growth.Wherein the growth temperature of GaN barrier layer is 850 DEG C, and growth thickness is 12 nm, and the ratio of V/III is the growth temperature of 15000, InGaN well layer is 730 DEG C, and growth thickness is 3 nm, and the ratio of V/III is 20000.
9, switching main carrier gas is H
2, raise reaction chamber temperature to 1050 DEG C, adjustment reative cell pressure, to 250mbar, passes into Ga source, Al source, NH
3and Cp
2the luxuriant magnesium of Mg(bis-), the ratio of V/III is 8000, and growth 25nm P type doped with Al GaN electronic barrier layer, Al component is 0.15-0.25, P type doping content is 5 × 10
17-5 × 10
18.
10, keep reaction chamber temperature and pressure constant, close Al source, pass into Ga source, NH
3and Cp
2mg, the ratio of V/III is 13000, and growth 200nm P type doped gan layer, P type doping content is 5 × 10
17-5 × 10
18.
11, switching main carrier gas is N
2, adjustment reative cell pressure is 400mbar, and temperature is 780 DEG C, and the InGaN/GaN superlattice contact layer of the P type doping in 4 cycles of growth, doping content is 1 × 10
18-5 × 10
19.Wherein the thickness of InGaN layer is 1nm, and the ratio of V/III is 20000, and the thickness of GaN layer is 1nm, and the ratio of V/III is 20000.
12, adjusting reaction chamber temperature is 800 DEG C, at pure N
2anneal under atmosphere 600s, reduces reaction chamber temperature to room temperature, terminate epitaxial growth.
Described GaN base LED preparation method, after alligatoring, as shown in Figure 1, the shape appearance figure on this first N-type doped layer surface records through atomic force microscope the pattern on the first N-type doped layer surface.Fig. 2 is MOCVD device in-situ monitoring gained epitaxial loayer reflectance curves of the present invention, the intensity of reflectivity curve, react the smoothness of epitaxial loayer to a certain extent, reflectivity curve intensity is less, surface epitaxial layer surface is more coarse, can find in figure in interruption of growth process, reflectivity curve intensity declines, and shows that its surface is roughening.Fig. 3 is the LED epitaxial structure schematic diagram that the present invention is formed, bottom is substrate 10, is N-type layer 20 on substrate 10, is multiple quantum well active layer 30 on N-type layer 20, multiple quantum well active layer 30 is formed semi-polarity face 301, and multiple quantum well active layer 30 is P-type layer 40.
Embodiment two
The present embodiment is different from embodiment one to be: the present embodiment, in interruption of growth process, adjusts NH
3the method of flow, as shown in Figure 5, is specially: in 0-15s, keep NH
3normal discharge passes into reative cell, in 15-65s, closes NH
3, in 65-80s, again open NH
3, keep NH
3normal discharge passes into reative cell.
Embodiment three
The present embodiment is different from embodiment one to be: the present embodiment, in interruption of growth process, adjusts NH
3flow adopts pulsed, as shown in Figure 6, is specially: NH is opened in pulse
3with closedown NH
3time be respectively 5s and 15s, altogether repeat 4 cycles.
Embodiment four
The present embodiment is different from embodiment one to be: the present embodiment, in interruption of growth process, adjusts NH
3the method of flow adopts staged, as shown in Figure 7, is specially: within the 0-5s time, keeps NH
3normally pass into reative cell, within the 5-10s time period, by NH
3flow is gradient to the 2nd NH
3flow, keeps the 2nd NH within the 10-15s time period
3flow passes into reative cell, by the 2nd NH within the 15-20s time period
3flow is gradient to 0, within the 20-40s time period, keep NH
3flow is 0, within the 40-45s time period, again by NH
3flow is gradient to the 2nd NH
3flow, keeps the 2nd NH within the 45-50s time period
3flow passes into reative cell, by the 2nd NH within the 50-55s time period
3flow is gradient to normal NH
3, within the 55-60s time, keep NH
3normally pass into reative cell.Wherein the 2nd NH
3flow can be normal NH
320%-80% of flow.
In above embodiment one to embodiment four, according to the requirement to N-type Doped GaN surface roughness, the total time of interruption of growth at 10-200s, wherein, NH
3shut-in time controls at 10-80s.The total time of interruption of growth and closedown NH
3time unsuitable oversize, otherwise GaN surface is too coarse, epitaxial crystal Quality Down, will make subsequently epitaxial growing difficult, and cause final p-GaN surface irregularity, be unfavorable for the lifting of light efficiency.
The foregoing is only the preferred embodiments of the present invention, not to the restriction of this case design, all equivalent variations done according to the design key of this case, all fall into the protection range of this case.
Claims (10)
1. one kind is improved the GaN base LED preparation method of luminous efficiency, it is characterized in that, comprise the following steps: grown buffer layer, involuntary doped layer, the first N-type doped layer, the second N-type doped layer, InGaN/GaN multiple quantum well active layer, electronic barrier layer, P type doped layer and contact layer successively on substrate; After having grown the first N-type doped layer, close organic source, reduced or stop NH
3pass into reative cell, at H
2or N
2pause under atmosphere growth 10-200s, obtains shaggy first N-type doped layer.
2. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, is characterized in that, during pause growth, the temperature of reative cell is 800-1250 DEG C, and pressure is 100-600mbar.
3. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, is characterized in that, reduces or stops NH
3the mode passing into reative cell is that staged changes NH
3intake, gradual change type change NH
3intake, pulsed close NH
3pass into the one in reative cell or combination.
4. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the first N-type doped layer is GaN material; First N-type doped layer growth temperature is 950-1150 DEG C, and pressure is 100-600mbar, and the ratio of V/III is 500-5000, and growth thickness is 1-4 μm, and N-type doping content is 1 × 10
18-1 × 10
19.
5. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the surface roughness of the first N-type doped layer is 5-50 nm, and the average height of alligatoring is 20-200nm.
6. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the second N-type doped layer is In
xga
1-xn material, wherein x gets any one numerical value in 0-0.2; Second N-type doped layer growth temperature is 800-1150 DEG C, and pressure is 100-600mbar, and the ratio of V/III is 500-10000, and growth thickness is 10-200nm, and N-type doping content is 1 × 10
18-1 × 10
19.
7. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the material of resilient coating and involuntary doped layer is GaN, and growth pressure is 100-600mbar, and the ratio of V/III is 500-5000; Wherein, the growth temperature of resilient coating is 500-700 DEG C, and thickness is 10-50nm, and the growth temperature of involuntary doped layer is 950-1150 DEG C, and thickness is 1-3 μm.
8. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, in InGaN/GaN multiple quantum well active layer, the growth temperature of GaN barrier layer is 750-900 DEG C, growth pressure is 100-600mbar, V/III is 3000-50000, and growth thickness is 8-15nm; The growth temperature of InGaN well layer is 650-800 DEG C, and growth pressure is 100-600mbar, and V/III is 3000-50000, and growth thickness is 2-5nm, In component is 0.15-0.25.
9. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the material of electronic barrier layer is AlGaN, wherein Al component is 0.1-0.3, and growth temperature is 950 DEG C-1150 DEG C, and pressure is 100-600mbar, V/III is 1000-30000, growth thickness is 15-50nm, and carry out P type Mg and adulterate, doping content is 1 × 10
17-5 × 10
18.
10. a kind of GaN base LED preparation method improving luminous efficiency as claimed in claim 1, it is characterized in that, the material of P type doped layer is GaN, growth temperature is 950-1150 DEG C, pressure is 100-600mbar, the ratio of V/III is 1000-30000, and growth thickness is 100-300nm, and doping content is 1 × 10
17-5 × 10
18; The material of contact layer is the InGaN/GaN superlattice layer of P type doping, and doping content is 1 × 10
18-5 × 10
19, growth temperature is 600-900 DEG C, and pressure is 100-600mbar, and the ratio of V/III is the In component of 3000-50000, InGaN is 0.02-0.12, and thickness is the thickness of 1-3nm, GaN is 1-3nm.
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| CN110571311A (en) * | 2019-07-30 | 2019-12-13 | 中国科学技术大学 | multi-quantum well structure, photoelectric device epitaxial wafer and photoelectric device |
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