CN103996758A - LED epitaxial wafer growing on Cu substrate and preparing method and application of LED epitaxial wafer - Google Patents
LED epitaxial wafer growing on Cu substrate and preparing method and application of LED epitaxial wafer Download PDFInfo
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- CN103996758A CN103996758A CN201410240589.2A CN201410240589A CN103996758A CN 103996758 A CN103996758 A CN 103996758A CN 201410240589 A CN201410240589 A CN 201410240589A CN 103996758 A CN103996758 A CN 103996758A
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Abstract
The invention discloses an LED epitaxial wafer growing on a Cu substrate. The LED epitaxial wafer growing on the Cu substrate comprises the Cu substrate, an AlN buffer layer, a U-GaN film layer, an N-GaN film layer, an InGaN/GaN multi-quantum-well layer and a P-GaN film. The AlN buffer layer, the U-GaN film layer, the N-GaN film layer, the InGaN/GaN multi-quantum-well layer and the P-GaN film sequentially grow on the Cu substrate. By the adoption of the low-temperature growth technology, a GaN film grows on the novel metal Cu substrate in an epitaxial mode, so that the LED epitaxial wafer with the high quality is obtained; by the adoption of the metal Cu substrate, the growth technology is simple, the price is low, and the manufacturing cost of a device can be reduced to a great extent; by the selection of the proper crystal orientation, the GaN epitaxial film with the high quality is obtained from the Cu substrate (111) and the efficiency of nitride devices such as a photoelectric detector can be improved to a great extent.
Description
Technical field
The present invention relates to a kind of LED epitaxial wafer, particularly relate to LED epitaxial wafer of a kind of Cu of being grown in substrate and its preparation method and application.
Background technology
Light-emitting diode (LED) is as a kind of novel solid lighting source and green light source, have that volume is little, power consumption is low, environmental protection, long service life, high brightness, the outstanding feature such as low in calories and colorful, all have a wide range of applications in fields such as outdoor lighting, commercial lighting and decorative engineerings.Current, under the increasingly severe background of global warming problem, energy savings, reduce greenhouse gas emission and become the major issue that the whole world is faced jointly.Taking low energy consumption, low pollution, low emission as basic low-carbon economy, the important directions of economic development will be become.At lighting field, the application of LED luminous product is just attracting common people's sight, and LED, as a kind of novel green light source product, must be the trend of future development, and 21st century is by the epoch that are the novel illumination light source taking LED as representative.But the application cost of present stage LED is higher, and luminous efficiency is lower, these factors all can limit the future development of LED to high-efficient energy-saving environment friendly greatly.
III group-III nitride GaN has extremely excellent character on electricity, optics and acoustics, is subject in recent years extensive concern.GaN is direct band gap material, and sonic transmissions speed is fast, chemistry and Heat stability is good, and thermal conductivity is high, and thermal coefficient of expansion is low, punctures dielectric strength high, is the ideal material of manufacturing efficient LED device.At present, the luminous efficiency of GaN base LED has reached 28% and in further growth now, and this numerical value is far away higher than the luminous efficiency of the lighting systems such as current normally used incandescent lamp (being about 2%) or fluorescent lamp (being about 10%).Data statistics shows, the current electric consumption on lighting of China more than 4,100 hundred million degree, exceedes Britain's whole nation power consumption of a year every year.If with LED replace whole incandescent lamps or part replace fluorescent lamp, can save the electric consumption on lighting that approaches half, exceed the Three Gorges Projects energy output of the whole year.Therefore the greenhouse gas emission producing because of illumination also can reduce greatly.In addition, compared with fluorescent lamp, GaN base LED is containing poisonous mercury element, and is about 100 times of this type of illuminations useful life.
LED will really realize extensive extensive use, needs further to improve the luminous efficiency of LED chip.Although the luminous efficiency of LED has exceeded fluorescent lamp and incandescent lamp, commercialization LED luminous efficiency or lower than sodium vapor lamp (150lm/W), unit lumens/watt on the high side.At present, the luminous efficiency of LED chip is not high enough, and a main cause is because its Sapphire Substrate causes.Because the lattice mismatch of sapphire and GaN is up to 17%, cause forming in extension GaN thin-film process very high dislocation density, thereby reduced the carrier mobility of material, shorten carrier lifetime, and then affected the performance of GaN base device.Secondly, due to sapphire thermal coefficient of expansion (6.63 × 10 under room temperature
-6/ K) compared with the thermal coefficient of expansion of GaN (5.6 × 10
-6/ K) large, thermal mismatching degree is between the two about-18.4%, and after outer layer growth finishes, device can produce very large compression from epitaxially grown High-temperature cooling to room temperature process, easily causes the be full of cracks of film and substrate.Again, due to sapphire thermal conductivity low (100 DEG C time be 0.25W/cmK), be difficult to the heat producing in chip to discharge in time, cause thermal accumlation, the internal quantum efficiency of device is reduced, finally affect the performance of device.In addition,, because sapphire is insulator, can not make vertical structure semiconductor devices.Therefore there is lateral flow in electric current in device, causes CURRENT DISTRIBUTION inhomogeneous, produces more heat transfer, affected to a great extent electricity and the optical property of GaN base LED device.
Therefore the material that the urgent heat of finding the high JiangLEDJie rapidly of a kind of thermal conductivity district transmits is out as substrate.And metal Cu is as the backing material of extension nitride, there are four large its unique advantages.The first, metal Cu has very high thermal conductivity, and the thermal conductivity of Cu is 4.19W/cmK, the heat producing in LED chip can be conducted timely, to reduce device Jie district temperature, improve on the one hand the internal quantum efficiency of device, contribute on the other hand to solve device heat dissipation problem.Second, metal Cu can be used as the backing material of the LED device of growing GaN based vertical structure, can directly on substrate, plate cathode material, the upper plating of P-GaN anode material, make electric current almost all vertical currents cross the epitaxial loayer of GaN-base, thereby resistance declines, there is no current crowding, CURRENT DISTRIBUTION is even, and the heat that electric current produces reduces, favourable to the heat radiation of device; In addition, cathode material directly can be plated in metal substrate, not need, by corrosion P-GaN layer and active layer, electrode is connected in to N-GaN layer, take full advantage of like this material of active layer.The 3rd, relatively other substrates of metal Cu backing material, cheaper, can greatly reduce the manufacturing cost of device.The 4th, the light through substrate surface can be reflected in smooth metal Cu surface, thereby improves the light extraction efficiency of LED.Just because of above-mentioned many advantages, metal substrate is now attempted as the epitaxially grown backing material of III group-III nitride.
But metal Cu substrate is at unstable chemcial property, when epitaxial temperature is higher than 620 DEG C time, between the meeting of extension nitride and metal substrate, there is interfacial reaction, have a strong impact on the quality of epitaxial film growth.The people such as the epitaxially grown pioneer researcher of III group-III nitride, famous scientist Akasaki just once attempted application traditional MOCVD or directly epitaxial growth nitride on the changeable backing material of chemical property of MBE technology, found that at high temperature quite difficulty of extension of film.How to be still a technical problem at the LED epitaxial wafer of Cu substrate growing high-quality.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide LED epitaxial wafer of a kind of Cu of being grown in substrate and its preparation method and application, the present invention adopts low-temperature epitaxy technique epitaxial growth GaN film on metal Cu Novel substrate, has obtained high-quality LED epitaxial wafer; The metal Cu substrate adopting, growth technique is simple, low price, can significantly reduce the manufacturing cost of device; By selecting suitable crystal orientation, the high-quality GaN epitaxial film obtaining on Cu (111) substrate, can increase substantially nitride device as the efficiency of photodetector.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
Be grown in the LED epitaxial wafer of Cu substrate, comprise Cu substrate, AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film, described AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film are grown on Cu substrate successively.
Preferably, described Cu substrate is taking (111) crystal face as epitaxial surface, and it is AlN[11-20 that crystal epitaxial orientation closes] //Cu[1-10].
Preferably, described AlN buffer layer thickness is 100nm; Described U-GaN thin layer thickness is 200-350nm; Described N-GaN thin layer thickness is 4000-5000nm; In described InGaN/GaN multiple quantum well layer, InGaN trap layer thickness is 3-5nm, and GaN barrier layer thickness is 10-15nm, and periodicity is 5-10; Described P-GaN film thickness is 300-400nm.
The preparation method who is grown in the LED epitaxial wafer of Cu substrate, is characterized in that, comprising:
1) substrate with and the choosing of crystal orientation: adopt Cu substrate, taking (111) face as epitaxial surface, crystal epitaxial orientation closes and is: AlN[11-20] //Cu[1-10];
2) substrate surface processing: Cu substrate surface is carried out to polishing, cleaning and annealing in process;
3) in step 2) carry out successively the epitaxial growth of AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film on Cu substrate after treatment, described in obtaining, be grown in the LED epitaxial wafer of Cu substrate.
Preferably, described step 2) in polishing be that Cu substrate surface diamond mud is polished to and is not had after cut, then adopt the method for chemico-mechanical polishing to carry out polishing; Described clean is that Cu substrate is put under deionized water room temperature after ultrasonic cleaning 3-5min, more successively through acetone, ethanol washing, finally dries up with high-purity drying nitrogen; Described annealing in process is that Cu substrate is put into pressure is 2 × 10
-10in the growth room of the UHV-PLD of Torr, high-temperature process 1-2h in 550-650 DEG C of air, is then cooled to room temperature.
Preferably, the epitaxial growth technology of described AlN resilient coating is: underlayer temperature 400-600 DEG C, chamber pressure is 8-10 × 10
-3torr, V/III is than being 50-60, the speed of growth is 0.4-0.6ML/s;
The epitaxial growth technology of described U-GaN thin layer is: adopt PLD technology, underlayer temperature 600-800 DEG C, chamber pressure 3-4 × 10
-3torr, V/III value 50-60, speed of growth 0.6-0.8ML/s;
The epitaxial growth technology of described N-GaN thin layer is: adopt PLD technology, underlayer temperature 400-500 DEG C, chamber pressure 3-4 × 10
-3torr, V/III value 30-40, speed of growth 0.7-0.8ML/s;
The epitaxial growth technology of described InGaN/GaN multiple quantum well layer is: adopt MBE technology, chamber pressure 1-5 × 10
-5torr, V/III value 30-35, speed of growth 0.5-0.6ML/s;
The epitaxial growth technology of described P-GaN film is: underlayer temperature 450-500 DEG C, chamber pressure 3.5-4 × 10
-3torr, V/III value 35-40, speed of growth 0.6-0.8ML/s.
Preferably, described AlN buffer layer thickness is 100nm; Described U-GaN thin layer thickness is 200-350nm; Described N-GaN thin layer thickness is 4000-5000nm; In described InGaN/GaN multiple quantum well layer, InGaN trap layer thickness is 3-5nm, and GaN barrier layer thickness is 10-15nm, and periodicity is 5-10; Described P-GaN film thickness is 300-400nm.
The application of the LED epitaxial wafer that is grown in Cu substrate in photodetector.
Compared to existing technology, beneficial effect of the present invention is:
1, the present invention has used metal Cu as substrate, can obtain lattice mismatch very low between substrate and GaN epitaxial loayer with outgrowth AlN resilient coating, is conducive to the GaN film of the low defect of depositing high-quality, has improved greatly the luminous efficiency of LED;
2, the present invention has used Cu as substrate, and Cu substrate easily obtains, and low price is conducive to reduce production costs;
3, the present invention adopts the method for MBE and PLD combination, grows the high-quality GaN base film of low temperature, prepares high-quality great power LED epitaxial wafer; Application MBE growth active layer, the extension of other layers adopts the PLD technology of low temperature, just can complete like this growth of film at lower temperature, has avoided high-temperature interface reaction, for the film of preparing the low defect of high-quality provides guarantee;
4, the present invention has prepared high-quality LED epitaxial wafer, can be used as the backing material of the LED device of growing GaN based vertical structure, make electric current almost all vertical currents cross the epitaxial loayer of GaN-base, thereby resistance declines, there is no current crowding, CURRENT DISTRIBUTION is even, and the heat that electric current produces reduces, to the favourable radiation recombination efficiency that improves charge carrier of the heat radiation of device, can increase substantially nitride device as the efficiency of photodetector;
5, the present invention prepares and adopts the higher metal Cu of thermal conductivity as substrate, can promptly the heat in device be conducted out, improves on the one hand the internal quantum efficiency of device, helps on the other hand solve device heat dissipation problem, is conducive to improve the life-span of LED device;
6, the present invention has adopted first grow on the Cu substrate low temperature AI N resilient coating of one deck 100nm of low-temperature epitaxy technology; Can ensure at low temperatures the stability of Cu substrate, reduce lattice mismatch and violent interfacial reaction that the volatilization of Cu ion causes, thereby lay good basis for next step high-quality epitaxial loayer;
In sum, the technology of the present invention growth substrates is unconventional, growth technique is unique and simple, have repeatable, epitaxially grown GaN base LED epitaxial wafer defect concentration is low, crystal mass is high, the advantages such as electricity and optical property excellence, can be widely used in the fields such as LED device, semiconductor photo detector, solar cell device, easy to utilize.
Brief description of the drawings
Fig. 1 is the LED epitaxial slice structure schematic diagram that is grown in Cu substrate in the present invention;
Fig. 2 is the HRXRD collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 1;
Fig. 3 is the luminescence generated by light collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 1;
Fig. 4 is the electroluminescence collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 1;
Fig. 5 is the HRXRD collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 2;
Fig. 6 is the luminescence generated by light collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 2;
Fig. 7 is the electroluminescence collection of illustrative plates of the LED epitaxial wafer that in the present invention prepared by embodiment 2;
Wherein, 1 is that Cu substrate, 2 is that AlN resilient coating, 3 is that U-GaN thin layer, 4 is that N-GaN thin layer, 5 is that InGaN/GaN multiple quantum well layer 6 is P-GaN film.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
As shown in Figure 1, for being grown in the LED epitaxial wafer of Cu substrate in the present invention, comprise Cu substrate 1, AlN resilient coating 2, U-GaN thin layer 3, N-GaN thin layer 4, InGaN/GaN multiple quantum well layer 5 and P-GaN film 6, described AlN resilient coating 2, U-GaN thin layer 3, N-GaN thin layer 4, InGaN/GaN multiple quantum well layer 5 and P-GaN film 6 are grown on Cu substrate 1 successively.
In preferred version, described Cu substrate 1 is taking (111) crystal face as epitaxial surface, and it is AlN[11-20 that crystal epitaxial orientation closes] //Cu[1-10]; Described AlN buffer layer thickness is 100nm; Described U-GaN thin layer thickness is 200-350nm; Described N-GaN thin layer thickness is 4000-5000nm; In described InGaN/GaN multiple quantum well layer, InGaN trap layer thickness is 3-5nm, and GaN barrier layer thickness is 10-15nm, and periodicity is 5-10; Described P-GaN film thickness is 300-400nm.
Embodiment 1
The preparation method who is grown in the LED epitaxial wafer of Cu substrate, comprises the following steps:
1) substrate with and the choosing of crystal orientation: adopt Cu substrate, taking (111) face as epitaxial surface, crystal epitaxial orientation closes and is: AlN[11-20] //Cu[1-10];
2) substrate surface polishing, cleaning and annealing in process: first, Cu substrate surface is carried out to polishing with diamond mud, coordinate observation by light microscope substrate surface, until do not have after cut, then adopt the method for chemico-mechanical polishing to carry out polishing; Secondly, Cu substrate is put into ultrasonic cleaning 5min under deionized water room temperature, remove Cu substrate surface pickup particle, more successively through acetone, ethanol washing, remove surface organic matter, dry up with high-purity drying nitrogen; Finally, Cu substrate being put into pressure is 2 × 10
-10in the growth room of the UHV-PLD of Torr, high-temperature process 1h in 550 DEG C of air, is then cooled to room temperature.
3) in step 2) carry out successively the epitaxial growth of AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film on Cu substrate after treatment, described in obtaining, be grown in the LED epitaxial wafer of Cu substrate.
The epitaxial growth of AlN resilient coating: Cu (111) substrate 10 temperature are down to 550 DEG C, and chamber pressure is 10 × 10
-3torr, V/III ratio are 50, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) the PLD ablation AlN target (99.99%) that is 20Hz, in the time of depositing Al N resilient coating, the internal pressure N of growth room
2(99.9999%) remain on 10 × 10
-3torr, the low temperature AI N resilient coating of the 100nm that grows under speed of growth 0.6ML/s condition;
U-GaN thin layer adopts PLD epitaxial growth, underlayer temperature is risen to 700 DEG C, at chamber pressure 4 × 10
-3under Torr, V/III value 40, speed of growth 0.8ML/s condition, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) PLD that is 20Hz for ablation target Ga (99.9999%) and radio frequency plasma free-radical generator be used as nitrogenous source and on AlN resilient coating, react and generate the U-GaN thin layer that thickness is 200nm.
N-GaN thin layer adopts PLD epitaxial growth, and the thickness of its epitaxial loayer is 5000nm, and the concentration of its charge carrier is 1 × 10
19cm
-3.Growth conditions is that temperature is down to 500 DEG C, at chamber pressure 4 × 10
-3under Torr, V/III value 40, speed of growth 0.8ML/s condition, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) PLD that is 20Hz for ablation target Ga (99.9999%) and radio frequency plasma free-radical generator be used as nitrogenous source and on N-GaN thin layer, react and generate N-GaN thin layer.
InGaN/GaN multiple quantum well layer adopts MBE epitaxial growth, and temperature rises to 750 DEG C, at chamber pressure 4 × 10
-5under Torr, V/III value 40, speed of growth 0.6ML/s condition, with energy be 3.0J/cm
2and the repetition rate KrF excimer laser (λ=248nm that is 20Hz, t=20ns) for PLD ablation, target Ga (99.9999%) and radio frequency plasma free-radical generator are used as nitrogenous source reaction and generate InGaN/GaN multiple quantum well layer, wherein InGaN trap layer is 3nm, building layer is 13nm, 7 periodicities of growing, thickness is 112nm.
P-GaN film adopts PLD epitaxial growth, and temperature is down to 500 DEG C, at chamber pressure 4 × 10
-10under Torr, V/III value 40, speed of growth 0.8ML/s condition, with energy be 3.0J/cm
2and the repetition rate KrF excimer laser (λ=248nm that is 20Hz, t=20ns) for PLD ablation, target Ga (99.9999%) and radio frequency plasma free-radical generator are used as nitrogenous source and on InGaN/GaN multiple quantum well layer, react and generate P-GaN film, thickness is 350nm, and its carrier concentration is 2 × 10
16cm
-3, last electron beam evaporation forms ohmic contact, makes the LED epitaxial wafer that is grown in Cu substrate.
Fig. 2 is the HRXRD collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, from X ray swing curve, can see, the half-peak breadth (FWHM) of the X ray swing curve of GaN (0002) is worth lower than 0.06 degree, demonstrates very high crystal property.
Fig. 3 is the luminescence generated by light collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, from luminescence generated by light, can see, photoluminescence wavelength is at 442nm, and FWHM is 22.5nm, demonstrates good photoelectric properties.
Fig. 4 is the electroluminescence collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, and emission wavelength is 432nm as seen from the figure, and FWHM is 22nm, has demonstrated the excellent electric property of LED device of the present invention.
Prepared by the present embodiment is grown in LED epitaxial wafer on metal Cu substrate for the preparation of semiconductor photo detector: the GaN that is grown on the AlN film on metal Cu substrate the non-Doped GaN of epitaxial growth, N-type successively and mixes silicon GaN, P type and mix magnesium preparing at the present embodiment, last electron beam evaporation forms ohmic contact and schottky junction.Wherein N-type is mixed silicon GaN thickness and is about 3 μ m, and the concentration of its charge carrier is 1 × 10
19cm
-3; Non-Doped GaN thickness is about 200nm, and its carrier concentration is 2.2 × 10
16cm
-3; The GaN degree that P type is mixed magnesium is about 1.5 μ m.The prepared photodetector of the present embodiment is under 1V bias voltage, and dark current is only 66pA, and device is under 1V bias voltage, has reached 0.91A/W in the maximum of 361nm place responsiveness.
Prepared by the present embodiment is grown in LED epitaxial wafer on metal Cu substrate for the preparation of solar cell device: for preparing at the present embodiment is grown on the AlN film on metal Cu substrate the non-Doped GaN of epitaxial growth, In successively
xga
1-xn resilient coating, N-type are mixed silicon In
xga
1-xn, P type are mixed the In of magnesium
xga
1-xn, last electron beam evaporation forms ohmic contact and schottky junction.Wherein growth has the In of component gradient
xga
1-xthe value of N resilient coating x can be adjustable between 0-0.2, and the N-type of then growing is mixed silicon In
xga
1-xn, the thickness of epitaxial loayer is about 5 μ m, and the concentration of its charge carrier is 1 × 10
19cm
-3.Then In grows
xga
1-xn multiple quantum well layer, thickness is about 300nm, and periodicity is 20, wherein In
0.2ga
0.8n trap layer is 3nm, In
0.08ga
0.92it is 10nm that N builds layer.The P type In of regrowth Mg doping
xga
1-xn layer, thickness is about 200nm, and its carrier concentration is 2 × 10
16cm
-3, last electron beam evaporation forms ohmic contact.Pass through at N on this basis
2under atmosphere, anneal, improved carrier concentration and the mobility of P type InGaN film; Be prepared into InGaN solar cell device.
Testing result shows, is no matter character or in application, the correlated results of the LED that the application Sapphire Substrate that is all better than having reported at present obtains, has a good application prospect.
Embodiment 2
The preparation method who is grown in the LED epitaxial wafer of Cu substrate, comprises the following steps:
1) substrate with and the choosing of crystal orientation: adopt Cu substrate, taking (111) face as epitaxial surface, crystal epitaxial orientation closes and is: AlN[11-20] //Cu[1-10];
2) substrate surface polishing, cleaning and annealing in process: first, Cu substrate surface is carried out to polishing with diamond mud, coordinate observation by light microscope substrate surface, until do not have after cut, then adopt the method for chemico-mechanical polishing to carry out polishing; Secondly, Cu substrate is put into ultrasonic cleaning 4min under deionized water room temperature, remove Cu substrate surface pickup particle, more successively through acetone, ethanol washing, remove surface organic matter, dry up with high-purity drying nitrogen; Finally, Cu substrate being put into pressure is 2 × 10
-10in the growth room of the UHV-PLD of Torr, high-temperature process 2h in 650 DEG C of air, is then cooled to room temperature.
3) in step 2) carry out successively the epitaxial growth of AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film on Cu substrate after treatment, described in obtaining, be grown in the LED epitaxial wafer of Cu substrate.
The epitaxial growth of AlN resilient coating: Cu (111) substrate 10 temperature are down to 550 DEG C, and chamber pressure is 10 × 10
-3torr, V/III ratio are 60, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) the PLD ablation AlN target (99.99%) that is 20Hz, in the time of depositing Al N resilient coating, the internal pressure N of growth room
2(99.9999%) remain on 10 × 10
-3torr, the low temperature AI N resilient coating of the 100nm that grows under speed of growth 0.6ML/s condition;
U-GaN thin layer adopts PLD epitaxial growth, underlayer temperature is risen to 700 DEG C, at chamber pressure 3.5 × 10
-3under Torr, V/III value 40, speed of growth 0.75ML/s condition, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) PLD that is 20Hz for ablation target Ga (99.9999%) and radio frequency plasma free-radical generator be used as nitrogenous source and on AlN resilient coating, react and generate the U-GaN thin layer that thickness is 300nm.
N-GaN thin layer adopts PLD epitaxial growth, and the thickness of its epitaxial loayer is 4500nm, and the concentration of its charge carrier is 1 × 10
19cm
-3.Growth conditions is that temperature is down to 500 DEG C, at chamber pressure 4 × 10
-4under Torr, V/III value 40, speed of growth 0.8ML/s condition, with energy be 3.0J/cm
2and repetition rate KrF excimer laser (λ=248nm, t=20ns) PLD that is 20Hz for ablation target Ga (99.9999%) and radio frequency plasma free-radical generator be used as nitrogenous source and on N-GaN thin layer, react and generate N-GaN thin layer.
InGaN/GaN multiple quantum well layer adopts MBE epitaxial growth, and temperature rises to 750 DEG C, at chamber pressure 1 × 10
-5under Torr, V/III value 40, speed of growth 0.6ML/s condition, growing InGaN/GaN multiple quantum well layer, wherein InGaN trap layer is 3nm, building layer is 13nm, 7 periodicities of growing, thickness is 112nm.
P-GaN film adopts PLD epitaxial growth, and temperature is down to 500 DEG C, at chamber pressure 3.5 × 10
-5under Torr, V/III value 40, speed of growth 0.7ML/s condition, with energy be 3.0J/cm
2and the repetition rate KrF excimer laser (λ=248nm that is 20Hz, t=20ns) for PLD ablation, target Ga (99.9999%) and radio frequency plasma free-radical generator are used as nitrogenous source and on InGaN/GaN multiple quantum well layer, react and generate P-GaN film, thickness is 400nm, and its carrier concentration is 2 × 10
16cm
-3, last electron beam evaporation forms ohmic contact, makes the LED epitaxial wafer that is grown in Cu substrate.
Fig. 5 is the HRXRD collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, from X ray swing curve, can see, the half-peak breadth (FWHM) of the X ray swing curve of GaN (0002) is worth lower than 0.06 degree, demonstrates very high crystal property.
Fig. 6 is the luminescence generated by light collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, from luminescence generated by light, can see, photoluminescence wavelength is at 442nm, and FWHM is 22.5nm, demonstrates good photoelectric properties.
Fig. 7 is the electroluminescence collection of illustrative plates of the LED epitaxial wafer prepared of the present embodiment, and emission wavelength is 432nm as seen from the figure, and FWHM is 22nm, has demonstrated the excellent electric property of LED device of the present invention.
Prepared by the present embodiment is grown in LED epitaxial wafer on metal Cu substrate for the preparation of semiconductor photo detector: the GaN that is grown on the AlN film on metal Cu substrate the non-Doped GaN of epitaxial growth, N-type successively and mixes silicon GaN, P type and mix magnesium preparing at the present embodiment, last electron beam evaporation forms ohmic contact and schottky junction.Wherein P type is mixed silicon GaN thickness and is about 3 μ m, and the concentration of its charge carrier is 1 × 10
19cm
-3; Non-Doped GaN thickness is about 200nm, and its carrier concentration is 2.2 × 10
16cm
-3; The GaN degree that P type is mixed magnesium is about 1.5 μ m.The prepared photodetector of the present embodiment is under 1V bias voltage, and dark current is only 66pA, and device is under 1V bias voltage, has reached 0.91A/W in the maximum of 361nm place responsiveness.
Prepared by the present embodiment is grown in LED epitaxial wafer on metal Cu substrate for the preparation of solar cell device: for preparing at the present embodiment is grown on the AlN film on metal Cu substrate the non-Doped GaN of epitaxial growth, In successively
xga
1-xn resilient coating, N-type are mixed silicon In
xga
1-xn, P type are mixed the In of magnesium
xga
1-xn, last electron beam evaporation forms ohmic contact and schottky junction.Wherein growth has the In of component gradient
xga
1-xthe value of N resilient coating x can be adjustable between 0-0.2, and the N-type of then growing is mixed silicon In
xga
1-xn, the thickness of epitaxial loayer is about 5 μ m, and the concentration of its charge carrier is 1 × 10
19cm
-3.Then In grows
xga
1-xn multiple quantum well layer, thickness is about 300nm, and periodicity is 20, wherein In
0.2ga
0.8n trap layer is 3nm, In
0.08ga
0.92it is 10nm that N builds layer.The P type In of regrowth Mg doping
xga
1-xn layer, thickness is about 200nm, and its carrier concentration is 2 × 10
16cm
-3, last electron beam evaporation forms ohmic contact.Pass through at N on this basis
2under atmosphere, anneal, improved carrier concentration and the mobility of P type InGaN film; Be prepared into InGaN solar cell device.
Testing result shows, is no matter character or in application, the correlated results of the LED epitaxial wafer that the application Sapphire Substrate that is all better than having reported at present obtains, has a good application prospect.
To one skilled in the art, can be according to technical scheme described above and design, make other various corresponding changes and deformation, and within these all changes and deformation all should belong to the protection range of the claims in the present invention.
Claims (8)
1. be grown in the LED epitaxial wafer of Cu substrate, it is characterized in that, comprise Cu substrate, AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film, described AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film are grown on Cu substrate successively.
2. the LED epitaxial wafer that is grown in Cu substrate as claimed in claim 1, is characterized in that, described Cu substrate is taking (111) crystal face as epitaxial surface, and it is AlN[11-20 that crystal epitaxial orientation closes] //Cu[1-10].
3. the LED epitaxial wafer that is grown in Cu substrate as claimed in claim 1, is characterized in that, described AlN buffer layer thickness is 100nm; Described U-GaN thin layer thickness is 200-350nm; Described N-GaN thin layer thickness is 4000-5000nm; In described InGaN/GaN multiple quantum well layer, InGaN trap layer thickness is 3-5nm, and GaN barrier layer thickness is 10-15nm, and periodicity is 5-10; Described P-GaN film thickness is 300-400nm.
4. the preparation method who is grown in the LED epitaxial wafer of Cu substrate described in claim 1, is characterized in that, comprising:
1) substrate with and the choosing of crystal orientation: adopt Cu substrate, taking (111) face as epitaxial surface, crystal epitaxial orientation closes and is: AlN[11-20] //Cu[1-10];
2) substrate surface processing: Cu substrate surface is carried out to polishing, cleaning and annealing in process;
3) in step 2) carry out successively the epitaxial growth of AlN resilient coating, U-GaN thin layer, N-GaN thin layer, InGaN/GaN multiple quantum well layer and P-GaN film on Cu substrate after treatment, described in obtaining, be grown in the LED epitaxial wafer of Cu substrate.
5. preparation method as claimed in claim 4, is characterized in that, described step 2) in polishing be that Cu substrate surface diamond mud is polished to and is not had after cut, then adopt the method for chemico-mechanical polishing to carry out polishing; Described clean is that Cu substrate is put under deionized water room temperature after ultrasonic cleaning 3-5min, more successively through acetone, ethanol washing, finally dries up with high-purity drying nitrogen; Described annealing in process is that Cu substrate is put into pressure is 2 × 10
-10in the growth room of the UHV-PLD of Torr, high-temperature process 1-2h in 550-650 DEG C of air, is then cooled to room temperature.
6. preparation method as claimed in claim 4, is characterized in that:
The epitaxial growth technology of described AlN resilient coating is: underlayer temperature 400-600 DEG C, chamber pressure is 8-10 × 10
-3torr, V/III is than being 50-60, the speed of growth is 0.4-0.6ML/s;
The epitaxial growth technology of described U-GaN thin layer is: adopt PLD technology, underlayer temperature 600-800 DEG C, chamber pressure 3-4 × 10
-3torr, V/III value 50-60, speed of growth 0.6-0.8ML/s;
The epitaxial growth technology of described N-GaN thin layer is: adopt PLD technology, underlayer temperature 400-500 DEG C, chamber pressure 3-4 × 10
-3torr, V/III value 30-40, speed of growth 0.7-0.8ML/s;
The epitaxial growth technology of described InGaN/GaN multiple quantum well layer is: adopt MBE technology, chamber pressure 1-5 × 10
-5torr, V/III value 30-35, speed of growth 0.5-0.6ML/s;
The epitaxial growth technology of described P-GaN film is: underlayer temperature 450-500 DEG C, chamber pressure 3.5-4 × 10
-3torr, V/III value 35-40, speed of growth 0.6-0.8ML/s.
7. preparation method as claimed in claim 4, is characterized in that, described AlN buffer layer thickness is 100nm; Described U-GaN thin layer thickness is 200-350nm; Described N-GaN thin layer thickness is 4000-5000nm; In described InGaN/GaN multiple quantum well layer, InGaN trap layer thickness is 3-5nm, and GaN barrier layer thickness is 10-15nm, and periodicity is 5-10; Described P-GaN film thickness is 300-400nm.
8. the application of the LED epitaxial wafer that is grown in Cu substrate described in claim 1-7 any one in LED device, semiconductor photo detector, solar cell device.
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Application publication date: 20140820 |