CN103035496B - A kind of growth GaN film on a si substrate and its preparation method and application - Google Patents
A kind of growth GaN film on a si substrate and its preparation method and application Download PDFInfo
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- CN103035496B CN103035496B CN201210535097.7A CN201210535097A CN103035496B CN 103035496 B CN103035496 B CN 103035496B CN 201210535097 A CN201210535097 A CN 201210535097A CN 103035496 B CN103035496 B CN 103035496B
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Abstract
The invention discloses a kind of growth GaN film on a si substrate, it comprises Si substrate layer, the Al grown on Si substrate layer
2o
3protective layer, to grow at Al
2o
3gaN film layer on protective layer.The preparation method of growth of the present invention GaN film on a si substrate comprises and chooses Si substrate; (111) crystal face choosing Si substrate plates one deck Al layer, then passes into oxygen plasma to forming Al
2o
3protective layer; Again at Al
2o
3growing GaN thin layer on protective layer.The defect concentration of GaN film of the present invention is low, crystal mass is high, electricity and optical property excellent, is applicable to being applied in LED component, in solar cell.
Description
Technical field
The present invention relates to GaN film field, be specifically related to a kind of growth GaN film on a si substrate and its preparation method and application.
Background technology
III race's gallium nitride polynary system material belongs to the semi-conducting material of direct band gap, band gap can be adjusted to 6.2eV continuously from 0.7eV, color covers from infrared to ultraviolet wavelength, at photoelectron as having important application and development in blue light, green glow, ultraviolet light-emitting diodes (LED), short wavelength laser diode (LD), ultraviolet detector, Bragg reflection waveguide etc.GaN is as one of third generation semi-conducting material representative in addition, there is direct band gap, broad stopband, high saturated electron drift velocity, high breakdown electric field and the excellent properties such as high heat conductance, excellent physical and chemical stability, have also been obtained in microelectronic applications and pay close attention to widely.Successfully obtain p-GaN first from I.Akasaki, after realizing the new breakthrough of blue-ray LED, GaN base compound semiconductor receives much concern always, has a wide range of applications in fields such as room lighting, commercial lighting, engineering illuminations.
High-quality GaN material is generally all made by heteroepitaxy method.The selection of substrate is very large to the quality influence of epitaxial growth GaN material, generally needs to follow the principles such as lattice constant match, matched coefficients of thermal expansion, affordable.Various substrates material also has very important impact to the preparation technology of GaN base LED component.For example because GaN crystal also exists piezoelectricity and spontaneous polarization effect, different substrates can make obtained material list reveal different polarization characteristics.In addition, because different materials price variance is comparatively large, the difference of backing material also can make the cost of LED produce larger difference.As can be seen here, the selection of GaN base LED substrate material is most important.
As the substrate being usually used in growing GaN, sapphire, SiC, Si have realized the preparation of device level LED at present all, but the outer layer growth problem that respective backing material brings, also need constantly to capture.Sapphire has stable physicochemical properties, but there is very large lattice mismatch (16%) and thermal stress mismatch (25%) between it and GaN, causes the GaN epitaxial layer of growth second-rate.Its heat conductivility is poor simultaneously, and this also seriously governs the development of Sapphire Substrate great power LED.Although the lattice mismatch of SiC with GaN only 3.5%, thermal conductivity is higher, and its thermal stress mismatch and sapphire are quite (25.6%), poor with the wetability of GaN, expensive.Si substrate has that cost is low, monocrystalline size is large and the various features such as quality is high, thermal conductivity is high, electric conductivity is good, and the microelectric technique of Si is very ripe, and therefore Si Grown GaN film is expected to realize photoelectron and microelectronic integrated.Exactly because the above-mentioned plurality of advantages of Si substrate, Si Grown GaN film and then preparation LED more and more receive much concern.But prepare the quality of GaN monocrystal thin films at present on a si substrate not as Sapphire Substrate, main cause is: one, Si and GaN thermal expansion mismatch is far away higher than sapphire, epitaxial wafer is caused to be easier to be full of cracks; Two, Si substrate is met active N and is easily formed unbodied Si in interface
xn
y, affect the growth quality of GaN; Three, Si also can reduce LED luminous efficiency greatly to the absorption of visible ray.
As can be seen here, even if Si substrate has, cost is low, good heat dissipation, and conveniently makes the advantages such as vertical devices, has very good development prospect, but will growing high-quality GaN film on a si substrate, need new method and the technique of finding Si Grown GaN film.
Summary of the invention
The object of the invention is to the defect overcoming above-mentioned prior art, a kind of growth GaN film on a si substrate and preparation method thereof is provided, this preparation method is unique and easy, there is repeatability, the defect concentration of obtained GaN film be low, crystal mass is high, electricity and optical property excellent.
For achieving the above object, the present invention adopts following technical scheme:
A growth GaN film on a si substrate, is characterized in that: comprise Si substrate layer, the Al grown on Si substrate layer
2o
3protective layer, to grow at Al
2o
3gaN film layer on protective layer.The present invention first grows Al on Si substrate layer
2o
3protective layer, the layer of regrowth GaN film afterwards, Al
2o
3protective layer effectively can prevent the interface of Si substrate and active N from reacting and form unbodied Si
xn
y, thus avoid Si
xn
ythe impact of layer on GaN growth quality, obtains high-quality GaN film.In addition, Al
2o
3protective layer can alleviate thermal stress mismatch (114%) huge between Si substrate and GaN, prevents Si to be diffused in GaN simultaneously.
Preferably, described Al
2o
3the thickness of protective layer is 3-5nm.
A preparation method for growth GaN film on a si substrate, comprises and chooses Si substrate; (111) crystal face choosing Si substrate plates one deck Al layer, then passes into oxygen plasma to forming Al
2o
3protective layer; Again at Al
2o
3growing GaN thin layer on protective layer.
Preferably, adopting molecular beam epitaxial growth method on Si (111) crystal face, plate the Al layer that thickness is 3-5nm, passing into oxygen plasma when Si substrate is 800-900 DEG C to forming Al
2o
3protective layer, insulation.
Preferably, adopt pulsed laser deposition growth method at Al
2o
3growing GaN thin layer on protective layer, underlayer temperature is 600-700 DEG C, and chamber pressure is 3-4 × 10
-10mTorr, V/III is than being 0.8-1.1ML/s for 30-40, the speed of growth, and after GaN film layer growth, insulation 25-35 minute, temperature is 650-750 DEG C.
Preferably, before plating Al layer, first polishing, surface cleaning process, annealing in process are carried out successively to Si substrate.
Preferably, polishing carries out polishing with diamond to Si substrate surface, after not having cut, then adopts the cmp method of prior art to carry out polishing to Si substrate with observation by light microscope Si substrate surface.
Preferably, described surface cleaning processing method is: Si substrate is put into the ultrasonic process of acetone soln, then use washed with de-ionized water; Then ultrasonic process in isopropyl acetone solution; Soak in a solution of hydrofluoric acid again; Then put into deionized water to soak; Finally soak in the mixed solution of sulfuric acid and hydrogen peroxide, then through hydrofluoric acid dips, then use deionized water rinsing, nitrogen dries up, and deposits in nitrogen cabinet.
Preferably, annealing in process is that Si substrate to be placed on pressure be 2 × 10
-10in the growth room of the ultra high vacuum of Torr, at 900-1000 DEG C, high-temperature baking 3-5h is to remove the pollutant of Si substrate surface, and then air cooling is to room temperature.
Growth of the present invention GaN film on a si substrate can be used in LED component or in solar cell.
Compared with prior art, the invention has the beneficial effects as follows:
1, choose Si substrate, first on Si substrate layer, grow Al
2o
3protective layer, the layer of regrowth GaN film afterwards, Al
2o
3protective layer effectively can prevent the interface of Si substrate and active N from reacting and form unbodied Si
xn
y, thus avoid Si
xn
ythe impact of layer on GaN growth quality, obtains high-quality GaN film.In addition, Al
2o
3protective layer can alleviate thermal stress mismatch (114%) huge between Si substrate and GaN, prevents Si to be diffused in GaN simultaneously.
2, pulsed laser deposition growth method growing GaN thin layer is under cryogenic adopted, by reducing growth temperature, effectively resist the amplification of conventional metals organic chemical vapor deposition technique (MOCVD) high growth temperature nitride (generally all more than 1000 DEG C) to the lattice mismatch of substrate and GaN, reduce the defect concentration of nitride film.
3, the present invention adopts Si substrate, its good heat dissipation, low price, is conducive to reducing production cost.
In sum, growth technique of the present invention is unique and easy, and have repeatability, epitaxially grown GaN film defect concentration is low, crystal mass is high, electricity and optical property excellent.
Accompanying drawing explanation
Fig. 1 is the structural representation of growth of the present invention GaN film on a si substrate;
Fig. 2 is the X ray Surface scan collection of illustrative plates of growth of the present invention GaN film on a si substrate;
Fig. 3 is the schematic diagram that growth of the present invention GaN film is on a si substrate applied in LED component;
Fig. 4 is growth of the present invention GaN film application schematic diagram in solar cells on a si substrate.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
Please refer to Fig. 1, growth of the present invention GaN film on a si substrate comprise Si substrate layer 11, the Al grown on Si substrate layer 11
2o
3protective layer 12, to grow at Al
2o
3gaN film layer 13 on protective layer 12.
Above-mentioned growth GaN film is on a si substrate adopted and is obtained with the following method: choose Si substrate; (111) crystal face choosing Si substrate plates one deck Al layer, then passes into oxygen plasma to forming Al
2o
3protective layer; Again at Al
2o
3growing GaN thin layer on protective layer.Detailed process is as follows:
(1) select Si substrate, select crystal orientation to be (111) crystal face.
(2) molecular beam epitaxial growth method is adopted at Si(111) upper plating one deck Al layer is 800 at underlayer temperature
Oxygen plasma is passed into forming Al when-900 DEG C
2o
3protective layer, insulation 30min.
(3) adopt pulsed laser deposition growth method at Al
2o
3growing GaN thin layer on protective layer: use target
Ga and operating pressure are 1.5-2.0 × 10
-6the N of Torr
2radio frequency plasma free-radical generator is at Al
2o
3protective layer reacts growing GaN thin layer, process conditions are: underlayer temperature is 600-700 DEG C, and chamber pressure is 3-4 × 10
-10mTorr, V/III ratio are 30-40, the speed of growth is 0.8-1.1ML/s.
(4) be incubated 25-35 minute, temperature is 650-750 DEG C.
In preferred version, described GaN film layer is monocrystal thin films.
In preferred version, Al
2o
3the thickness of protective layer is 3-5nm, and concrete operation method is: step poly-(2)
At Si(111) above plate the Al layer that thickness is 3-5nm, pass into oxygen plasma when underlayer temperature is 800-900 DEG C to forming Al
2o
3protective layer, insulation 30min.
Embodiment 2
The present embodiment carries out improving on the basis of embodiment 1, and difference is: before plating Al layer, and first carry out polishing, surface cleaning process, annealing in process successively to Si substrate, concrete operation method is as follows:
Polishing: carry out polishing to Si substrate surface with diamond, after not having cut, then adopts the cmp method of prior art to carry out polishing to Si substrate with observation by light microscope Si substrate surface.
Surface cleaning process: the draw-in groove that Si substrate is housed is put into clean square cup, adds deionized water and the acetone that prepared until solution complete submergence Si substrate, ultrasonic 5-10 minute; Square cup is put into ultrasonic tank, and add deionized water until the liquid level of water is a little less than square cup, carry out ultrasonic cleaning 5-10 minute, ultrasonic power is 60-80 watt; Square cup after ultrasonic is taken out, with washed with de-ionized water 2-3 time, until cleaned by acetone; Isopropyl acetone solution is injected, ultrasonic 5-10 minute in square cup; Square cup is put into ultrasonic tank, and add isopropyl acetone until the liquid level of solution is a little less than square cup, carry out ultrasonic cleaning 5-10 minute, ultrasonic power is 60-80 watt; Square cup after ultrasonic is taken out, spends isopropyl acetone solution cleaning 2-3 time; In square cup, add deionized water, until submergence Si substrate, then put it into cleaning 5-10 minute in ultrasonic tank; The side's of taking-up cup, then the draw-in groove in the side's of taking-up cup, in square cup, hydrogen injecting fluoric acid and water are until its liquid level is slightly less than or equals the diameter of Si substrate; With the clip of polytetrafluoroethylene by the Si substrate side of standing on cup, Si substrate is taken out from hydrofluoric acid solution, puts into deionized water and soak 1-2 minute; The preparation concentrated sulfuric acid: the solution of hydrogen peroxide=4:1, in square cup, adds the deionized water of equivalent, is taken out by Si substrate and put into dioxysulfate water 5-7 minute from hydrofluoric acid; Again Si substrate is put into hydrofluoric acid 1-2 minute, electronic-stage hydrofluoric acid: water=1:10; With deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
Annealing in process: Si substrate being placed on pressure is 2 × 10
-10in the growth room of the ultra high vacuum of Torr, at 900-1000 DEG C, high-temperature baking 3-5h is to remove the pollutant of Si substrate surface, and then air cooling is to room temperature.
Please refer to Fig. 2, can see from X ray Surface scan collection of illustrative plates, GaN film layer is at use Al
2o
3protective layer grows at Si substrate epitaxial as under the condition of protection, and epitaxial relationship is: GaN (0002) //Al
2o
3(0006) //Si (111).
The embodiment 3 growth of the present invention application of GaN film in LED component on a si substrate
Please refer to Fig. 3, the growth GaN film on a si substrate embodiment 2 obtained is applied in LED component, and method is: at the high-quality Al of Si (111) crystal face Epitaxial growth
2o
3protective layer, then at Al
2o
3protective layer Epitaxial growth GaN monocrystal thin films, after defining GaN monocrystal thin films layer 10, the N-shaped of growing high-quality mixes silicon GaN epitaxial layer 11, In successively
xga
1-xn multiple quantum well layer 12, p-type mixes magnesium GaN layer 13, and obtain the electric elements containing long GaN film on a si substrate, detailed process is as follows:
On GaN monocrystal thin films layer 10, growing n-type mixes silicon GaN epitaxial layer 11, and its thickness is about 5 μm, and the concentration of its charge carrier is 1 × 10
19cm
-3.Then In is grown
xga
1-xn multiple quantum well layer 12, thickness is about 112nm, and periodicity is 7, wherein In
xga
1-xn well layer is 3nm, and barrier layer is 13nm, 0 < x < 1.The p-type that regrowth Mg adulterates afterwards mixes magnesium GaN layer 13, and thickness is about 350nm, and its carrier concentration is 2 × 10
16cm
-3.Last electron beam evaporation forms ohmic contact.Pass through at N on this basis
2anneal under atmosphere, improve carrier concentration and mobility that p-type mixes magnesium GaN layer 13.
The electric elements containing long GaN film on a si substrate obtained are applied in LED component, can improve luminous efficiency and the radiating efficiency of LED component.
Embodiment 4 growth of the present invention GaN film application in solar cells on a si substrate
Please refer to Fig. 4, in solar cells, method is: at the high-quality Al of Si (111) crystal face Epitaxial growth in growth embodiment 2 obtained GaN film application on a si substrate
2o
3protective layer, then at Al
2o
3protective layer Epitaxial growth GaN monocrystal thin films, after defining GaN monocrystal thin films layer 30, regrowth has the In of component gradient
xga
1-xn resilient coating 31, N-shaped mix silicon In
xga
1-xn layer 32, In
xga
1-xn multiple quantum well layer 33, p-type mix magnesium In
xga
1-xn layer 34, obtain the electric elements containing long GaN film on a si substrate, detailed process is as follows:
The In with component gradient of growing high-quality on GaN monocrystal thin films layer 30
xga
1-xthe value of N resilient coating 31, its x can be adjustable between 0-0.2; Then growing n-type mixes silicon In
xga
1-xn layer 32, its thickness is about 5 μm, and the concentration of its charge carrier is 1 × 10
19cm
-3, 0 < x < 1.Then In is grown
xga
1-xn multiple quantum well layer 33, thickness is about 300nm, and periodicity is 20,0 < x < 1, wherein In
0.2ga
0.8n well layer is 3nm, In
0.08ga
0.92n barrier layer is 10nm.The p-type that regrowth Mg adulterates mixes magnesium In
xga
1-xn layer 34, thickness is about 200nm, and 0 < x < 1, its carrier concentration is 2 × 10
16cm
-3.Last electron beam evaporation forms ohmic contact.Pass through at N on this basis
2anneal under atmosphere, improve p-type and mix magnesium In
xga
1-xthe carrier concentration of N layer 34 and mobility.
The electric elements containing long GaN film on a si substrate obtained are applicable to application in solar cells.
Above-described embodiment is only the preferred embodiment of the present invention, can not limit protection scope of the present invention with this, and change and the replacement of any unsubstantiality that those skilled in the art does on basis of the present invention all belong to protection scope of the present invention.
Claims (5)
1. a preparation method for growth GaN film on a si substrate, is characterized in that: choose Si substrate; (111) crystal face choosing Si substrate adopts molecular beam epitaxial growth method to plate one deck Al layer, then passes into oxygen plasma when Si substrate is 800-900 DEG C to forming 3-5nmAl
2o
3protective layer; Again at Al
2o
3protective layer adopts pulsed laser deposition growth method growing GaN thin layer;
Described pulsed laser deposition growth method response parameter: underlayer temperature is 600-700 DEG C, chamber pressure is 3-4 × 10
-10mTorr, V/III is than being 0.8-1.1ML/s for 30-40, the speed of growth, and after GaN film layer growth, be incubated 25-35 minute, temperature is 650-750 DEG C;
Before plating Al layer, first polishing, surface cleaning process, annealing in process are carried out successively to Si substrate.
2. the preparation method of growth as claimed in claim 1 GaN film on a si substrate, it is characterized in that: polishing carries out polishing with diamond to Si substrate surface, after not having cut with observation by light microscope Si substrate surface, then the cmp method of prior art is adopted to carry out polishing to Si substrate.
3. the preparation method of growth as claimed in claim 1 GaN film on a si substrate, it is characterized in that, described surface cleaning processing method is: Si substrate is put into the ultrasonic process of acetone soln, then use washed with de-ionized water; Then ultrasonic process in isopropyl acetone solution; Soak in a solution of hydrofluoric acid again; Then put into deionized water to soak; Finally soak in the mixed solution of sulfuric acid and hydrogen peroxide, then through hydrofluoric acid dips, then use deionized water rinsing, nitrogen dries up, and deposits in nitrogen cabinet.
4. the preparation method of growth as claimed in claim 1 GaN film on a si substrate, is characterized in that: annealing in process is that Si substrate to be placed on pressure be 2 × 10
-10in the growth room of the ultra high vacuum of Torr, at 900-1000 DEG C, high-temperature baking 3-5h is to remove the pollutant of Si substrate surface, and then air cooling is to room temperature.
5. the preparation method of the GaN film on a si substrate of the growth described in Claims 1-4 any one is applied in LED component or in solar cell.
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| CN103633203B (en) * | 2013-05-08 | 2016-12-28 | 南京邮电大学 | Unsettled nitride film LED component and preparation method thereof |
| CN103388178B (en) * | 2013-08-07 | 2016-12-28 | 厦门市三安光电科技有限公司 | Group III-nitride epitaxial structure and growing method thereof |
| CN103681992A (en) | 2014-01-07 | 2014-03-26 | 苏州晶湛半导体有限公司 | Semiconductor substrate, semiconductor device and semiconductor substrate manufacturing method |
| CN103996758A (en) * | 2014-05-30 | 2014-08-20 | 广州市众拓光电科技有限公司 | LED epitaxial wafer growing on Cu substrate and preparing method and application of LED epitaxial wafer |
| CN104037282B (en) * | 2014-06-10 | 2017-03-08 | 广州市众拓光电科技有限公司 | Growth AlGaN thin film on a si substrate and its preparation method and application |
| CN104037285B (en) * | 2014-06-10 | 2017-03-08 | 广州市众拓光电科技有限公司 | A kind of growth GaN film on a si substrate and its preparation method and application |
| CN104051044A (en) * | 2014-06-29 | 2014-09-17 | 西安电子科技大学 | Series-connection sandwich-type epitaxy GaN PIN-type beta irradiation battery and preparation method |
| CN105742374B (en) * | 2014-12-09 | 2017-12-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | photovoltaic device and preparation method thereof |
| CN105591004B (en) * | 2016-03-29 | 2020-07-10 | 苏州晶湛半导体有限公司 | L ED epitaxial wafer based on patterned Si substrate and preparation method thereof |
| CN106601854A (en) * | 2016-11-28 | 2017-04-26 | 中国电子科技集团公司第四十八研究所 | Heterojunction solar cell and manufacturing method thereof |
| CN111341915B (en) * | 2020-05-19 | 2020-09-01 | 季华实验室 | Method for manufacturing organic crystal solar cell device and photoelectric equipment |
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Effective date of registration: 20170410 Address after: 517000 Guangdong high tech Development Zone, Industrial Avenue, east of the East, the first high tech service center on the third floor, room 317, Patentee after: HEYUAN ZHONGTUO PHOTOELECTRIC TECHNOLOGY CO., LTD. Address before: The science city of Guangzhou high tech Industrial Development Zone 510000 Guangdong province Guangzhou Nanxiang Road No. 62 building Patentee before: Guangzhou Zhongtuo Optoelectrical Technology Co., Ltd. |