CN103022295A - Aluminum nitride film growing on silicon substrate and preparation method and application thereof - Google Patents
Aluminum nitride film growing on silicon substrate and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an aluminum nitride film growing on a silicon substrate and a preparation method and the application thereof. The aluminum nitride film is obtained by the following preparation method: adopting the silicon substrate, selecting the (111) crystal face of the silicon substrate as crystal orientation, growing an aluminum buffer layer on the (111) crystal face of the silicon and then growing an aluminum nitride film in epitaxial growth mode. The silicon is adopted as the substrate, simultaneously a pulse laser deposition growth method is adopted to grow the aluminum nitride film on the Si (111) substrate, the aluminum nitride film crystal grows in preferred orientation to obtain low lattice mismatch degree between the substrate and the aluminum nitride, quality of the aluminum nitride crystal is greatly improved, and the aluminum nitride film is suitable for being applied to photoelectric detectors and light-emitting diode (LED) devices.
Description
Technical field
The present invention relates to AlN film field, be specifically related to AlN film on a kind of Si of being grown in substrate and its preparation method and application.
Background technology
AlN is III A compounds of group, generally exist with the wurtzite structure in the hexagonal crystal system, the performance that many excellences are arranged is such as high heat conductivity, low thermal coefficient of expansion, high electrical insulation property, high dielectric breakdown strength, excellent mechanical strength, excellent chemical stability and low toxic, good optical property etc.Because AlN has many excellent properties, band gap length, polarization are by force, energy gap is 6. 2eV, makes it at machinery, microelectronics, optics, and the fields such as electronic devices and components, SAW (Surface Acoustic Wave) device manufacturing, high-frequency wideband communication and power semiconductor have broad application prospects.
At present, the application of AlN is mainly reflected in the following aspects: piezoelectric, epitaxial buffer layer material, luminescent layer material.On the one hand, because the AlN material has the excellent specific properties such as the electron drift saturation rate is high, thermal conductivity is high, dielectric breakdown strength is high, it has huge potentiality in high frequency, high temperature, high voltage electronics field, and the AlN film of wurtzite structure has the piezoelectric property that the two-forty sound wave is learned, its surperficial acoustics is the highest in known piezoelectric, and have larger electromechanical coupling factor, so AlN is the preferred material for the preparation of the high frequency surface wave device.On the other hand, because AlN has advantages of high thermal conductance, low-thermal-expansion and than broad-band gap, and with the GaN lattice coupling is arranged preferably, with AlN as resilient coating can Effective Raise GaN, the crystal mass of InN epitaxial film, obviously improve its electricity and optical property.In addition, AlN can be used as the luminescent material of blue light ultraviolet light, if mix or make composite membrane, luminescent spectrum will cover whole visible region.
The AlN film must have higher crystalline quality, could satisfy above many-sided application.The method that is usually used at present preparing the AlN film has chemical vapour deposition technique, magnetron sputtering method, pulsed laser deposition and molecular beam epitaxy etc.Yet most preparation methods requires substrate is heated to higher temperature, but higher temperature may cause the damage of backing material, and this is a great problem of AlN film preparation.And, reach the requirement of growing high-quality AlN crystal, then need complicated equipment and instrument, involve great expense, and the speed of growth of single film is slower the high cost of single sample.
Summary of the invention
The object of the invention is to overcome the defective of above-mentioned prior art, AlN film on a kind of Si of being grown in substrate and preparation method thereof is provided, it obtains high-quality AlN film, and has reduced preparation cost by selecting the control of suitable substrate and crystallographic direction and technological parameter.
Another object of the present invention is to provide the application of above-mentioned AlN film.
For achieving the above object, the present invention adopts following technical scheme:
A kind of AlN film that is grown on the Si substrate, it adopts the method that is prepared as follows to obtain: adopt the Si substrate, selecting (111) crystal face of Si substrate is crystal orientation, grows the Al resilient coating at Si (111) crystal face first, again epitaxial growth AlN film.Different Grown AlN films, its performance is different, but the lattice mismatch between various types of substrates material and AlN crystal is the key factor that affects the film growth quality.Depositing Al N film can be practical, integrated with its photoelectric characteristic on the Si substrate.Si atom on Si (111) crystal face has the class hexagonal structure to be arranged, and is fit to direct growth AlN film.
Preferably, before growth Al resilient coating, the pre-treatment step that substrate is carried out successively surface finish, cleaning, annealing.
The concrete grammar of surface finish is: the Si substrate surface is polished with diamond mud, do not have cut with the observation by light microscope substrate surface after, adopt the chemical mechanical polishing method of prior art that substrate is carried out polishing.
The concrete grammar of cleaning step is: the Si substrate is placed on first ultrasonic cleaning in the acetone soln, and then is placed on the deionized water for ultrasonic cleaning; Then ultrasonic cleaning in isopropyl acetone solution; Then ultrasonic cleaning in hydrofluoric acid solution is soaked in deionized water again; Again the Si substrate is placed in the mixed solution of sulfuric acid and hydrogen peroxide and soaks; At last the Si substrate is put into hydrofluoric acid and soak, use deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
The concrete grammar of annealing is: the Si substrate is placed in the growth room of ultra high vacuum, removes the pollutant on surface at 900-1000 ℃ of lower baking 3-5h, then air cooling is to room temperature.After above annealing in process, can make substrate obtain the surface of atomically flating, be conducive to growing high-quality AlN film.
Adopt molecular beam epitaxial growth method growth Al resilient coating, substrate temperature is 500-600 ℃, and vacuum degree is 10
-10More than the Torr.
Adopt pulsed laser deposition growth method epitaxial growth AlN film, underlayer temperature is 650-750 ℃, and chamber pressure is that 10-15mTorr, V/III ratio is 0.4-0.6 ML/s for 50-60, the speed of growth.
Adopt the molecular beam epitaxial growth method to combine with the pulsed laser deposition growth method, utilize first molecular beam epitaxial growth Al resilient coating, recycling pulsed laser deposition epitaxial growth method growing AIN film, can improve epitaxially grown efficient, characteristic optimum selecting epitaxy method according to base material is conducive to the raising of the quality of epitaxial loayer.In addition, lattice mismatch between AlN film and the Si substrate is up to 19%, thermal coefficient of expansion differs 44%, the problem such as Presence of an interface diffusion also, cause directly the AlN of Si Grown film crystal second-rate, defect concentration is high, thereby reduced the luminous efficiency of AlN thin film based device, be difficult to reach the requirement of photoelectric device.And by reducing growth temperature, establishment the amplification of the hot conditions of traditional metal organic chemical vapor deposition technique (MOCVD) growing nitride (generally all more than 1000 ℃) to substrate and AlN lattice mismatch and coefficient of thermal expansion mismatch degree, the nitride film defective is reduced, improved the quality of AlN film.In addition, the factors such as technological parameter and oxygen content all can affect the quality of the AlN crystal of acquisition, and when oxygen content was higher, oxygen very easily and reactive aluminum generated in the lattice structure that oxide enters the AlN film and forms defective, thereby reduced the luminous efficiency of AlN base device.In order to reduce oxygen to the impact of membrane structure, take above-mentioned technological parameter, control vacuum degree, reative cell are pressed, evacuation time etc., can obtain high-quality AlN film.
Preferably, the thickness of Al resilient coating is 3-5nm.Can detect by RHEED, control the growing state of this layer.
AlN film on the Si of the being grown in substrate of the present invention can be applied in photodetector, the LED device.
Compared with prior art, the invention has the beneficial effects as follows:
1, use Si to be substrate, adopt simultaneously the pulsed laser deposition growth method at Si(111) growing AIN film on the crystal face, the growth of AlN crystal preferred orientation obtains lattice mismatch very low between substrate and the AlN, has greatly improved the quality of AlN crystal.
2, adopt pulsed laser deposition growth method growing AIN film, both for low-temperature epitaxy AlN provides the basis, can effectively shorten again the nucleated time of nitride, the unicity of the AlN film that assurance obtains.
3, adopt the molecular beam epitaxial growth method to combine with the pulsed laser deposition epitaxial growth method, utilize first molecular beam epitaxy technique growth Al resilient coating, recycling pulsed laser deposition epitaxy technology growing AIN film, improved epitaxially grown efficient, characteristic optimum selecting epitaxy method according to base material is conducive to the raising of epitaxial layer quality.Simultaneously, by reducing growth temperature, establishment the hot conditions (generally all more than 1000oC) of traditional metal organic chemical vapor deposition technique (MOCVD) growing nitride to the lattice mismatch of substrate and AlN and the amplification of coefficient of thermal expansion mismatch degree, the nitride film defective is reduced.
4, Si easily obtains as substrate, low price, and adopted low temperature growth techniques, be conducive to reduce production costs.
In sum, the unique and easy row of preparation technology of the present invention, production cost is low, and the AlN film of acquisition has advantages of that defect concentration is low, crystal mass is high, electricity and optical property excellence.
Description of drawings
Fig. 1 is the structural representation that is grown in the AlN film on the Si substrate of the present invention;
Fig. 2 is the X ray face scanning spectra that is grown in the AlN film on the Si substrate of the present invention;
Fig. 3 is (002) the face X ray swing curve figure that is grown in the AlN film on the Si substrate of the present invention;
Fig. 4 is the GIXR collection of illustrative plates that is grown in the AlN film on the Si substrate of the present invention;
Fig. 5 is that the AlN film on the Si of the being grown in substrate of the present invention is applied in the schematic diagram in the LED device;
Fig. 6 is that the AlN film on the Si of the being grown in substrate of the present invention is applied in the schematic diagram in the photodetector.
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, the AlN film on the Si of the being grown in substrate of the present invention comprises Si substrate layer 11, is grown in the AlN thin layer 12 on the Si substrate layer 11.Described AlN thin layer 12 is monocrystal thin films layer or polycrystal film layer.
This AlN film that is grown on the Si substrate adopts following method to make:
(1) selection in substrate and crystal orientation: choose the Si substrate, choose simultaneously (111) crystal face of Si substrate.
(2) adopt the molecular beam epitaxial growth method, at Si Grown Al resilient coating, process conditions are:
Underlayer temperature is 500-600 ℃, and vacuum degree is 10
-10More than the Torr, the speed of growth is 0.6nm/min, and growth Al buffer layer thickness is 3-5nm, detects, controls growing state by RHEED.
(3) plasma that passes into nitrogen carries out nitrogenize to the Al resilient coating.
(4) adopt pulsed laser deposition growth method growing AIN film, process conditions are: underlayer temperature is
650-750 ℃, chamber pressure is that 10-15mTorr, V/III ratio is 0.4-0.6 ML/s for 50-60, the speed of growth.Specifically: be that 2.0-3.0 J/cm2 and repetition rate are KrF excimer laser (λ=248nm of 20-25Hz with ability, t=20ns) PLD ablation AlN target, when depositing Al N film, the internal pressure N2 of growth room remains on 10-15mTorr, guarantees to obtain high-quality AlN film.
(5) insulation is 25-35 minute, and temperature is 650-750 ℃.
Embodiment 2
The present embodiment is to change one's profession on the basis of embodiment 1, and difference is: before the growing AIN resilient coating, substrate is carried out successively the pre-treatment step of surface finish, cleaning, annealing, concrete grammar is as follows:
Surface finish is processed: the Si substrate surface is polished with diamond mud, do not have cut with the observation by light microscope substrate surface after, adopt again the cmp method of prior art that substrate is carried out polishing.
Clean: the draw-in groove that the Si sheet will be housed is put into clean square cup, add deionized water and the acetone that prepared until the complete submergence Si of solution sheet, ultrasonic 5-10 minute; Square cup is put into ultrasonic tank, add deionized water until the liquid level of water a little less than square cup, carried out ultrasonic cleaning 5-10 minute, ultrasonic power is 60-80 watt; Square cup after ultrasonic is taken out, use washed with de-ionized water 2-3 time, until acetone is cleaned; In square cup, inject IPA solution, ultrasonic 5-10 minute; Square cup is put into ultrasonic tank, add IPA until the liquid level of solution a little less than square cup, carried out ultrasonic cleaning 5-10 minute, ultrasonic power is 60-80 watt; Square cup after ultrasonic is taken out, spend IPA solution and clean 2-3 time; In square cup, add deionized water, until submergence Si sheet puts it in the ultrasonic tank again and cleaned 5-10 minute; The side's of taking-up cup, the draw-in groove in the side's of taking-up cup again, hydrogen injecting fluoric acid and water are until its liquid level is slightly less than or equals the diameter of Si sheet in square cup; , with in the Si sheet side of standing on cup the Si sheet is taken out from hydrofluoric acid solution with the clip of polytetrafluoroethylene, put into deionized water and soaked 1-2 minute; The solution of the preparation concentrated sulfuric acid: hydrogen peroxide=4:1 adds the deionized water of equivalent in square cup, the Si sheet is taken out from hydrofluoric acid and put into dioxysulfate water 5-7 minute; Again the Si sheet is put into hydrofluoric acid 1-2 minute electronic-stage hydrofluoric acid: water=1:10; Use deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
Annealing: it is 2 * 10 that substrate is placed on pressure
-10In the growth room of the ultra high vacuum of Torr, to remove the pollutant of substrate surface, then air cooling is to room temperature at 900-1000 ℃ of lower high-temperature baking 3-5 h.
Please refer to Fig. 2, can see from X ray face scanning spectra, the success of AlN film is in the capable epitaxial growth of Si substrate, and epitaxial relationship is: AlN (002) //Si (111).
Please refer to Fig. 3, can see from X ray backswing allusion quotation line chart, half-peak breadth (FWHM) value of AlN (002) film is lower than 0.1 °, calculates as can be known thus, and its defect concentration is lower than 2 * 10
8Cm
-2, show that on Si (111) face epitaxial growth has gone out the high-quality AlN film of fabricating low-defect-density.
Please refer to Fig. 4, X ray glancing incidence (GIXR) test shows that the heterogeneous joint of AlN/Si is the atom level sudden change, for growing high-quality AlN film is given security.
In sum, no matter be in defect concentration, or aspect crystalline quality, adopt the molecular beam epitaxial growth method AlN film that obtains at the Si substrate that combines with the pulsed laser deposition epitaxial growth method to have excellent properties, be better than the correlated results of the AlN film of the application conventional substrate acquisition reported at present.
Embodiment 3 application of AlN film in the LED device that are grown on the Si substrate of the present invention
Please refer to Fig. 5, the AlN film that embodiment 2 is obtained is applied to the method in the LED device, and it is included in epitaxial growth high-quality AlN film on Si (111) crystal face, after forming AlN film 10, the U-GaN thin layer 11 of growing high-quality successively, N-shaped is mixed silicon GaN epitaxial loayer 12, In
xGa
1-xN multiple quantum well layer 13, p-type are mixed magnesium GaN layer 14, and be specific as follows:
The U-GaN thin layer 11 of growing high-quality on AlN film 10; Growing n-type is mixed silicon GaN epitaxial loayer 12 on U-GaN thin layer 11 again, and its thickness is about 5 μ m, and the concentration of its charge carrier is 1 * 10
19Cm
-3In then grows
xGa
1-xN multiple quantum well layer 13, thickness are about 112 nm, and periodicity is 7, wherein In
xGa
1-xN trap layer is 3 nm, and building layer is 13 nm, 0＜x＜1.The p-type of afterwards regrowth Mg doping is mixed magnesium GaN layer 14, and thickness is about 350 nm, and its carrier concentration is 2 * 10
16Cm
-3Last electron beam evaporation forms ohmic contact.Pass through at N on this basis
2Anneal under the atmosphere, improved carrier concentration and mobility that p-type is mixed magnesium GaN layer 14.
Embodiment 4 application of AlN film in photodetector that are grown on the Si substrate of the present invention
Please refer to Fig. 6, the AlN film of embodiment 2 acquisitions is applied to the method for photodetector, comprising epitaxial growth high-quality AlN film on Si (111) crystal face, after forming AlN film 20, the U-GaN thin layer 21 of growing high-quality successively, N-shaped is mixed silicon GaN epitaxial loayer 22, non-Doped GaN layer 23, and p-type is mixed magnesium GaN layer 24.
At AlN film 20 growth U-GaN thin layers 21, its thickness is about 300nm; Growing n-type is mixed silicon GaN epitaxial loayer 22 on U-GaN thin layer 21, and its thickness is about 3 μ m, and the concentration of its charge carrier is 1 * 10
19Cm
-3The non-Doped GaN epitaxial loayer 23 of then growing, thickness is about 200 nm, and its carrier concentration is 2. 2 * 10
16Cm
-3The p-type of afterwards regrowth Mg doping is mixed magnesium GaN layer 24, and thickness is about 1. 5 μ m.Last electron beam evaporation forms ohmic contact and schottky junction.Pass through at N on this basis
2Anneal under the atmosphere, improved carrier concentration and mobility that p-type is mixed magnesium GaN layer 24.The GaN UV photodetector of prepared p-i-n structure is under 1 V bias voltage, and dark current only is 65 pA, and device is under 1 V bias voltage, has reached 0. 92 A/W in the maximum of 361 nm place responsivenesses.
Above-described embodiment only is preferred implementation of the present invention, can not limit protection scope of the present invention with this, and the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to protection scope of the present invention.
Claims (10)
1. AlN thin film technology method that is grown on the Si substrate is characterized in that: adopt the Si substrate, selecting (111) crystal face of Si substrate is crystal orientation, grows the Al resilient coating at Si (111) crystal face first, again epitaxial growth AlN film.
2. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 1 is characterized in that: before growth Al resilient coating, and the pre-treatment step that substrate is carried out successively surface finish, cleaning, annealing.
3. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 2, it is characterized in that, the concrete grammar of surface finish is: the Si substrate surface is polished with diamond mud, after not having cut with the observation by light microscope substrate surface, adopt the chemical mechanical polishing method of prior art that substrate is carried out polishing.
4. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 2 is characterized in that, the concrete grammar of cleaning step is: the Si substrate is placed on first ultrasonic cleaning in the acetone soln, and then is placed on the deionized water for ultrasonic cleaning; Then ultrasonic cleaning in isopropyl acetone solution; Then ultrasonic cleaning in hydrofluoric acid solution is soaked in deionized water again; Again the Si substrate is placed in the mixed solution of sulfuric acid and hydrogen peroxide and soaks; At last the Si substrate is put into hydrofluoric acid and soak, use deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
5. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 2, it is characterized in that, the concrete grammar of annealing is: the Si substrate is placed in the growth room of ultra high vacuum, removes the pollutant on surface at 900-1000 ℃ of lower baking 3-5h, then air cooling is to room temperature.
6. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 1 is characterized in that: adopt molecular beam epitaxial growth method growth Al resilient coating, substrate temperature is 500-600 ℃, and vacuum degree is 10
-10More than the Torr.
7. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 1, it is characterized in that: adopt pulsed laser deposition growth method epitaxial growth AlN film, underlayer temperature is 650-750 ℃, and chamber pressure is that 10-15mTorr, V/III ratio is 0.4-0.6 ML/s for 50-60, the speed of growth.
8. the AlN thin film technology method that is grown on the Si substrate as claimed in claim 1, it is characterized in that: the thickness of Al resilient coating is 3-5nm.
9. an AlN film that is grown on the Si substrate is characterized in that: adopt the described preparation method of claim 1 to 8 any one to obtain.
10. the application of AlN film in preparation photodetector, LED device that is grown on the Si substrate claimed in claim 9.
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| CN104037285A (en) * | 2014-06-10 | 2014-09-10 | 广州市众拓光电科技有限公司 | GaN thin film growing on Si substrate and preparation method and applications thereof |
| CN104037282A (en) * | 2014-06-10 | 2014-09-10 | 广州市众拓光电科技有限公司 | AlGaN film grown on Si substrate, preparation method and application thereof |
| CN105703732A (en) * | 2016-01-18 | 2016-06-22 | 佛山市艾佛光通科技有限公司 | Method for preparing film bulk acoustic wave resonator on the basis of monocrystal AlN |
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| CN103022295B (en) | 2015-03-04 |
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