CN103022295B - 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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- CN103022295B CN103022295B CN201210536779.XA CN201210536779A CN103022295B CN 103022295 B CN103022295 B CN 103022295B CN 201210536779 A CN201210536779 A CN 201210536779A CN 103022295 B CN103022295 B CN 103022295B
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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 applications, be specifically related to a kind of growth AlN film on a si substrate and its preparation method and application.
Background technology
AlN is III A compounds of group, generally exist with the wurtzite structure in hexagonal crystal system, there is the performance of many excellences, 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 field such as electronic devices and components, SAW (Surface Acoustic Wave) device manufacture, high-frequency wideband communication and power semiconductor has broad application prospects.
At present, the application of AlN is mainly reflected in the following aspects: piezoelectric, epitaxial buffer layer material, emitting layer material.On the one hand, because AlN material has the excellent specific properties such as 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 of two-forty sound wave, its surface acoustic is the highest in known piezoelectric, and there is larger electromechanical coupling factor, therefore AlN is the preferred material for the preparation of Frequency Surface wave device.On the other hand, because AlN has the advantage of high thermal conductance, low-thermal-expansion and wider band gap, and have good coupling with GaN lattice, effectively can improve the crystal mass of GaN, InN epitaxial film with AlN as resilient coating, obviously improve its electricity and optical property.In addition, AlN can as the luminescent material of blue light ultraviolet light, if carry out adulterating or making composite membrane, luminescent spectrum will cover whole visible region.
AlN film must have higher crystalline quality, could meet above many-sided application.The method being usually used in preparing AlN film at present has chemical vapour deposition technique, magnetron sputtering method, pulsed laser deposition and molecular beam epitaxy etc.But most preparation methods requires by silicon to higher temperature, but higher temperature may cause the damage of backing material, and this is a great problem of AlN film preparation.Further, the requirement of growing high-quality AlN crystal be reached, then need complicated equipment and instrument, involve great expense, and the speed of growth of single film is comparatively slow, the high cost of single sample.
Summary of the invention
The object of the invention is to the defect overcoming above-mentioned prior art, a kind of growth AlN film on a si substrate and preparation method thereof is provided, it obtains high-quality AlN film by selecting the control of suitable substrate and crystallographic direction and technological parameter, and reduces preparation cost.
Another object of the present invention is to the application that above-mentioned AlN film is provided.
For achieving the above object, the present invention adopts following technical scheme:
A growth AlN film on a si substrate, it adopts following preparation method to obtain: adopt Si substrate, and (111) crystal face selecting Si substrate is crystal orientation, first on Si (111) crystal face, grows Al resilient coating, then epitaxial growth AlN film.Growing AIN film on various substrates, its performance is different, but the lattice mismatch between various types of substrates material and AlN crystal is the key factor affecting film growth quality.Depositing Al N thin film can by practical for its photoelectric characteristic, integrated on a si substrate.Si atom on Si (111) crystal face has the arrangement of class hexagonal structure, is applicable to direct growth AlN film.
Preferably, before growth Al resilient coating, substrate is carried out successively to the pre-treatment step of surface finish, cleaning, annealing.
The concrete grammar of surface finish is: Si substrate surface diamond mud is carried out polishing, after not having cut, adopts the chemical mechanical polishing method of prior art to carry out polishing to substrate with observation by light microscope substrate surface.
The concrete grammar of cleaning step is: Si substrate is first placed on ultrasonic cleaning in acetone soln, and then is placed on deionized water for ultrasonic cleaning; Then ultrasonic cleaning in isopropyl acetone solution; Then ultrasonic cleaning in a solution of hydrofluoric acid, then soak in deionized water; Again Si substrate is placed in the mixed solution of sulfuric acid and hydrogen peroxide and soaks; Finally Si substrate is put into hydrofluoric acid to soak, with deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
The concrete grammar of annealing is: be placed in the growth room of ultra high vacuum by Si substrate, and at 900-1000 DEG C, toast the pollutant that 3-5h removes surface, then air cooling is to room temperature.After above annealing in process, substrate can be made to 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 DEG C, and vacuum degree is 10
-10more than Torr.
Adopt pulsed laser deposition growth method epitaxial growth AlN film, underlayer temperature is 650-750 DEG C, and chamber pressure is that 10-15mTorr, V/III ratio is 50-60, the speed of growth is 0.4-0.6 ML/s.
Molecular beam epitaxial growth method is adopted to combine with pulsed laser deposition growth method, first utilize molecular beam epitaxial growth Al resilient coating, recycling pulsed laser deposition epitaxial growth method growing AIN film, epitaxially grown efficiency can be improved, according to the characteristic optimum selecting epitaxy method of base material, be conducive to the raising of the quality of epitaxial loayer.In addition, lattice mismatch between AlN film and Si substrate is up to 19%, thermal coefficient of expansion difference 44%, the also problem such as Presence of an interface diffusion, cause the AlN film crystal directly grown on a si substrate second-rate, defect concentration is high, thus reduce the luminous efficiency of AlN thin film based device, be difficult to the requirement reaching photoelectric device.And by reducing growth temperature, effectively inhibit the hot conditions (generally all more than 1000 DEG C) of conventional metals organic chemical vapor deposition technique (MOCVD) growing nitride to the amplification of substrate and AlN lattice mismatch and coefficient of thermal expansion mismatch degree, nitride film defect is reduced, improves the quality of AlN film.In addition, the factor such as technological parameter and oxygen content all can affect the quality of the AlN crystal of acquisition, and when oxygen content is higher, oxygen very easily and reactive aluminum, generates oxide and enters in the lattice structure of AlN film and form defect, thus reduce the luminous efficiency of AlN base device.In order to reduce the impact of oxygen on membrane structure, taking above-mentioned technological parameter, controlling that vacuum degree, reative cell are pressed, evacuation time etc., high-quality AlN film can be obtained.
Preferably, the thickness of Al resilient coating is 3-5nm.Can be detected by RHEED, control the growing state of this layer.
Growth of the present invention AlN film on a si substrate can be applied in photodetector, LED component.
Compared with prior art, the invention has the beneficial effects as follows:
1, use Si to be substrate, adopt pulsed laser deposition growth method at Si(111 simultaneously) growing AIN film on crystal face, AlN crystal preferred orientation grows, and obtains lattice mismatch very low between substrate and AlN, drastically increases the quality of AlN crystal.
2, have employed pulsed laser deposition growth method growing AIN film, both for low-temperature epitaxy AlN provides basis, effectively can shorten again the nucleated time of nitride, and ensure the unicity of the AlN film obtained.
3, molecular beam epitaxial growth method is adopted to combine with pulsed laser deposition epitaxial growth method, molecular beam epitaxy technique is first utilized to grow Al resilient coating, recycling pulsed laser deposition epitaxy technology growing AIN film, improve epitaxially grown efficiency, according to the characteristic optimum selecting epitaxy method of base material, be conducive to the raising of epitaxial layer quality.Simultaneously, by reducing growth temperature, effectively inhibit the hot conditions (generally all at more than 1000oC) of conventional metals organic chemical vapor deposition technique (MOCVD) growing nitride to substrate and the lattice mismatch of AlN and the amplification of coefficient of thermal expansion mismatch degree, nitride film defect is reduced.
4, Si is as substrate, easily obtains, low price, and have employed low temperature growth techniques, is conducive to reducing production cost.
In sum, preparation technology of the present invention is unique and easy, and production cost is low, and the AlN thin film defectiveness density of acquisition is low, crystal mass is high, the advantage of electricity and optical property excellence.
Accompanying drawing explanation
Fig. 1 is the structural representation of growth of the present invention AlN film on a si substrate;
Fig. 2 is the X ray Surface scan collection of illustrative plates of growth of the present invention AlN film on a si substrate;
Fig. 3 is (002) face X ray swing curve figure of growth of the present invention AlN film on a si substrate;
Fig. 4 is the GIXR collection of illustrative plates of growth of the present invention AlN film on a si substrate;
Fig. 5 is the schematic diagram that growth of the present invention AlN film is on a si substrate applied in LED component;
Fig. 6 is the schematic diagram that growth of the present invention AlN film is on a si substrate applied in 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, growth of the present invention AlN film on a si substrate comprise Si substrate layer 11, the AlN thin layer 12 grown on Si substrate layer 11.Described AlN thin layer 12 is monocrystal thin films layer or polycrystal film layer.
This growth AlN film is on a si substrate adopted and is obtained with the following method:
(1) selection in substrate and crystal orientation: choose Si substrate, chooses (111) crystal face of Si substrate simultaneously.
(2) adopt molecular beam epitaxial growth method, grow Al resilient coating on a si substrate, process conditions are:
Underlayer temperature is 500-600 DEG C, and vacuum degree is 10
-10more than Torr, the speed of growth is 0.6nm/min, and growth Al buffer layer thickness is 3-5nm, is detected, controls growing state by RHEED.
(3) plasma passing into nitrogen carries out nitrogenize to Al resilient coating.
(4) adopt pulsed laser deposition growth method growing AIN film, process conditions are: underlayer temperature is
650-750 DEG C, chamber pressure is that 10-15mTorr, V/III ratio is 50-60, the speed of growth is 0.4-0.6 ML/s.Specifically: with the KrF excimer laser (λ=248nm of ability to be 2.0-3.0 J/cm2 and repetition rate be 20-25Hz, t=20ns) PLD ablation AlN target, when depositing Al N thin film, growth room internal pressure N2 remains on 10-15mTorr, ensures to obtain high-quality AlN film.
(5) be incubated 25-35 minute, temperature is 650-750 DEG C.
Embodiment 2
The present embodiment carries out changing one's profession on the basis of embodiment 1, and difference is: before growing AIN resilient coating, and substrate is carried out successively to the pre-treatment step of surface finish, cleaning, annealing, concrete grammar is as follows:
Surface finish process: Si substrate surface diamond mud is carried out polishing, after not having cut, then adopts the cmp method of prior art to carry out polishing to substrate with observation by light microscope substrate surface.
Cleaning: the draw-in groove that Si sheet is housed is put into clean square cup, adds deionized water and the acetone that prepared until solution complete submergence Si sheet, 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; IPA solution is injected, ultrasonic 5-10 minute in square cup; Square cup is put into ultrasonic tank, and add IPA 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 IPA solution cleaning 2-3 time; In square cup, add deionized water, until submergence Si sheet, 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 sheet; With the clip of polytetrafluoroethylene by the Si sheet side of standing on cup, Si sheet 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 sheet and put into dioxysulfate water 5-7 minute from hydrofluoric acid; Again Si sheet 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: 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 3-5 h is to remove the pollutant of 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, 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 °, and calculate known thus, its defect concentration is lower than 2 × 10
8cm
-2, show the high-quality AlN film having gone out fabricating low-defect-density at Si (111) face Epitaxial growth.
Please refer to Fig. 4, X ray glancing incidence (GIXR) test shows that the heterogeneous joint of AlN/Si is atom level sudden change, for growing high-quality AlN film is given security.
In sum, no matter be in defect concentration, or in crystalline quality, adopt the molecular beam epitaxial growth method AlN film obtained on a si substrate that combines with 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.
The embodiment 3 growth of the present invention application of AlN film in LED component on a si substrate
Please refer to Fig. 5, AlN film embodiment 2 obtained is applied to the method in LED component, and it is included in Si (111) crystal face Epitaxial growth high-quality AlN film, after forming AlN film 10, the U-GaN thin layer 11 of growing high-quality successively, N-shaped mixes silicon GaN epitaxial loayer 12, In
xga
1-xn multiple quantum well layer 13, p-type mixes magnesium GaN layer 14, specific as follows:
The U-GaN thin layer 11 of growing high-quality on AlN film 10; On U-GaN thin layer 11, growing n-type mixes silicon GaN epitaxial layer 12 again, 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 13, thickness is about 112 nm, and periodicity is 7, wherein In
xga
1-xn well layer is 3 nm, and barrier layer is 13 nm, 0 < x < 1.The p-type that regrowth Mg adulterates afterwards mixes magnesium GaN layer 14, and thickness is about 350 nm, 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 14.
The embodiment 4 growth of the present invention application of AlN film in photodetector on a si substrate
Please refer to Fig. 6, AlN film embodiment 2 obtained is applied to the method for photodetector, comprising Si (111) crystal face Epitaxial growth high-quality AlN film, after forming AlN film 20, the U-GaN thin layer 21 of growing high-quality successively, N-shaped mixes silicon GaN epitaxial loayer 22, undoped GaN layer 23, and p-type mixes magnesium GaN layer 24.
AlN film 20 grows U-GaN thin layer 21, and its thickness is about 300nm; On U-GaN thin layer 21, growing n-type mixes silicon GaN epitaxial layer 22, and its thickness is about 3 μm, and the concentration of its charge carrier is 1 × 10
19cm
-3.Then grow undoped GaN epitaxial loayer 23, thickness is about 200 nm, and its carrier concentration is 2. 2 × 10
16cm
-3.The p-type that regrowth Mg adulterates afterwards mixes magnesium GaN layer 24, and thickness is about 1. 5 μm.Last electron beam evaporation forms ohmic contact and schottky junction.Pass through at N on this basis
2anneal under atmosphere, improve carrier concentration and mobility that p-type mixes magnesium GaN layer 24.The GaN UV photodetector of prepared p-i-n structure is under 1 V bias voltage, and dark current is only 65 pA, and device is under 1 V bias voltage, reaches 0. 92 A/W in the maximum of 361 nm place responsivenesses.
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 (7)
1. the preparation method of growth AlN film on a si substrate, it is characterized in that: adopt Si substrate, (111) crystal face selecting Si substrate is crystal orientation, first on Si (111) crystal face, adopt molecular beam epitaxy accretion method to grow the thick Al resilient coating of 3-5nm, then adopt pulsed laser deposition growth method epitaxial growth AlN film; Described molecular beam epitaxy accretion method response parameter is: substrate temperature is 500-600 DEG C, and vacuum degree is 10
-10more than Torr; Described pulsed laser deposition growth method response parameter: underlayer temperature is 650-750 DEG C, chamber pressure is that 10-15mTorr, V/III ratio is 50-60, the speed of growth is 0.4-0.6 ML/s.
2. the preparation method of growth as claimed in claim 1 AlN film on a si substrate, is characterized in that: before growth Al resilient coating, substrate is carried out successively to the pre-treatment step of surface finish, cleaning, annealing.
3. the preparation method of growth as claimed in claim 2 AlN film on a si substrate, it is characterized in that, the concrete grammar of cleaning step is: Si substrate is first placed on ultrasonic cleaning in acetone soln, and then is placed on deionized water for ultrasonic cleaning; Then ultrasonic cleaning in aqueous isopropanol; Then ultrasonic cleaning in a solution of hydrofluoric acid, then soak in deionized water; Again Si substrate is placed in the mixed solution of sulfuric acid and hydrogen peroxide and soaks; Finally Si substrate is put into hydrofluoric acid to soak, with deionized water rinsing, nitrogen dries up, and puts into nitrogen cabinet.
4. the preparation method of growth as claimed in claim 2 AlN film on a si substrate, it is characterized in that, the concrete grammar of surface finish is: Si substrate surface diamond mud is carried out polishing, after not having cut with observation by light microscope substrate surface, the chemical mechanical polishing method of prior art is adopted to carry out polishing to substrate.
5. the preparation method of growth as claimed in claim 2 AlN film on a si substrate, it is characterized in that, the concrete grammar of annealing is: be placed in the growth room of ultra high vacuum by Si substrate, and at 900-1000 DEG C, toast the pollutant that 3-5h removes surface, then air cooling is to room temperature.
6. a growth AlN film on a si substrate, is characterized in that: adopt the preparation method described in claim 1 to 5 any one to obtain.
7. growth according to claim 6 AlN film is on a si substrate preparing the application in photodetector, LED component.
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Cited By (1)
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| CN109599324A (en) * | 2018-11-22 | 2019-04-09 | 合肥彩虹蓝光科技有限公司 | A kind of aluminum nitride epitaxial layer growing method |
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| 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 |
| 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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| CN106244984B (en) * | 2016-08-04 | 2018-08-31 | 电子科技大学 | Enhanced AlN films of a kind of a axis orientation and preparation method thereof |
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| CN111101204A (en) * | 2019-12-12 | 2020-05-05 | 华南师范大学 | Single crystal AlN film and preparation method and application thereof |
| CN111334781A (en) * | 2020-04-20 | 2020-06-26 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Large-size composite seed crystal for aluminum nitride crystal growth and preparation method thereof |
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| CN112599646B (en) * | 2020-12-25 | 2022-12-16 | 惠州学院 | Full-spectrum photoelectric dual-channel device and preparation method and application thereof |
| CN113178498A (en) * | 2021-04-29 | 2021-07-27 | 中国科学院长春光学精密机械与物理研究所 | Deep ultraviolet detector and preparation method thereof |
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Denomination of invention: An AlN Thin Film Grown on Si Substrate and Its Preparation Method and Application Effective date of registration: 20220926 Granted publication date: 20150304 Pledgee: Agricultural Bank of China Co.,Ltd. Heyuan Yuancheng District Sub branch Pledgor: Guangzhou Everbright Technology Co.,Ltd. Registration number: Y2022980016273 |
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