CN108950477A - A kind of aluminium nitride film and its preparation method and application - Google Patents

A kind of aluminium nitride film and its preparation method and application Download PDF

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Publication number
CN108950477A
CN108950477A CN201810744218.6A CN201810744218A CN108950477A CN 108950477 A CN108950477 A CN 108950477A CN 201810744218 A CN201810744218 A CN 201810744218A CN 108950477 A CN108950477 A CN 108950477A
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aln layer
aln
preparation
layer
aluminium nitride
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黄小辉
徐孝灵
郑远志
陈向东
康建
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EPITOP PHOTOELECTRIC TECHNOLOGY Co Ltd
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EPITOP PHOTOELECTRIC TECHNOLOGY Co Ltd
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/12—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer

Abstract

The present invention provides a kind of aluminium nitride film and its preparation method and application, and preparation method includes following steps in sequence: 1) the first aln layer with a thickness of 5~300nm is sputtered on substrate layer；2) reaction chamber temperature for controlling growth apparatus is 1400~1700 DEG C, carries out the high temperature anneal to first aln layer, obtains the first rearrangement aln layer；Wherein, when a length of 5~200min of the high temperature anneal；3) temperature for controlling the reaction chamber is down to 1100~1350 DEG C, is passed through trimethyl aluminium and ammonia, resets the second aln layer generated on aln layer with a thickness of 500~5000nm described first；The collection of the first rearrangement aln layer and second aln layer is combined into the aluminium nitride film.This method can improve AlN film crystal quality and AlN film surface crackle, to be conducive to be promoted the performance of AlN device.

Description

A kind of aluminium nitride film and its preparation method and application
Technical field
The present invention relates to a kind of aluminium nitride films of skill and its preparation method and application, belong to LED technology field.
Background technique
Aluminium nitride (AlN) belongs to third generation semiconductor material with wide forbidden band, has forbidden bandwidth high, breakdown electric field is high, thermal conductivity The advantages that rate is high, and electron saturation velocities are high and capability of resistance to radiation is high.AlN crystal has stable hexagonal wurtzite structure, brilliant Lattice constantAlN has maximum direct band gap in iii-v not semiconductor material, about 6.2eV is important blue light and ultra-violet light-emitting material.Its thermal conductivity is high, and resistivity is high, and breakdown field is powerful, and dielectric coefficient is small, is Excellent high-temperature high-frequency and high power device electronic material.Also, the AlN being orientated along c-axis has extraordinary piezoelectric property It is propagated with surface acoustic wave high speed, it is excellent SAW device piezoelectric material.AlN crystal and gallium nitride have very Close lattice constant and thermal expansion coefficient is the preferred substrate material of epitaxial growth AlGaN photoelectric device.
Based on the characteristic that AlN or more is excellent, AlN is widely used in ultraviolet detector, high electron mobility transistor (HEMT), UV LED (LED).
Although AlN has the advantages that many, AlN material is but very difficult to prepare.Preparation AlN needs high temperature and pressure to set It is standby, and accurately source stream amount control system.Currently, commercial gas phase depositing Al N uses the depositing device of high temperature, the AlN of preparation Crystal quality is not good enough, and since AlN lattice constant and Sapphire Substrate lattice constant difference are larger, has biggish lattice Mismatch is very easy to cracked so as to cause the surface AlN.Simultaneously because migration rate of the Al atom on surface is lower, AlN It is merged into that complete film crystal is extremely difficult, so the AlN thin-film material of high quality flawless is difficult to obtain, therefore AlN material The application of material receives very big limitation.
Summary of the invention
In view of the foregoing drawbacks, the present invention provides a kind of aluminium nitride film and its preparation method and application, this method can be mentioned High AlN film crystal quality, and can be reduced AlN film surface crackle, can obtain low-dislocation-density, high lattice quality and without splitting The AlN thin-film material of line, to be conducive to be promoted the performance of AlN device.
The present invention provides a kind of preparation method of aluminium nitride film, including following steps in sequence:
1) the first aln layer with a thickness of 5~300nm is sputtered on substrate layer；
2) reaction chamber temperature for controlling growth apparatus is 1400~1700 DEG C, carries out high temperature to first aln layer and moves back Fire processing, obtains the first rearrangement aln layer；Wherein, the high temperature anneal when it is 5~200 minutes a length of；
3) temperature for controlling the reaction chamber is down to 1100~1350 DEG C, trimethyl aluminium and ammonia is passed through, described first Reset the second aln layer generated on aln layer with a thickness of 500~5000nm；
The collection of the first rearrangement aln layer and second aln layer is combined into the aluminium nitride film.
The preparation method of aluminium nitride film as described above, wherein the power of the sputtering is 1~10KW, the sputtering Time is 10s~20min.
The preparation method of aluminium nitride film as described above, wherein oxygen and nitrogen are passed through in step 1)；
The flow of the oxygen is 1~10mL/min, and the flow of the nitrogen is 100~300mL/min.
The preparation method of aluminium nitride film as described above, wherein the annealing atmosphere of the high temperature anneal is nitrogen.
The preparation method of aluminium nitride film as described above, wherein in step 3), the pressure for controlling the reaction chamber is 20~ 100mbar。
The preparation method of aluminium nitride film as described above, wherein in step 3), control the growth of second aln layer Speed is 0.5~3 μm/h, and growth time is 10~180min.
The preparation method of aluminium nitride film as described above, wherein in step 3), the molar flow of the ammonia and trimethyl aluminium Amount is than being (10~2000): 1.
The preparation method of aluminium nitride film as described above, wherein the growth apparatus is heavy selected from Metallo-Organic Chemical Vapor One of product equipment, molecular beam epitaxial device or hydride gas-phase epitaxy equipment.
The present invention also provides a kind of aluminium nitride films, obtain according to any of the above-described preparation method.
The present invention also provides a kind of light emitting diodes, including aluminium nitride film as described above.
Implementation of the invention, at least has the advantage that
1, the growing method of aluminium nitride film of the invention passes through the first aln layer with certain temperature to sputtering generation The high temperature anneal for carrying out certain time length, it is flat to generate surface to change the unformed spread pattern of the first aln layer Whole first resets aln layer, and then certain basis is established in the improvement for the quality and roughness of aluminium nitride film；
2, the quality for the first rearrangement aln layer that the present invention is generated by the high temperature anneal is greatly improved, from And good substrate is provided for the growth of the second aln layer, and then can effectively promote the quality of aluminium nitride film；
3, its arrangement mode regularization that the present invention is by the high temperature anneal to the first aln layer, to increase Reduction aluminium nitride film face crack generation；
4, method of the invention is simple and easy, and the AlN film that can be obtained high quality flawless is assisted without large scale equipment；
5, the AlN film generated through the invention not only flawless, and there is high crystal quality, therefore the present invention can Greatly improve the performance of device on AlN film, such as luminous efficiency height, work longevity can be obtained on the basis of the AlN film Order long light emitting diode.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is this hair Bright some embodiments for those of ordinary skill in the art without any creative labor, can be with It obtains other drawings based on these drawings.
Fig. 1 is the flow chart of the preparation method of aluminium nitride film of the present invention；
Fig. 2 is the schematic diagram of the first aln layer of the invention；
Fig. 3 is the schematic diagram that the present invention first resets aln layer.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Fig. 1 is the flow chart of the preparation method of aluminium nitride film of the present invention, as shown in Figure 1, the present invention provides a kind of aluminium nitride The preparation method of film, including following steps in sequence:
S101: the first aln layer with a thickness of 5~300nm is sputtered on substrate layer.
Fig. 2 is the schematic diagram of the first aln layer of the invention.
As shown in Fig. 2, can use sputtering technology in S101 and sputter the first aln layer 2 on substrate layer 1.
It is understood that being unformed, rambling nitridation by the first aln layer 2 that sputtering technology generates Aluminium molecule the stacked state, therefore the surface roughness of first aln layer 2 is higher, quality is very poor.
The high temperature anneal is carried out to it make to reset for the ease of subsequent, the parameter of control sputtering technology can be passed through Make the first aln layer 2 with a thickness of 5~300nm, in concrete operations, can control sputtering equipment sputtering power be 1~ 10KW, the time for controlling sputtering is 10s~20min.
By adjusting sputtering power and sputtering time within the above range, to obtain with a thickness of the first of 5~300nm Aln layer.
In addition, also needing to be passed through working gas into sputtering equipment when carrying out sputtering technology, wherein working gas is oxygen Gas and nitrogen, and the flow of oxygen is 1~10mL/min, the flow of nitrogen is 100~300mL/min.
S102: the reaction chamber temperature for controlling growth apparatus is 1400~1700 DEG C, carries out high temperature to the first aln layer and moves back Fire processing, obtains the first rearrangement aln layer；Wherein, when a length of 5~200min of the high temperature anneal.
Fig. 3 is the schematic diagram that the present invention first resets aln layer.
As shown in figure 3, in S102, after the reaction chamber temperature for adjusting growth apparatus is 1400~1700 DEG C, by the first nitrogen Change aluminium layer 2, which is put into reaction chamber, carries out the high temperature anneal, and the duration of the high temperature anneal continues 5~200min.High temperature The first aln layer 2 after annealing can be reset, by the rambling aluminium nitride molecule stacking of the first aln layer 2 Status re-arrangement is the aluminum nitride crystal of regular hexagonal closs packing arrangement, i.e. the first aln layer 2 is rearranged to the first rearrangement aluminium nitride Layer 3.
First rearrangement aln layer 3 is significantly improved relative to the quality of the first aln layer 2, dislocation density drop It is low, while the surfacing of the first rearrangement aln layer 3, roughness significantly reduce.
By the comparison between Fig. 2 and Fig. 3, we can clearly be had found, the present invention is by existing to the first aln layer 2 The high temperature anneal that the first duration is carried out under certain temperature can be such that the first aln layer 2 resets, and it is brilliant to generate aluminium nitride Body queueing discipline, surfacing and roughness it is low first reset aln layer 3.
In addition, the present invention uses and is passed through nitrogen into reaction chamber as annealing atmosphere when carrying out the high temperature anneal, and And the flow for controlling nitrogen is 1~100L/min.
S103: the temperature for controlling reaction chamber is down to 1100~1350 DEG C, is passed through trimethyl aluminium and ammonia, resets nitrogen first Change the second aln layer generated on aluminium layer with a thickness of 500~5000nm.
The collection of first rearrangement aln layer and the second aln layer is combined into aluminium nitride film.
After the high temperature anneal, the temperature of reaction chamber can be reduced to 1100~1350 DEG C, then to reaction chamber In be passed through trimethyl aluminium and ammonia, by controlling the flow of trimethyl aluminium and ammonia, first reset grown on aln layer 3 it is thick Degree is the second aln layer of 500~5000nm.
In S103, the pressure of reaction chamber is 20~100mbar, and the molar flow of ammonia and trimethyl aluminium ratio is (10 ~2000): 1.
It is worth noting that, when generating the second aln layer, in addition to temperature, pressure and the ammonia and three to reaction chamber Outside the volume ratio of aluminium methyl is controlled, it is also necessary to the speed of growth of the second aln layer is controlled, specifically, control the The speed of growth of nitride aluminium layer is 0.5~3 μm/h.If the speed of growth is too small, crystal is difficult to form；The speed of growth is too fast, Crystal quality can be poor.
In addition, the growth time of the second aln layer of control is 10~180min
Due to the second aln layer be grown in high quality, surfacing first reset aln layer 3 on, the first weight It arranges aln layer 3 and provides good substrate for the second aln layer, thus the second aln layer generated on this basis Crystal quality can greatly promote, therefore can be effectively reduced a possibility that aluminium nitride film is cracked.
After the growth of the second aln layer, the set of the first rearrangement aln layer 3 and the second aln layer is this Invent the aluminium nitride film for the high quality flawless being prepared.
Further, growth apparatus of the invention is selected from equipment of metal organic chemical vapor deposition, molecular beam epitaxial device Or one of hydride gas-phase epitaxy equipment.
Further, substrate layer of the invention is selected from one of sapphire, silicon, silicon carbide and glass.
The present invention by the above method can prepare butterfly flawless and it is flawless have certain thickness aluminium nitride Film.
By successively growing n-type doping layer, Quantum Well in flawless prepared by the present invention and flawless aluminium nitride film Luminescent layer and p-type doped layer can obtain the epitaxial structure with aluminium nitride film of the present invention.Since the smooth nothing of aluminium nitride film is split Line and crystal quality is higher, thus the epitaxial structure and LED obtained on the basis of the present invention have good light emission luminance with And longer working life.
Hereinafter, being described in detail by preparation method of several specific embodiments to aluminium nitride film of the invention.
Embodiment 1
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 2 inches sapphire substrates are put into AlN sputtering equipment, sputtering power are controlled in 3KW, oxygen flux control exists 2mL/min, nitrogen flow 180mL/min, sputtering time are 1 minute.Obtain the first aln layer with a thickness of 30nm；
2) the first aln layer of 30nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) reaction Room carries out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1400 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 20 liters/min, and the first aln layer is put into reaction chamber and the residence time is 10 minutes, the first aln layer It is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1150 DEG C, chamber pressure is controlled in 50mbar, is subsequently passed 500mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 2.5 μm/h, and growth time is 60 minutes, is generated thick Degree is the second aln layer of 2500nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 80arcsec, the half-breadth in (102) direction is 400arcsec.
Embodiment 2
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 4 inches sapphire substrates are put into AlN sputtering equipment, sputtering power are controlled in 6KW, oxygen flux control exists 2mL/min, nitrogen flow 160mL/min, sputtering time are 1 minute.Obtain the first aln layer with a thickness of 50nm；
2) the first aln layer of 50nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) reaction Room carries out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1400 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 20 liters/min, and the first aln layer is put into reaction chamber and the residence time is 20 minutes, the first aln layer It is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1250 DEG C, chamber pressure is controlled in 20mbar, is subsequently passed 400ml/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 2.5 μm/h, and growth time is 120 minutes, is generated With a thickness of the second aln layer of 5000nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 60arcsec, the half-breadth in (102) direction is 180arcsec.
Embodiment 3
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 2 inches of silicon substrates are put into AlN sputtering equipment, sputtering power are controlled in 4KW, oxygen flux control is in 4mL/ Min, nitrogen flow 200mL/min, sputtering time are 2 minutes.Obtain the first aln layer with a thickness of 100nm；
2) the first aln layer of 100nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) instead Room is answered to carry out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1450 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 20 liters/min, and the first aln layer is put into reaction chamber and the residence time is 40 minutes, the first aln layer It is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1200 DEG C, chamber pressure is controlled in 80mbar, is subsequently passed 400mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 1.8 μm/h, and growth time is 90 minutes, is generated thick Degree is the second aln layer of 2700nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 60arcsec, the half-breadth in (102) direction is 350arcsec.
Embodiment 4
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 4 inches of silicon substrates are put into AlN sputtering equipment, sputtering power are controlled in 10KW, oxygen flux control exists 4mL/min, nitrogen flow 190mL/min, sputtering time are 3 minutes.Obtain the first aln layer with a thickness of 300nm；
2) the first aln layer of 300nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) instead Room is answered to carry out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1600 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 20 liters/min, and the first aln layer is put into reaction chamber and the residence time is 200 minutes, the first aluminium nitride Layer is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1100 DEG C, chamber pressure is controlled in 50mbar, is subsequently passed 600mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 3.0 μm/h, and growth time is 90 minutes, is generated thick Degree is the second aln layer of 4500nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 50arcsec, the half-breadth in (102) direction is 300arcsec.
Hereinafter, being carried out by several specific embodiments to the preparation for carrying out LED using aluminium nitride film of the invention detailed It introduces.
Embodiment 5
The preparation method of the LED of the present embodiment includes following steps in sequence:
1) 4 inches sapphire substrates are put into AlN sputtering equipment, sputtering power are controlled in 5KW, oxygen flux control exists 4mL/min, nitrogen flow 180mL/min, sputtering time are 3 minutes.Obtain the first aln layer with a thickness of 200nm；
2) the first aln layer of 200nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) instead Room is answered to carry out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1700 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 40 liters/min, and the first aln layer is put into reaction chamber and the residence time is 120 minutes, the first aluminium nitride Layer is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1350 DEG C, chamber pressure is controlled in 100mbar, is subsequently passed The trimethyl aluminium of 600mL/min and the NH of 10000mL/min3, Controlling Growth Rate is 2.0 μm/h, and growth time is 90 minutes, Generate the second aln layer with a thickness of 3000nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 50arcsec, the half-breadth in (102) direction is 300arcsec.
4) temperature when control reaction is 1250 DEG C, is passed through hydrogen, trimethyl gallium (100ml/min), trimethyl aluminium (300ml/min) and NH390 minutes, pressure kept 50mtorr, and the N-type that a layer thickness is 1500nm is grown on aluminium nitride film AlGaN layer, Al content 70%, the doping concentration of N-type GaN are 1 × 1019cm-3；
5) temperature when control reaction is 1000 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (20ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN quantum and build and mix Si impurity, doping concentration is 1 × 1018cm-3；
Wherein, growth time is 2 minutes, with a thickness of 12nm, Al content 60%；
6) temperature when control reaction is 1000 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (15ml/min), Trimethyl aluminium (40ml/min) and NH3, grow AlGaN Quantum Well and this layer do not mix Si.
Wherein, growth time is 0.5 minute, with a thickness of 2.5nm, Al content 40%；
Repeat step 5) and recycled for totally 6 to step 6), forms the quantum well structure in 6 periods；
7) temperature when control reaction is 1150 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (17ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN electronic barrier layer, Al content 75%；
8) p-type GaN is grown on the basis of electronic barrier layer.Reaction chamber temperature is reduced to 950 DEG C, pressure is adjusted to 200torr is passed through hydrogen, trimethyl gallium (40ml/min), two luxuriant magnesium (150ml/min), NH3, p-type GaN layer is generated, Mg's mixes Miscellaneous concentration is 5.5 × 1019cm-3；
Wherein, growth time is 55 minutes, with a thickness of 320nm.
So far, the growth of the LED of the present embodiment is completed.
The LED of the present embodiment is tested as follows:
1, this LED is fabricated to 350 μ m, 350 μm of chips, is passed through the electric current of 20mA, ultra-violet light-emitting wavelength is 265nm, work Making voltage is 6.0V, light emission luminance 5mW；
2, this LED component service life is 10,000 hours.
Embodiment 6
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 2 inches of silicon substrates are put into AlN sputtering equipment, sputtering power are controlled in 6KW, oxygen flux control is in 1mL/ Min, nitrogen flow 160mL/min, sputtering time are 1 minute.Obtain the first aln layer with a thickness of 25nm；
2) the first aln layer of 25nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) reaction Room carries out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1500 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 40 liters/min, and the first aln layer is put into reaction chamber and the residence time is 200 minutes, the first aluminium nitride Layer is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1280 DEG C, chamber pressure is controlled in 60mbar, is subsequently passed 800mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 2.5 μm/h, and growth time is 60 minutes, is generated thick Degree is the second aln layer of 2500nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 50arcsec, the half-breadth in (102) direction is 150arcsec.
4) temperature when control reaction is 1220 DEG C, is passed through hydrogen, trimethyl gallium (80ml/min), trimethyl aluminium (300ml/min) and NH3120 minutes, pressure kept 50mtorr, and the N that a layer thickness is 2000nm is grown on aluminium nitride film Type AlGaN layer, Al content 72%, the doping concentration of N-type GaN are 1 × 1019cm-3；
5) temperature when control reaction is 1050 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (20ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN quantum and build and mix Si impurity, doping concentration is 1 × 1018cm-3；
Wherein, growth time is 2 minutes, with a thickness of 12nm, Al content 65%；
6) temperature when control reaction is 1050 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (25ml/min), Trimethyl aluminium (40ml/min) and NH3, grow AlGaN Quantum Well and this layer do not mix Si.
Wherein, growth time is 0.5 minute, with a thickness of 3nm, Al content 35%；
Repeat step 5) and recycled for totally 7 to step 6), forms the quantum well structure in 7 periods；
7) temperature when control reaction is 1050 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (17ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN electronic barrier layer, Al content 60%；
8) p-type GaN is grown on the basis of electronic barrier layer.Reaction chamber temperature is reduced to 900 DEG C, pressure is adjusted to 200torr is passed through hydrogen, trimethyl gallium (40ml/min), two luxuriant magnesium (150ml/min), NH3, p-type GaN layer is generated, Mg's mixes Miscellaneous concentration is 2 × 1019cm-3；
Wherein, growth time is 25 minutes, with a thickness of 150nm.
So far, the growth of the LED of the present embodiment is completed.
The LED of the present embodiment is tested as follows:
1, this LED is fabricated to 350 μ m, 350 μm of chips, is passed through the electric current of 20mA, ultra-violet light-emitting wavelength is 280nm, work Making voltage is 6.0V, light emission luminance 4mW；
2, this LED component service life is 10,000 hours.
Embodiment 7
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 2 inches of silicon substrates are put into AlN sputtering equipment, sputtering power are controlled in 8KW, oxygen flux control is in 1mL/ Min, nitrogen flow 160mL/min, sputtering time are 1 minute.Obtain the first aln layer with a thickness of 30nm；
2) the first aln layer of 30nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) reaction Room carries out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1550 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 40 liters/min, and the first aln layer is put into reaction chamber and the residence time is 50 minutes, the first aln layer It is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1220 DEG C, chamber pressure is controlled in 20mbar, is subsequently passed 800mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 3.0 μm/h, and growth time is 60 minutes, is generated thick Degree is the second aln layer of 3000nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 50arcsec, the half-breadth in (102) direction is 250arcsec.
4) temperature when control reaction is 1180 DEG C, is passed through hydrogen, trimethyl gallium (80ml/min), trimethyl aluminium (300ml/min) and NH3120 minutes, pressure kept 50mtorr, and the N that a layer thickness is 2000nm is grown on aluminium nitride film Type AlGaN layer, Al content 70%, the doping concentration of N-type GaN are 1 × 1019cm-3；
5) temperature when control reaction is 1000 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (20ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN quantum and build and mix Si impurity, doping concentration is 1 × 1018cm-3；
Wherein, growth time is 2 minutes, with a thickness of 12nm, Al content 55%；
6) temperature when control reaction is 1000 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (25ml/min), Trimethyl aluminium (40ml/min) and NH3, grow AlGaN Quantum Well and this layer do not mix Si.
Wherein, growth time is 0.5 minute, with a thickness of 3nm, Al content 28%；
Repeat step 5) and recycled for totally 12 to step 6), forms the quantum well structure in 12 periods；
7) temperature when control reaction is 1000 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (17ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN electronic barrier layer, Al content 50%；
8) p-type GaN is grown on the basis of electronic barrier layer.Reaction chamber temperature is reduced to 930 DEG C, pressure is adjusted to 200torr is passed through hydrogen, trimethyl gallium (40ml/min), two luxuriant magnesium (150ml/min), NH3, p-type GaN layer is generated, Mg's mixes Miscellaneous concentration is 2 × 1019cm-3；
Wherein, growth time is 50 minutes, with a thickness of 300nm.
So far, the growth of the LED of the present embodiment is completed.
The LED of the present embodiment is tested as follows:
1, this LED is fabricated to 350 μ m, 350 μm of chips, is passed through the electric current of 20mA, ultra-violet light-emitting wavelength is 295nm, work Making voltage is 6.0V, light emission luminance 4.5mW；
2, this LED component service life is 10,000 hours.
Embodiment 8
The preparation method of the aluminium nitride film of the present embodiment includes following steps in sequence:
1) 4 inch silicon carbide silicon substrates are put into AlN sputtering equipment, sputtering power are controlled in 8KW, oxygen flux control exists 1mL/min, nitrogen flow 240mL/min, sputtering time are 1 minute.Obtain the first aln layer with a thickness of 50nm；
2) the first aln layer of 50nm obtained in step 1) is put into Metallo-Organic Chemical Vapor deposition (MOCVD) reaction Room carries out the high temperature anneal.
Specifically, MOCVD reaction chamber temperature is increased to 1520 DEG C, is passed through nitrogen as high annealing atmosphere and control nitrogen The flow of gas is 40 liters/min, and the first aln layer is put into reaction chamber and the residence time is 200 minutes, the first aluminium nitride Layer is rearranged to the first rearrangement aln layer；
3) MOCVD reaction chamber temperature is reduced to 1250 DEG C, chamber pressure is controlled in 20mbar, is subsequently passed 400mL/ The trimethyl aluminium of min and the NH of 10000mL/min3, Controlling Growth Rate is 1.5 μm/h, and growth time is 120 minutes, is generated With a thickness of the second aln layer of 3000nm；
MOCVD reaction chamber is cooled down, (i.e. first resets aln layer and the second aln layer to the AlN film taken out Set).
To above-mentioned acquisition high-crystal quality and the AlN thin-film material without face crack carries out XRD test, wherein (002) side To half-breadth be 80arcsec, the half-breadth in (102) direction is 220arcsec.
4) temperature when control reaction is 1100 DEG C, is passed through hydrogen, trimethyl gallium (100ml/min), trimethyl aluminium (300ml/min) and NH3100 minutes, pressure kept 50mtorr, and the N that a layer thickness is 2000nm is grown on aluminium nitride film Type AlGaN layer, Al content 60%, the doping concentration of N-type GaN are 1 × 1019cm-3；
5) temperature when control reaction is 980 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (20ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN quantum and build and mix Si impurity, doping concentration is 1 × 1018cm-3；
Wherein, growth time is 2 minutes, with a thickness of 14nm, Al content 50%；
6) temperature when control reaction is 980 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (27ml/min), Trimethyl aluminium (40ml/min) and NH3, grow AlGaN Quantum Well and this layer do not mix Si.
Wherein, growth time is 0.5 minute, with a thickness of 3nm, Al content 22%；
Repeat step 5) and recycled for totally 10 to step 6), forms the quantum well structure in 10 periods；
7) temperature when control reaction is 980 DEG C, pressure 50mtorr, is passed through hydrogen, trimethyl gallium (17ml/min), Trimethyl aluminium (60ml/min) and NH3, grow AlGaN electronic barrier layer, Al content 45%；
8) p-type GaN is grown on the basis of electronic barrier layer.Reaction chamber temperature is reduced to 850 DEG C, pressure is adjusted to 200torr is passed through hydrogen, trimethyl gallium (40ml/min), two luxuriant magnesium (150ml/min), NH3, p-type GaN layer is generated, Mg's mixes Miscellaneous concentration is 2 × 1019cm-3；
Wherein, growth time is 50 minutes, with a thickness of 300nm.
So far, the growth of the LED of the present embodiment is completed.
The LED of the present embodiment is tested as follows:
1, this LED is fabricated to 350 μ m, 350 μm of chips, is passed through the electric current of 20mA, ultra-violet light-emitting wavelength is 310nm, work Making voltage is 6.0V, light emission luminance 5mW；
2, this LED component service life is 10,000 hours.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (10)

1. a kind of preparation method of aluminium nitride film, which is characterized in that including following steps in sequence:
1) the first aln layer with a thickness of 5~300nm is sputtered on substrate layer；
2) reaction chamber temperature for controlling growth apparatus is 1400~1700 DEG C, is carried out at high annealing to first aln layer Reason, obtains the first rearrangement aln layer；Wherein, when a length of 5~200min of the high temperature anneal；
3) temperature for controlling the reaction chamber is down to 1100~1350 DEG C, is passed through trimethyl aluminium and ammonia, resets described first The second aln layer with a thickness of 500~5000nm is generated on aln layer；
The collection of the first rearrangement aln layer and second aln layer is combined into the aluminium nitride film.
2. preparation method according to claim 1, which is characterized in that the power of the sputtering is 1~10KW, the sputtering Time be 10s~20min.
3. preparation method according to claim 2, which is characterized in that be passed through oxygen and nitrogen in step 1)；
The flow of the oxygen is 1~10mL/min, and the flow of the nitrogen is 100~300mL/min.
4. preparation method according to claim 3, which is characterized in that the annealing atmosphere of the high temperature anneal is nitrogen Gas.
5. the preparation method according to claim 4, which is characterized in that in step 3), the pressure for controlling the reaction chamber is 20~100mbar.
6. preparation method according to claim 5, which is characterized in that in step 3), control second aln layer The speed of growth is 0.5~3 μm/h, and growth time is 10~180min.
7. preparation method according to claim 6, which is characterized in that in step 3), the ammonia and trimethyl aluminium rub Your flow-rate ratio is (10~2000): 1.
8. -7 any preparation method according to claim 1, which is characterized in that the growth apparatus is selected from Organometallic Learn one of vapor deposition apparatus, molecular beam epitaxial device or hydride gas-phase epitaxy equipment.
9. a kind of aluminium nitride film, which is characterized in that obtained according to any preparation method of claim 1-8.
10. a kind of light emitting diode, which is characterized in that including aluminium nitride film as claimed in claim 9.
CN201810744218.6A 2018-07-09 2018-07-09 A kind of aluminium nitride film and its preparation method and application Pending CN108950477A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109554678A (en) * 2018-12-26 2019-04-02 浙江清华柔性电子技术研究院 Flexible aluminium nitride film and its manufacturing method
CN109873056A (en) * 2019-01-18 2019-06-11 华灿光电（浙江）有限公司 The preparation method of the epitaxial wafer of light emitting diode
CN111146078A (en) * 2019-12-27 2020-05-12 中国电子科技集团公司第十三研究所 Preparation method of AlN thin film
CN111690907A (en) * 2019-03-15 2020-09-22 马鞍山杰生半导体有限公司 Aluminum nitride film and preparation method and application thereof
WO2021138771A1 (en) * 2020-01-06 2021-07-15 奥趋光电技术(杭州)有限公司 Heating device and preparation method for mass preparation of high-quality aluminium nitride templates

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070259534A1 (en) * 2006-05-08 2007-11-08 Tokyo Electron Limited In-situ formation of oxidized aluminum nitride films
CN101343733A (en) * 2008-08-28 2009-01-14 上海蓝光科技有限公司 Method for MOVCD growth nitride epitaxial layer
US20130078454A1 (en) * 2011-09-23 2013-03-28 Applied Materials, Inc. Metal-Aluminum Alloy Films From Metal Amidinate Precursors And Aluminum Precursors
CN105543969A (en) * 2016-01-25 2016-05-04 南通同方半导体有限公司 Growth method for improving quality of AlN thin film crystal
CN106244984A (en) * 2016-08-04 2016-12-21 电子科技大学 A kind of a axle orientational strengthening type AlN thin film and preparation method thereof
CN106367730A (en) * 2015-07-24 2017-02-01 气体产品与化学公司 Methods for depositing group 13 metal or metalloid nitride films

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070259534A1 (en) * 2006-05-08 2007-11-08 Tokyo Electron Limited In-situ formation of oxidized aluminum nitride films
CN101343733A (en) * 2008-08-28 2009-01-14 上海蓝光科技有限公司 Method for MOVCD growth nitride epitaxial layer
US20130078454A1 (en) * 2011-09-23 2013-03-28 Applied Materials, Inc. Metal-Aluminum Alloy Films From Metal Amidinate Precursors And Aluminum Precursors
CN106367730A (en) * 2015-07-24 2017-02-01 气体产品与化学公司 Methods for depositing group 13 metal or metalloid nitride films
CN105543969A (en) * 2016-01-25 2016-05-04 南通同方半导体有限公司 Growth method for improving quality of AlN thin film crystal
CN106244984A (en) * 2016-08-04 2016-12-21 电子科技大学 A kind of a axle orientational strengthening type AlN thin film and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109554678A (en) * 2018-12-26 2019-04-02 浙江清华柔性电子技术研究院 Flexible aluminium nitride film and its manufacturing method
CN109873056A (en) * 2019-01-18 2019-06-11 华灿光电（浙江）有限公司 The preparation method of the epitaxial wafer of light emitting diode
CN109873056B (en) * 2019-01-18 2020-09-29 华灿光电（浙江）有限公司 Preparation method of epitaxial wafer of light-emitting diode
CN111690907A (en) * 2019-03-15 2020-09-22 马鞍山杰生半导体有限公司 Aluminum nitride film and preparation method and application thereof
CN111146078A (en) * 2019-12-27 2020-05-12 中国电子科技集团公司第十三研究所 Preparation method of AlN thin film
WO2021138771A1 (en) * 2020-01-06 2021-07-15 奥趋光电技术(杭州)有限公司 Heating device and preparation method for mass preparation of high-quality aluminium nitride templates

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