CN106244984A - A kind of a axle orientational strengthening type AlN thin film and preparation method thereof - Google Patents
A kind of a axle orientational strengthening type AlN thin film and preparation method thereof Download PDFInfo
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- CN106244984A CN106244984A CN201610633215.6A CN201610633215A CN106244984A CN 106244984 A CN106244984 A CN 106244984A CN 201610633215 A CN201610633215 A CN 201610633215A CN 106244984 A CN106244984 A CN 106244984A
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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
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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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
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Abstract
The invention discloses a kind of a axle orientational strengthening type AlN thin film and preparation method thereof, belong to electronic information function material and device arts.The present invention uses following preparation method: use Si (100) substrate of N-shaped, put it into after magnetic control sputtering system chamber carries out application of vacuum, use different magnetron sputtering technique and combine annealing, first a axle orientation AlN cushion is prepared, preferred orientation growing AIN thin film the most on this basis, owing to the two lattice match is high, thus improve the growth quality of AlN thin film, reduce its surface roughness, and then be conducive to improving the piezoelectric effect of AlN thin film and reducing the propagation loss of surface acoustic wave;In preparation process of the present invention, operation is simple, environmental protection and energy saving, and raw material supply is sufficient and cheap, mass production technique controllable, it is simple to batch production and application, is suitable for making high performance communication components and parts in modern communication technology.
Description
Technical field
The invention belongs to electronic information function material and device arts, be specifically related to a kind of a axle orientational strengthening type AlN
Thin film and preparation method thereof, can be used for the communication unit devices such as the resonator in making modern communication technology, transducer, piezoelectric transducer
Part.
Background technology
The quickly growing of communications industry in recent years, the frequency of communication system and communication apparatus improves day by day, and integrated level is more come
The highest, size reduces day by day, and the wave filter being applied to communication apparatus is had higher requirement by this.And traditional dielectric filter
Body amasss excessive, and LTCC filter filtering performance is relatively poor, and these are all difficult to meet communication apparatus miniaturization, collection
One-tenthization and the requirement of high reliability.
Surface acoustic wave techniques in the late 1860s phase as a kind of emerging electronics, acoustics and materialogy phase
In conjunction with new discipline, start to go on the reason developed rapidly.Because it has, volume is little, lightweight, good stability, reliability
Many-sided advantages such as height, power are little so that SAW device is widely used in radar, electronic warfare, sonar system, channel radio
The fields such as letter, fiber optic communication and radio data system.Particularly at moving communicating field, surface acoustic wave techniques is irreplaceablely
Position has promoted correlational study to advance.
Along with developing rapidly of the third generation wireless communication techniques such as W-CDMA, communication system medium-high frequency section (more than 5GHz) is humorous
The demand of device and wave filter of shaking is increasing.Zinc oxide (ZnO), Lithium metaniobate (LiTaO3) etc. the piezoelectric film material that commonly uses
Acoustic surface wave propagation speed is below 6000m/s, and by contrast, aluminium nitride (AlN) has in all non-ferroelectric substances
Fast acoustic surface wave propagation speed.For the surface acoustic wave crystalline material that acoustic surface wave propagation speed is relatively low, make of it
The SAW device of 2.5GHz, its IDT finger widths d is generally less than 0.4 micron, and it is micro-that finger widths d corresponding for 5GHz should be less than 0.2
Rice, finger widths d corresponding for 10GHz is less than 0.1 micron, approaches the limit of current semi-conductor industry level, causes severed finger serious, and
And, due to intensive interdigital metal finger one-tenth arranged in parallel wiring capacitance, when high frequency, interdigital is easy to conducting, seriously restricts
The further raising of SAW device frequency.Therefore, the material of high acoustic surface wave propagation speed is selected to enable to interdigital
High frequency, powerful requirement is reached when finger beam is wider.
Aluminium nitride (AlN) is III-V group compound, typically exists with the wurtzite structure in hexagonal crystal system.Aluminium nitride film
There is many excellent properties, for example, high pyroconductivity, excellent chemical stability and low toxic, good optical
Can, it has direct band gap broad stopband structure after deliberation, and energy gap is 6.2eV, and highly oriented aluminium nitride film is gathered around especially
Have the plurality of advantages such as high-insulativity, low thermal coefficient of expansion, high dielectric breakdown strength, excellent mechanical strength so that it is machinery,
The fields such as microelectronics, optics and electronic devices and components, the manufacture of SAW device, high-frequency wideband communication and power semiconductor
Have broad application prospects.Wherein aluminium nitride film becomes because of high acoustic wave propagation velocity and big piezoelectric coupling coefficient
Preferably piezoelectric, is particularly suitable for making SAW device (SAW) and bulk wave (BAW) device of 5 GHz band.
Owing to the degree of crystallinity of aluminium nitride film, crystalline quality are to the resistivity of material, leakage current, surface roughness, dielectric
Coefficient, service life and prior piezoelectric property have a very big impact, and therefore prepare the aluminium nitride piezoelectricity of high-orientation
Thin film just seems significant.
Summary of the invention
Based on mentioned above, the present invention provides a kind of a axle orientational strengthening type AlN thin film and preparation method thereof, the present invention's
The equipment of preparation technology and use is the most conventional, and the aluminum nitride piezoelectric film prepared can be applicable to high frequency, dynamo-electric coupling high-power, high
Close PTC device, and prepared product reliability is strong, yield rate is high, low cost, the most large-scale popularization and application.
First, the present invention discloses the technical scheme of a kind of a axle orientational strengthening type AlN thin film:
Including N-shaped Si (100) substrate, a axle orientation AlN cushion being deposited on its surface delays with being deposited on a axle orientation AlN
Rush a axle orientation AlN thin film on layer;Wherein, N-shaped Si (100) substrate single-sided polishing, its thickness is preferably 525 μm, and surface is thick
It is 3~10nm that rugosity is not higher than 4nm, a axle orientation AlN buffer layer thickness, and the thickness of a axle orientation AlN thin film is 400~500nm,
Its surface roughness is less than 2.3nm.
Secondly, the present invention discloses the technical scheme of a kind of technical scheme preparing a axle orientational strengthening type AlN thin film:
The preparation method of a kind of a axle orientational strengthening type AlN thin film, comprises the following steps:
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
Step E: described a axle orientation AlN thin film is made annealing treatment;Prepare a axle uniform, flawless orientation AlN thin
Film.
According to the preparation method of above a axle orientational strengthening type AlN thin film, before carrying out step A, N-shaped Si (100) is served as a contrast
The end, carries out single-sided polishing and cleaning step successively;Described single-sided polishing and cleaning step can be to be any suitable mode, purpose
It is that and obtains clean and smooth N-shaped Si (100) surface, so that the AlN thin film that subsequent step prepares can be more preferable
Deposition.The present invention specifically uses following cleaning step:
N-shaped Si (100) substrate is sequentially placed in acetone, dehydrated alcohol and deionized water and carries out ultrasonic cleaning, the most clearly
The time of washing is 10~20 minutes, and N-shaped Si (100) substrate after then using nitrogen to clean dries up.
In the present invention, substrate is carried out vacuum argon process by step A, after above process, substrate can be made to obtain atom level
Even curface, is conducive to growing high-quality thin film.Concrete operations are as follows: N-shaped Si (100) substrate is placed in magnetic control sputtering system
Chamber in, treat that vacuum is less than 8 × 10-5Time, it is 400~600 DEG C that chamber is warming up to temperature, is continually fed into argon and maintains
15~25 minutes.
AlN thin film is a kind of covalent crystal thin film with hexagonal wurtzite structure, lattice paprmeter
Al atom forms the [AlN of distortion with adjacent atom N4] tetrahedron, along c-axis direction Al-N bond distance it isAlong a direction of principal axis
Al-N bond distance beAnd the lattice paprmeter of monocrystal silicon isMismatch (lattice mismatch) due to lattice
Existence will affect the shape of depositing Al N thin film crystal grain, nucleation density, crystalline quality, the average-size of cluster and distribution etc.
Feature, therefore in the present invention, step B uses magnetron sputtering technique to prepare the AlN thin film of one layer of a axle orientation as further magnetic control
The cushion of sputtering, concrete technology parameter is as follows: N-shaped Si (100) substrate temperature is 400~600 DEG C;Sputtering power is 140W
~170W;Target-substrate distance is 7cm~9cm;The gas flow ratio of nitrogen and argon is 9: 19;Sputtering pressure is 1.0Pa~1.5Pa;
Sputtering time is 10~20 minutes;The target purity of nitrogen, argon and Al is 99.99%.
In the present invention, step C uses annealing;Stop during annealing being passed through nitrogen, argon and closing magnetron sputtering,
The process time is 20~30 minutes;The atom of the AlN thin film made of annealing under high temperature obtains higher energy, and makes atom at it
Surface migrates, and forms the AlN thin film of a axle orientation.
In the present invention, step D uses magnetron sputtering technique, at the AlN buffer-layer surface further precipitation height a axle of a axle orientation
The AlN thin film of orientation, due to the existence of cushion, not only slow down thermal mismatching effect, and decreases and produce because of dislocation
Crystal defect, and due to a axle orientation cushion existence so that the thin film deposited afterwards along a axle orientation grow,
And then the growth to the AlN thin film forming high a axle orientation has positive influences;Concrete technology parameter is as follows: deposition has cushion
N-shaped Si (100) underlayer temperature be 300 DEG C~600 DEG C;Sputtering power is 90W~120W;Target-substrate distance is 5cm~7cm;Nitrogen
It is 9: 19 with the gas flow ratio of argon;Sputtering pressure is 1.0Pa~1.5Pa;Sputtering time is 20~30 minutes;Nitrogen, argon
The purity of gas and Al target is 99.99%.
In the present invention, step E uses annealing to improve with the particle activation respond realizing on substrate, and then makes
Particle can rearrange redistribution at substrate surface, and promote crystal grain to grow up, space between crystal grain reduces, point defect and crystal boundary
Diminish, it is easier to form the AlN thin film of highly crystalline orientation, stop during annealing being passed through nitrogen, argon and closing magnetron sputtering,
The annealing time is 25~35 minutes.
According to mentioned above, the present invention has a following major advantage:
1. the present invention use AlN that a axle is orientated as cushion, due to the crystalline substance of the AlN thin film of its lattice and subsequent deposition
Lattice matching degree is high, and both similar thermal expansion coefficient;The cushion of the present invention has and the structure of AlN thin film homogeneity simultaneously,
Avoid dispersal behavior common between conventional transition layer and AlN thin film;Therefore, the magnetron sputtering technique pre-deposition that the present invention uses
Cushion improves the growth quality of AlN thin film, reduces its surface roughness, is conducive to improving the piezoelectric effect of AlN thin film also
Reduce the propagation loss of surface acoustic wave.
In preparation technology the most of the present invention, the preparation of the AlN thin film of cushion and highly oriented, high-quality is carried out without locellus,
Same vacuum chamber then can realize, and in preparation process, operation is simple, environmental protection and energy saving, and raw material supply is sufficient and cheap,
It is suitable for making high performance communication components and parts in modern communication technology.
3. the AlN thin film tool degree of orientation that prepared by the present invention is high, is orientated in a axle completely;Product reliability is strong, yield rate
Height, cost is relatively low, is advantageously applied in SAW device realize improving the spread speed of surface acoustic wave.
Accompanying drawing explanation
Fig. 1 is the structural representation of a axle orientational strengthening type AlN thin film that the present invention prepares.
Fig. 2 is the XRD analysis collection of illustrative plates of a axle orientational strengthening type AlN thin film that the embodiment of the present invention 1 prepares.
Fig. 3 is the XRD analysis collection of illustrative plates of a axle orientational strengthening type AlN thin film that the embodiment of the present invention 3 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment and Figure of description, the present invention is further elaborated:
The structural representation of a kind of a axle orientational strengthening type AlN thin film disclosed by the invention is as shown in Figure 1;The present embodiment has
Body is: by N-shaped Si (100) substrate of single-sided polishing, a axle orientation AlN cushion and a axle orientation AlN thin film the most from the bottom to top
Superposition forms;Wherein, the thickness of N-shaped Si (100) substrate is preferably 525 μm, and its surface roughness is not higher than 4nm, a axle orientation
AlN buffer layer thickness is 3~10nm, and the thickness of a axle orientation AlN thin film is 400~500nm, and its surface roughness is less than
2.3nm。
Embodiment 1:
The preparation method of a kind of a axle orientational strengthening type AlN thin film, comprises the following steps:
Before carrying out step A, generally N-shaped Si (100) substrate surface is polished, cleaning treatment;
Surface finish processes: is polished by the surface diamond mud of N-shaped Si (100) substrate, uses optical microscope
After observation substrate surface does not has cut, then use the cmp method of prior art that substrate is processed by shot blasting.
Cleaning treatment: first N-shaped Si (100) substrate is put supersound process about 10 minutes in acetone, clear with deionized water
Wash clean, puts into supersound process about 10 minutes in ethanol, cleans up with deionized water, puts in deionized water supersound process about
10 minutes, finally dry up with pure nitrogen gas.
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
N-shaped Si (100) substrate cleaned up is put in the chamber of magnetic control sputtering system and (notice that chamber to keep clean
Only), first by mechanical pump, sputtering chamber is evacuated to low vacuum state, then with molecular pump, chamber is evacuated to high vacuum state,
The vacuum of the present embodiment is 3 × 10-5Pa;Then pass to a small amount of argon, and N-shaped Si (100) substrate is heated, heat up
After 420 DEG C, it is incubated 15 minutes, then tackles chamber before carrying out next step and carry out dehumidifying to guarantee chamber interior sufficiently dry;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
By target-substrate distance regulation to 7cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 140W,
Sputtering pressure is 1.2Pa, and N-shaped Si (100) underlayer temperature is 450 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 12 minutes, prepares the AlN cushion of a axle orientation;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 20 minutes;This step is used for improving knot
Brilliant performance, improves crystal mass;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
By target-substrate distance regulation to 5cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, and the Al target using a diameter of 110mm, purity to be 99.99%, regulation sputtering power is 90W, spatters
Pressure of emanating is 300 DEG C for 1.0Pa, N-shaped Si (100) underlayer temperature;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 25 minutes, prepares the AlN thin film of a axle orientational strengthening;This step purpose
For: further growth high-quality, highly oriented a axle orientation AlN thin film on the AlN cushion of a axle orientation;
Step E: described a axle orientation AlN thin film is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 27 minutes;Degree of crystallinity is optimized with this
And crystal mass, finally prepare high-quality, highly oriented a axle orientation AlN thin film.
Embodiment 2:
The preparation method of a kind of a axle orientational strengthening type AlN thin film, comprises the following steps:
Before carrying out step A, generally N-shaped Si (100) substrate surface is polished, cleaning treatment;
Surface finish processes: is polished by the surface diamond mud of N-shaped Si (100) substrate, uses optical microscope
After observation substrate surface does not has cut, then use the cmp method of prior art that substrate is processed by shot blasting.
Cleaning treatment: first N-shaped Si (100) substrate is put supersound process about 10 minutes in acetone, clear with deionized water
Wash clean, puts into supersound process about 10 minutes in ethanol, cleans up with deionized water, puts in deionized water supersound process about
10 minutes, finally dry up with pure nitrogen gas.
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
N-shaped Si (100) substrate cleaned up is put in the chamber of magnetic control sputtering system and (notice that chamber to keep clean
Only), first by mechanical pump, sputtering chamber is evacuated to low vacuum state, then with molecular pump, chamber is evacuated to high vacuum state,
The vacuum of the present embodiment is 1 × 10-5Pa;Then pass to a small amount of argon, and N-shaped Si (100) substrate is heated, heat up
After 580 DEG C, it is incubated 25 minutes, then tackles chamber before carrying out next step and carry out dehumidifying to guarantee chamber interior sufficiently dry;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
By target-substrate distance regulation to 9cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 170W,
Sputtering pressure is 1.5Pa, and N-shaped Si (100) underlayer temperature is 600 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 20 minutes, prepares the AlN cushion of a axle orientation;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 25 minutes;This step is used for improving knot
Brilliant performance, improves crystal mass;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
By target-substrate distance regulation to 7cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 110W,
Sputtering pressure is 1.4Pa, and N-shaped Si (100) underlayer temperature is 300 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 28 minutes, prepares the AlN thin film of a axle orientational strengthening;This step purpose
For: further growth high-quality, highly oriented a axle orientation AlN thin film on the AlN cushion of a axle orientation;
Step E: described a axle orientation AlN thin film is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 30 minutes;Degree of crystallinity is optimized with this
And crystal mass, finally prepare high-quality, highly oriented a axle orientation AlN thin film.
Embodiment 3:
The preparation method of a kind of a axle orientational strengthening type AlN thin film, comprises the following steps:
Before carrying out step A, generally N-shaped Si (100) substrate surface is polished, cleaning treatment;
Surface finish processes: is polished by the surface diamond mud of N-shaped Si (100) substrate, uses optical microscope
After observation substrate surface does not has cut, then use the cmp method of prior art that substrate is processed by shot blasting.
Cleaning treatment: first N-shaped Si (100) substrate is put supersound process about 10 minutes in acetone, clear with deionized water
Wash clean, puts into supersound process about 10 minutes in ethanol, cleans up with deionized water, puts in deionized water supersound process about
10 minutes, finally dry up with pure nitrogen gas.
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
N-shaped Si (100) substrate cleaned up is put in the chamber of magnetic control sputtering system and (notice that chamber to keep clean
Only), first by mechanical pump, sputtering chamber is evacuated to low vacuum state, then with molecular pump, chamber is evacuated to high vacuum state,
The vacuum 8 × 10 of the present embodiment-7Pa;Then pass to a small amount of argon, and N-shaped Si (100) substrate is heated, be warming up to
It is incubated 20 minutes after 500 DEG C, then tackles chamber before carrying out next step and carry out dehumidifying to guarantee chamber interior sufficiently dry;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
By target-substrate distance regulation to 8cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 160W,
Sputtering pressure is 1.0Pa, and N-shaped Si (100) underlayer temperature is 550 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 15 minutes, prepares the AlN cushion of a axle orientation;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 30 minutes;This step is used for improving knot
Brilliant performance, improves crystal mass;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
By target-substrate distance regulation to 6cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 110W,
Sputtering pressure is 1.3Pa, and N-shaped Si (100) underlayer temperature is 450 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 20 minutes, prepares the AlN thin film of a axle orientational strengthening;This step purpose
For: further growth high-quality, highly oriented a axle orientation AlN thin film on the AlN cushion of a axle orientation;
Step E: described a axle orientation AlN thin film is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 35 minutes;Degree of crystallinity is optimized with this
And crystal mass, finally prepare high-quality, highly oriented a axle orientation AlN thin film.
Embodiment 4:
The preparation method of a kind of a axle orientational strengthening type AlN thin film, comprises the following steps:
Before carrying out step A, generally N-shaped Si (100) substrate surface is polished, cleaning treatment;
Surface finish processes: is polished by the surface diamond mud of N-shaped Si (100) substrate, uses optical microscope
After observation substrate surface does not has cut, then use the cmp method of prior art that substrate is processed by shot blasting.
Cleaning treatment: first N-shaped Si (100) substrate is put supersound process about 10 minutes in acetone, clear with deionized water
Wash clean, puts into supersound process about 10 minutes in ethanol, cleans up with deionized water, puts in deionized water supersound process about
10 minutes, finally dry up with pure nitrogen gas.
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
N-shaped Si (100) substrate cleaned up is put in the chamber of magnetic control sputtering system and (notice that chamber to keep clean
Only), first by mechanical pump, sputtering chamber is evacuated to low vacuum state, then with molecular pump, chamber is evacuated to high vacuum state,
The vacuum of the present embodiment is 3 × 10-5Pa;Then pass to a small amount of argon, and N-shaped Si (100) substrate is heated, heat up
After 400 DEG C, it is incubated 15 minutes, then tackles chamber before carrying out next step and carry out dehumidifying to guarantee chamber interior sufficiently dry;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
By target-substrate distance regulation to 7cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, the Al target using a diameter of 110mm, purity to be 99.99%, and regulation sputtering power is 140W,
Sputtering pressure is 1.0Pa, and N-shaped Si (100) underlayer temperature is 400 DEG C;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 10 minutes, prepares the AlN cushion of a axle orientation;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 20 minutes;This step is used for improving knot
Brilliant performance, improves crystal mass;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
By target-substrate distance regulation to 5cm, nitrogen and the argon that the present embodiment uses purity to be 99.99%, and make nitrogen and
The flow-rate ratio of argon is 9: 19, and the Al target using a diameter of 110mm, purity to be 99.99%, regulation sputtering power is 90W, spatters
Pressure of emanating is 300 DEG C for 1.0Pa, N-shaped Si (100) underlayer temperature;Then utilize the method for magnetron sputtering at described N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time is 20 minutes, prepares the AlN thin film of a axle orientational strengthening;This step purpose
For: further growth high-quality, highly oriented a axle orientation AlN thin film on the AlN cushion of a axle orientation;
Step E: described a axle orientation AlN thin film is made annealing treatment;
Stop being passed through argon and nitrogen, and close magnetron sputtering power, make annealing treatment 25 minutes;Degree of crystallinity is optimized with this
And crystal mass, finally prepare high-quality, highly oriented a axle orientation AlN thin film.
Above embodiments of the invention are described in detail, but described content have been only presently preferred embodiments of the present invention,
And need not be with the restriction present invention.All any amendments made in the application range of the present invention, equivalent and improvement etc. all should
Within being included in protection scope of the present invention.
Claims (9)
1. an a axle orientational strengthening type AlN thin film, it is characterised in that include N-shaped Si (100) substrate, be deposited on a on its surface
Axle orientation AlN cushion and a axle orientation AlN thin film being deposited on a axle orientation AlN cushion;Described N-shaped Si (100) substrate
Surface roughness be not higher than 4nm, described a axle orientation AlN buffer layer thickness is 3~10nm, described a axle orientation AlN thin film
Thickness is 400~500nm, and surface roughness is less than 2.3nm.
2. the preparation method of an a axle orientational strengthening type AlN thin film, it is characterised in that comprise the following steps:
Step A: N-shaped Si (100) substrate is put in the chamber of magnetic control sputtering system and carry out vacuum argon process;
Step B: use magnetron sputtering technique to deposit a axle orientation AlN cushion on Si (100) crystal face;
Step C: described a axle orientation AlN cushion is made annealing treatment;
Step D: use magnetron sputtering technique to deposit a axle orientation AlN thin film on a axle orientation AlN cushion;
Step E: described a axle orientation AlN thin film is made annealing treatment;Prepare a axle uniform, flawless orientation AlN thin film.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that carrying out
Before step A, N-shaped Si (100) substrate is carried out single-sided polishing and cleaning step successively.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described clearly
Wash step particularly as follows: be sequentially placed in acetone, dehydrated alcohol and deionized water by N-shaped Si (100) substrate and carry out ultrasonic cleaning, often
Secondary scavenging period is 10~20 minutes, and N-shaped Si (100) substrate after then using nitrogen to clean dries up.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described step
Rapid A, particularly as follows: be placed in the chamber of magnetic control sputtering system by N-shaped Si (100) substrate, treats that vacuum reaches 8 × 10-5Time, by chamber
It is 400~600 DEG C that room is warming up to temperature, is continually fed into argon and maintains 15~25 minutes.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described step
In rapid B, the parameter of magnetron sputtering technique is specific as follows: N-shaped Si (100) substrate temperature is 400~600 DEG C;Sputtering power is
140W~170W;Target-substrate distance is 7cm~9cm;The gas flow ratio of nitrogen and argon is 9: 19;Sputtering pressure be 1.0Pa~
1.5Pa;Sputtering time is 10~20 minutes;The target purity of nitrogen, argon and Al is 99.99%.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described step
Stopping being passed through nitrogen, argon and closing magnetron sputtering during annealing in rapid C, the annealing time is 20~30 minutes.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described step
In rapid D, the parameter of magnetron sputtering technique is specific as follows: deposition has N-shaped Si (100) underlayer temperature of cushion to be 300 DEG C~600
℃;Sputtering power is 90W~120W;Target-substrate distance is 5cm~7cm;The gas flow ratio of nitrogen and argon is 9: 19;Sputtering pressure
For 1.0Pa~1.5Pa;Sputtering time is 20~30 minutes;The purity of nitrogen, argon and Al target is 99.99%.
The preparation method of a kind of a axle orientational strengthening type AlN thin film the most according to claim 2, it is characterised in that described step
Stopping being passed through nitrogen, argon and closing magnetron sputtering during annealing in rapid E, the annealing time is 25~35 minutes.
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