CN106244984B - Enhanced AlN films of a kind of a axis orientation and preparation method thereof - Google Patents
Enhanced AlN films of a kind of a axis orientation and preparation method thereof Download PDFInfo
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- CN106244984B CN106244984B CN201610633215.6A CN201610633215A CN106244984B CN 106244984 B CN106244984 B CN 106244984B CN 201610633215 A CN201610633215 A CN 201610633215A CN 106244984 B CN106244984 B CN 106244984B
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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
- 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
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
Abstract
The invention discloses a kind of a axis to be orientated enhanced AlN films and preparation method thereof, belongs to electronic information function material and device arts.The present invention is using following preparation method：Using Si (100) substrate of N-shaped, it puts it into magnetic control sputtering system chamber after being vacuum-treated, using different magnetron sputtering techniques and combine annealing, a axis is prepared first is orientated AlN buffer layers, then preferred orientation growing AIN film on this basis, since the two lattice match is high, so as to improve the growth quality of AlN films, its surface roughness is reduced, and then is conducive to the propagation loss for improving the piezoelectric effect of AlN films and reducing surface acoustic wave；Operation is simple in preparation process of the present invention, environmental protection and energy saving, and raw material supply is sufficient and cheap, and mass production technique is controllable, convenient for batch production and application, is suitable for making high performance communication component in modern communication technology.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to a kind of enhanced AlN of a axis orientation
Film and preparation method thereof can be used for making the first device of the communications such as resonator, energy converter, the piezoelectric transducer in modern communication technology
Part.
Background technology
Communications industry is quickly grown in recent years, and the frequency of communication system and communication apparatus increasingly improves, integrated level is more next
Higher, size increasingly reduces, and to the filter applied to communication apparatus, more stringent requirements are proposed for this.And traditional dielectric filter
Body product is excessive, and low-temperature co-fired ceramics filter filtering performance is relatively poor, these are all difficult to meet communication apparatus miniaturization, collection
At the requirement changed with high reliability.
Surface acoustic wave techniques is in the late 1860s phase as a kind of emerging electronics, acoustics and materialogy phase
In conjunction with new discipline, start the reason for going on rapid development.Because it is with small, light-weight, stability is good, reliability
High, many-sided advantage such as power is small 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.Especially on mobile communication field, the irreplaceable ground of surface acoustic wave techniques
Position has pushed correlative study to advance.
With the rapid development of the third generations wireless communication technique such as W-CDMA, communication system medium-high frequency section (5GHz or more) is humorous
Shake device and filter demand it is increasing.Zinc oxide (ZnO), lithium niobate (LiTaO3) etc. the piezoelectric film material that generally uses
Acoustic surface wave propagation speed is below 6000m/s, and in contrast, aluminium nitride (AlN) has most in all non-ferroelectric substances
Fast acoustic surface wave propagation speed.For the lower surface acoustic wave crystalline material of acoustic surface wave propagation speed, made of it
The SAW device of 2.5GHz, IDT finger widths d are generally less than 0.4 micron, and it is micro- that the corresponding finger widths d of 5GHz should be less than 0.2
Rice, the corresponding finger widths d of 10GHz are less than 0.1 micron, approach the limit of current semi-conductor industry level, cause severed finger serious, and
And at wiring capacitance, in high frequency, interdigital is easy to be connected since intensive interdigital metal finger is arranged in parallel, it is serious to restrict
The further increasing of SAW device frequency.Therefore, the material of high acoustic surface wave propagation speed is selected to enable to interdigital
Reach high frequency, powerful requirement when finger beam is wider.
Aluminium nitride (AlN) is III-V group compound, is generally existed with the wurtzite structure in hexagonal crystal system.Aluminium nitride film
With many excellent properties, for example, it is high pyroconductivity, excellent chemical stability and low toxic, good optical
Can, through studying it with direct band gap broad stopband structure, energy gap 6.2eV, and highly oriented aluminium nitride film is even more to gather around
Have many advantages, such as high-insulativity, low thermal coefficient of expansion, high dielectric breakdown strength, excellent mechanical strength, make its machinery,
Microelectronics, optics and electronic component, the manufacture of SAW device, high-frequency wideband communicates and the fields such as power semiconductor
It has broad application prospects.Wherein aluminium nitride film becomes because of high acoustic wave propagation velocity and big piezoelectric coupling coefficient
Ideal piezoelectric material, particularly suitable for making the SAW device (SAW) and bulk wave (BAW) device of 5 GHz band.
Resistivity, leakage current due to the crystallinity of aluminium nitride film, crystalline quality to material, surface roughness, dielectric
Coefficient, service life and prior piezoelectric property have a very big impact, therefore prepare the aluminium nitride piezoelectricity of high-orientation
Film just seems significant.
Invention content
It is of the invention based on a kind of described above, enhanced AlN films of a axis orientation of present invention offer and preparation method thereof
Preparation process and the equipment used are more common, and aluminum nitride piezoelectric film obtained can be applied to high frequency, high-power, high electromechanical coupling
PTC device is closed, and obtained product reliability is strong, high yield rate, it is at low cost, be conducive to promote and apply on a large scale.
First, the present invention discloses the technical solution that a kind of a axis is orientated enhanced AlN films：
Including N-shaped Si (100) substrate, a axis for being deposited on its surface, which is orientated AlN buffer layers and is deposited on a axis orientation AlN, to be delayed
The a axis rushed on layer is orientated AlN films；Wherein, N-shaped Si (100) substrate single-sided polishing, thickness is preferably 525 μm, and surface is thick
Rugosity is not higher than 4nm, and it is 3~10nm that a axis, which is orientated AlN buffer layer thicknesses, and the thickness that a axis is orientated AlN films is 400~500nm,
Its surface roughness is less than 2.3nm.
Secondly, the present invention discloses a kind of technical solution for preparing a axis and being orientated the technical solution of enhanced AlN films：
A kind of a axis is orientated the preparation method of enhanced AlN films, includes the following steps：
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers；
Step C：AlN buffer layers are orientated to a axis to make annealing treatment；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films；
Step E：AlN films are orientated to a axis to make annealing treatment；It is thin that uniform, flawless a axis orientation AlN is made
Film.
It is orientated the preparation method of enhanced AlN films according to the above a axis, before carrying out step A, N-shaped Si (100) are served as a contrast
Bottom carries out single-sided polishing and cleaning step successively；The single-sided polishing and cleaning step can be any suitable way, purpose
Acquisition cleaning and smooth N-shaped Si (100) surface are that, so that AlN films made from subsequent step can be better
Deposition.The present invention specifically uses following cleaning step：
N-shaped Si (100) substrate is sequentially placed into acetone, absolute ethyl alcohol and deionized water and is cleaned by ultrasonic, it is clear every time
It is 10~20 minutes to wash the time, then nitrogen is used to dry up N-shaped Si (100) substrate after cleaning.
Substrate is carried out vacuum argon gas processing by step A in the present invention, after handling above, substrate can be made to obtain atom level
Even curface is conducive to grow high-quality thin film.Concrete operations are as follows：N-shaped Si (100) substrate is placed in magnetic control sputtering system
Chamber in, wait for vacuum degree be less than 8 × 10-5When, it is 400~600 DEG C that chamber, which is warming up to temperature, is continually fed into argon gas and maintains
15~25 minutes.
AlN films are a kind of covalent crystal film with hexagonal wurtzite structure, lattice constantAl atoms form the [AlN of distortion with adjacent N atoms4] tetrahedron, along c-axis direction Al-N
Bond distance isAl-N bond distance along a axis directions isAnd the lattice constant of monocrystalline silicon isDue to lattice
The presence of mismatch (lattice mismatch) will influence the shape of depositing Al N thin film crystal grain, nucleation density, crystalline quality, group
The features such as average-size of cluster and distribution, therefore step B prepares what one layer of a axis was orientated using magnetron sputtering technique in the present invention
Buffer layer of the AlN films as further magnetron sputtering, specific process parameter are 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 gas is 9: 19；It splashes
Pressure of emanating is 1.0Pa~1.5Pa；Sputtering time is 10~20 minutes；The target purity of nitrogen, argon gas and Al is 99.99%.
Step C is using annealing in the present invention；Stop being passed through nitrogen, argon gas and closing magnetron sputtering when annealing,
Processing time is 20~30 minutes；The atom of the AlN films made of annealing under high temperature obtains higher energy, and makes atom at it
Surface migrates, and forms the AlN films that a axis is orientated.
Step D uses magnetron sputtering technique in the present invention, and high a axis is further deposited in the AlN buffer-layer surfaces that a axis is orientated
The AlN films of orientation not only slow down thermal mismatching effect, but also reduce and generated because of dislocation due to the presence of buffer layer
Crystal defect, and due to a axis be orientated buffer layer presence so that the film deposited later is orientated along a axis to be grown,
And then there are positive influences to the growth for forming the AlN films that high a axis is orientated；Specific process parameter is as follows：Deposition has buffer layer
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
Gas flow ratio with argon gas is 9: 19；Sputtering pressure is 1.0Pa~1.5Pa；Sputtering time is 20~30 minutes；Nitrogen, argon
The purity of gas and Al targets is 99.99%.
Step E uses annealing to realize that the particle activation respond on substrate improves in the present invention, so that
Particle can rearrange redistribution in substrate surface, and promote crystal grain to grow up, gap reduction, point defect and crystal boundary between crystal grain
Become smaller, it is easier to form the AlN films of highly crystalline orientation, when annealing, stops being passed through nitrogen, argon gas and closing magnetron sputtering,
It is 25~35 minutes to make annealing treatment the time.
According to described above, the present invention has following major advantage：
1. the AlN that the present invention is orientated using a axis is as buffer layer, due to the crystalline substance of its lattice and the AlN films of subsequent deposition
Lattice matching degree is high, and the two similar thermal expansion coefficient；The buffer layer of the present invention has the structure with AlN film homogeneities simultaneously,
Avoid dispersal behavior common between conventional transition layer and AlN films；Therefore, the magnetron sputtering technique pre-deposition that the present invention uses
Buffer layer improves the growth quality of AlN films, reduces its surface roughness, is conducive to the piezoelectric effect of raising AlN films simultaneously
Reduce the propagation loss of surface acoustic wave.
2. the preparation of buffer layer and highly oriented, high-quality AlN films is carried out without locellus in preparation process of the present invention,
Same vacuum chamber can then realize that operation is simple in preparation process, environmental protection and energy saving, and raw material supply is sufficient and cheap,
It is suitable for making high performance communication component in modern communication technology.
3. the AlN films tool degree of orientation prepared by the present invention is high, it is orientated in complete a axis；Product reliability is strong, yield rate
Height, cost is relatively low, is advantageously applied in SAW device to realize the spread speed for improving surface acoustic wave.
Description of the drawings
Fig. 1 is the structural schematic diagram that a axis produced by the present invention is orientated enhanced AlN films.
Fig. 2 is the XRD analysis collection of illustrative plates that a axis is orientated enhanced AlN films made from the embodiment of the present invention 1.
Fig. 3 is the XRD analysis collection of illustrative plates that a axis is orientated enhanced AlN films made from the embodiment of the present invention 3.
Specific implementation mode
With reference to specific embodiment and Figure of description, the present invention is further elaborated：
The structural schematic diagram that a kind of a axis disclosed by the invention is orientated enhanced AlN films is as shown in Figure 1；The present embodiment has
Body is：By N-shaped Si (100) substrate of single-sided polishing, a axis is orientated AlN buffer layers and a axis is orientated AlN films successively from the bottom to top
Superposition composition；Wherein, the thickness of N-shaped Si (100) substrate is preferably 525 μm, and surface roughness is not higher than 4nm, and a axis is orientated
AlN buffer layer thicknesses are 3~10nm, and the thickness that a axis is orientated AlN films is 400~500nm, and surface roughness is less than
2.3nm。
Embodiment 1：
A kind of a axis is orientated the preparation method of enhanced AlN films, includes the following steps：
Before carrying out step A, usually N-shaped Si (100) substrate surface is polished, cleaning treatment；
Surface polishing treatment：The surface of N-shaped Si (100) substrate is polished with diamond mud, uses light microscope
After observation substrate surface does not have cut, then the cmp method of the prior art is used to be processed by shot blasting substrate.
Cleaning treatment：N-shaped Si (100) substrate is put first and is ultrasonically treated in acetone about 10 minutes, it is clear with deionized water
Wash clean is put into ethyl alcohol and is ultrasonically treated about 10 minutes, cleaned up with deionized water, be put into deionized water and be ultrasonically treated about
It 10 minutes, is finally dried up with pure nitrogen gas.
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
N-shaped Si (100) substrate cleaned up is put into the chamber of magnetic control sputtering system and (notices that chamber will keep clean
Only), sputtering chamber is evacuated to low vacuum state using mechanical pump first, chamber is then evacuated to high vacuum state with molecular pump,
The vacuum degree of the present embodiment is 3 × 10-5Pa；A small amount of argon gas is then passed to, and N-shaped Si (100) substrate is heated, is heated up
15 minutes are kept the temperature after to 420 DEG C, then should be dehumidified to chamber before carrying out next step to ensure chamber interior sufficiently dry；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers；
Target-substrate distance is adjusted to 7cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 12 minutes, and the AlN buffer layers that a axis is orientated are made；
Step C：AlN buffer layers are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 20 minutes；This step is tied for improving
Brilliant performance improves crystal quality；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films；
Target-substrate distance is adjusted to 5cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, adjusting sputtering power is 90W, is splashed
Pressure of emanating is 1.0Pa, and N-shaped Si (100) underlayer temperature is 300 DEG C；Then utilize the method for magnetron sputtering in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 25 minutes, and the AlN films that a axis is orientated enhancing are made；This step purpose
For：Further growth high-quality, highly oriented a axis are orientated AlN films on the AlN buffer layers that a axis is orientated；
Step E：AlN films are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 27 minutes；Optimize crystallinity with this
And crystal quality, high-quality is finally made, highly oriented a axis is orientated AlN films.
Embodiment 2：
A kind of a axis is orientated the preparation method of enhanced AlN films, includes the following steps：
Before carrying out step A, usually N-shaped Si (100) substrate surface is polished, cleaning treatment；
Surface polishing treatment：The surface of N-shaped Si (100) substrate is polished with diamond mud, uses light microscope
After observation substrate surface does not have cut, then the cmp method of the prior art is used to be processed by shot blasting substrate.
Cleaning treatment：N-shaped Si (100) substrate is put first and is ultrasonically treated in acetone about 10 minutes, it is clear with deionized water
Wash clean is put into ethyl alcohol and is ultrasonically treated about 10 minutes, cleaned up with deionized water, be put into deionized water and be ultrasonically treated about
It 10 minutes, is finally dried up with pure nitrogen gas.
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
N-shaped Si (100) substrate cleaned up is put into the chamber of magnetic control sputtering system and (notices that chamber will keep clean
Only), sputtering chamber is evacuated to low vacuum state using mechanical pump first, chamber is then evacuated to high vacuum state with molecular pump,
The vacuum degree of the present embodiment is 1 × 10-5Pa；A small amount of argon gas is then passed to, and N-shaped Si (100) substrate is heated, is heated up
25 minutes are kept the temperature after to 580 DEG C, then should be dehumidified to chamber before carrying out next step to ensure chamber interior sufficiently dry；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers；
Target-substrate distance is adjusted to 9cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 20 minutes, and the AlN buffer layers that a axis is orientated are made；
Step C：AlN buffer layers are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 25 minutes；This step is tied for improving
Brilliant performance improves crystal quality；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films；
Target-substrate distance is adjusted to 7cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 28 minutes, and the AlN films that a axis is orientated enhancing are made；This step purpose
For：Further growth high-quality, highly oriented a axis are orientated AlN films on the AlN buffer layers that a axis is orientated；
Step E：AlN films are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 30 minutes；Optimize crystallinity with this
And crystal quality, high-quality is finally made, highly oriented a axis is orientated AlN films.
Embodiment 3：
A kind of a axis is orientated the preparation method of enhanced AlN films, includes the following steps：
Before carrying out step A, usually N-shaped Si (100) substrate surface is polished, cleaning treatment；
Surface polishing treatment：The surface of N-shaped Si (100) substrate is polished with diamond mud, uses light microscope
After observation substrate surface does not have cut, then the cmp method of the prior art is used to be processed by shot blasting substrate.
Cleaning treatment：N-shaped Si (100) substrate is put first and is ultrasonically treated in acetone about 10 minutes, it is clear with deionized water
Wash clean is put into ethyl alcohol and is ultrasonically treated about 10 minutes, cleaned up with deionized water, be put into deionized water and be ultrasonically treated about
It 10 minutes, is finally dried up with pure nitrogen gas.
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
N-shaped Si (100) substrate cleaned up is put into the chamber of magnetic control sputtering system and (notices that chamber will keep clean
Only), sputtering chamber is evacuated to low vacuum state using mechanical pump first, chamber is then evacuated to high vacuum state with molecular pump,
The vacuum degree 8 × 10 of the present embodiment-7Pa；A small amount of argon gas is then passed to, and N-shaped Si (100) substrate is heated, is warming up to
20 minutes are kept the temperature after 500 DEG C, then should be dehumidified to chamber before carrying out next step to ensure chamber interior sufficiently dry；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers；
Target-substrate distance is adjusted to 8cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 15 minutes, and the AlN buffer layers that a axis is orientated are made；
Step C：AlN buffer layers are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 30 minutes；This step is tied for improving
Brilliant performance improves crystal quality；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films；
Target-substrate distance is adjusted to 6cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 20 minutes, and the AlN films that a axis is orientated enhancing are made；This step purpose
For：Further growth high-quality, highly oriented a axis are orientated AlN films on the AlN buffer layers that a axis is orientated；
Step E：AlN films are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 35 minutes；Optimize crystallinity with this
And crystal quality, high-quality is finally made, highly oriented a axis is orientated AlN films.
Embodiment 4：
A kind of a axis is orientated the preparation method of enhanced AlN films, includes the following steps：
Before carrying out step A, usually N-shaped Si (100) substrate surface is polished, cleaning treatment；
Surface polishing treatment：The surface of N-shaped Si (100) substrate is polished with diamond mud, uses light microscope
After observation substrate surface does not have cut, then the cmp method of the prior art is used to be processed by shot blasting substrate.
Cleaning treatment：N-shaped Si (100) substrate is put first and is ultrasonically treated in acetone about 10 minutes, it is clear with deionized water
Wash clean is put into ethyl alcohol and is ultrasonically treated about 10 minutes, cleaned up with deionized water, be put into deionized water and be ultrasonically treated about
It 10 minutes, is finally dried up with pure nitrogen gas.
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
N-shaped Si (100) substrate cleaned up is put into the chamber of magnetic control sputtering system and (notices that chamber will keep clean
Only), sputtering chamber is evacuated to low vacuum state using mechanical pump first, chamber is then evacuated to high vacuum state with molecular pump,
The vacuum degree of the present embodiment is 3 × 10-5Pa；A small amount of argon gas is then passed to, and N-shaped Si (100) substrate is heated, is heated up
15 minutes are kept the temperature after to 400 DEG C, then should be dehumidified to chamber before carrying out next step to ensure chamber interior sufficiently dry；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers；
Target-substrate distance is adjusted to 7cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, and adjusting 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 in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 10 minutes, and the AlN buffer layers that a axis is orientated are made；
Step C：AlN buffer layers are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 20 minutes；This step is tied for improving
Brilliant performance improves crystal quality；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films；
Target-substrate distance is adjusted to 5cm, the present embodiment use purity for 99.99% nitrogen and argon gas, and make nitrogen and
The flow-rate ratio of argon gas is 9: 19, uses a diameter of 110mm, purity for 99.99% Al targets, adjusting sputtering power is 90W, is splashed
Pressure of emanating is 1.0Pa, and N-shaped Si (100) underlayer temperature is 300 DEG C；Then utilize the method for magnetron sputtering in the N-shaped Si
(100) depositing Al N thin film on substrate, sputtering time are 20 minutes, and the AlN films that a axis is orientated enhancing are made；This step purpose
For：Further growth high-quality, highly oriented a axis are orientated AlN films on the AlN buffer layers that a axis is orientated；
Step E：AlN films are orientated to a axis to make annealing treatment；
Stopping is passed through argon gas and nitrogen, and closes magnetron sputtering power, makes annealing treatment 25 minutes；Optimize crystallinity with this
And crystal quality, high-quality is finally made, highly oriented a axis is orientated AlN films.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
And without of the invention with limitation.All any modifications made in the application range of the present invention, equivalent replacement and improvement etc. should all
It is included within protection scope of the present invention.
Claims (4)
1. a kind of a axis is orientated the preparation method of enhanced AlN films, which is characterized in that include the following steps：
Step A：N-shaped Si (100) substrate is put into progress vacuum argon gas processing in the chamber of magnetic control sputtering system；
Step B：A axis is deposited on Si (100) crystal face using magnetron sputtering technique and is orientated AlN buffer layers, the magnetron sputtering work
The parameter of skill is specific as follows：N-shaped Si (100) substrate temperature is 400~600 DEG C；Sputtering power is 140W~170W；Target-substrate distance
For 7cm~9cm；The gas flow ratio of nitrogen and argon gas is 9: 19；Sputtering pressure is 1.0Pa~1.5Pa；Sputtering time be 10~
20 minutes；The target purity of nitrogen, argon gas and Al is 99.99%；
Step C：It is orientated AlN buffer layers to a axis to make annealing treatment, stops when annealing being passed through nitrogen, argon gas and closing
Magnetron sputtering is closed, the annealing time is 20~30 minutes；
Step D：Deposition a axis on AlN buffer layers is orientated in a axis using magnetron sputtering technique and is orientated AlN films, the magnetron sputtering
The parameter of technique is specific as follows：It is 300 DEG C~600 DEG C that deposition, which has N-shaped Si (100) underlayer temperature of buffer layer,；Sputtering power is
90W~120W；Target-substrate distance is 5cm~7cm；The gas flow ratio of nitrogen and argon gas is 9: 19；Sputtering pressure be 1.0Pa~
1.5Pa；Sputtering time is 20~30 minutes；The purity of nitrogen, argon gas and Al targets is 99.99%；
Step E：It is orientated AlN films to a axis to make annealing treatment, stops when annealing being passed through nitrogen, argon gas and closing
Magnetron sputtering, annealing time are 25~35 minutes, and uniform, flawless a axis is made and is orientated AlN films.
2. a kind of a axis according to claim 1 is orientated the preparation method of enhanced AlN films, which is characterized in that carrying out
Before step A, single-sided polishing and cleaning step are carried out successively to N-shaped Si (100) substrate.
3. a kind of a axis according to claim 2 is orientated the preparation method of enhanced AlN films, which is characterized in that described clear
Washing step is specially：N-shaped Si (100) substrate is sequentially placed into acetone, absolute ethyl alcohol and deionized water and is cleaned by ultrasonic, often
Secondary scavenging period is 10~20 minutes, then nitrogen is used to dry up N-shaped Si (100) substrate after cleaning.
4. a kind of a axis according to claim 1 is orientated the preparation method of enhanced AlN films, which is characterized in that the step
Suddenly A is specially：N-shaped Si (100) substrate is placed in the chamber of magnetic control sputtering system, waits for that vacuum degree reaches 8 × 10-5It, will when Pa
It is 400~600 DEG C that chamber, which is warming up to temperature, is continually fed into argon gas and maintains 15~25 minutes.
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| CN109722631B (en) * | 2019-01-24 | 2019-12-17 | 中国地质大学（武汉） | NiFe magnetic alloy film based on TiN substrate and preparation method thereof |
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