CN104862659B - A kind of medium frequency magnetron reaction sputtering method of aluminium nitride film - Google Patents
A kind of medium frequency magnetron reaction sputtering method of aluminium nitride film Download PDFInfo
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Abstract
The present invention relates to a kind of medium frequency magnetron reaction sputtering method in piezoelectric membrane manufacture field, more particularly to aluminium nitride film.The deposition film process of the present invention：High-purity argon gas and high pure nitrogen are passed through simultaneously first into vacuum cavity, and the content of wherein nitrogen is maintained at 20%~30%, sputtering sedimentation aluminium nitride film is started after aura is stable；Then with the 0.5sccm/min~4sccm/min ratio of argon gas and nitrogen at the uniform velocity in 10~20 minutes regulation sputter chambers, nitrogen content is made to increase to 50% from previous 20%~30% content；It is last not adjust sputtering power, and sputtering sedimentation aluminium nitride closes instrument under this atmosphere after 10 minutes, terminates film growth.The present invention can be being prepared while meeting the growth of C axle preferrel orientations, and surface microstructure growth is normal, even grain size, surfacing, is adapted to the high-quality aluminum nitride piezoelectric film for making SAW device.
Description
Technical field：
Field, more particularly to a kind of medium frequency magnetron reaction sputtering side of aluminium nitride film are manufactured the present invention relates to piezoelectric membrane
Method.
Background technology：
Aluminium nitride (AlN) is the compound of unique stabilization of aluminium (Al) and nitrogen (N) formation, is typical iii-v element
Compound semiconductor.Its structure cell belongs to hexagonal wurtzite structure, is that centered on aluminium atom, outside is folded around four nitrogen-atoms
The distorted tetrahedral closed.Aluminium nitride has a series of excellent physicochemical properties, for example：Big energy gap
(6.2eV)；High thermal conductivity (320W/mK)；Low-density (3.26g/cm3)；Big resistivity (1013Ω·cm)；High heat
Stability (more than 700 DEG C just occur surface oxidation)；High acoustic surface wave propagation speed (is 12000m/s along C axles, perpendicular to C
Axle is 6000m/s)；Big electromechanical coupling factor (K2=3%~8%)；It is mutually compatible with CMOS technology etc..These excellent things
Physicochemical property causes aluminum nitride piezoelectric film has in surface acoustic wave sensor and MEMS (MEMS) well should
Use prospect.And in current SAW device field, with radio communication and the high speed development of data transmission technology,
So that SAW device develops to GHz wave bands, and the loud propagation velocity of aluminium nitride film becomes preparation high workload
The preferred piezoelectric of the thin-film sound surface wave device of frequency.Therefore the high-quality aluminium nitride piezoelectricity for preparing satisfaction requirement is thin
Film seems particularly important.
At present, a variety of methods prepare the aluminium nitride film of C axle preferrel orientations, but wherein most suitable method
For intermediate frequency (40KHz) reactive magnetron sputtering method.MF reactive magnetron sputtering, compared to metal-organic chemical vapor deposition equipment
(MOCVD), the method for manufacturing thin film such as pulsed laser deposition (PLD), molecular beam epitaxy (MBE) has low growth temperature, Seedling height
Large area film deposition can be achieved, and meets the advantages such as the requirement of large-scale industrial production in speed, low cost.And should
Preparation method can be largely avoided the phenomenon of the sparking of target surface in d.c. sputtering and target poison ing, and greatly reduce and penetrate
Injury of radio frequency source (5~30MHz) electromagnetic wave to human body in RF sputtering.
But in medium frequency reactive sputtering technology, splash-proofing sputtering process parameter for aluminium nitride film growth quality influence very
Greatly, there is plasma and sputtering aluminum particulate is too high to the film surface temperature caused by the bombardment of film surface, Yi Jixiang
Film surface crystal grain can be all set the phenomenon of abnormal growth occur larger sputtering power, film surface will occur that some are micro-
The aluminium nitride bulky grain of rice-submicron order.This will cause very big influence to the quality of aluminium nitride film, and crystallite dimension is uneven
It is even to influence the piezoelectric property harmony propagation velocity of aluminium nitride film, and the bulky grain meeting of the micrometer-submicrometer level on surface
To the consequence of the bringing on a disaster property of manufacture of ensuing SAW device, send out the interdigital electrode (IDT) of SAW device
Raw fracture or short circuit, so as to cause device performance to fail.
The content of the invention：
There is problem or deficiency for above-mentioned, the invention provides a kind of medium frequency magnetron reaction sputtering side of aluminium nitride film
Method.
Specifically include following steps：
Step 1, substrate cleaning：Successively with acetone, alcohol, deionized water to being surpassed the substrate surface of deposition film
Sound is cleaned, after respectively cleaning 15 minutes, after cleaned substrate is dried up with nitrogen gun, is put into the drying baker for be filled with pure nitrogen gas and is added
Hot to 100 DEG C dry 1 hour.
Step 2, vacuum pre-treatment：The substrate that step 1 processing is obtained is positioned over the sample of medium frequency magnetron reaction sputtering system
In sample platform, cavity is closed.It is normal to start magnetron sputtering apparatus, 5 × 10 are evacuated to cavity-4Below Pa.
Step 3, pre-sputtering：70~80sccm high-purity argon gas is passed through into vacuum cavity, and (purity of argon is
99.999%) mid frequency sputtering power supply pre-sputter cleaning aluminium target (aluminium target purity is 99.999%) surface, is opened 15 minutes.
Step 4, deposition film, include three steps：
4.1st, into vacuum cavity, while being passed through high-purity argon gas (purity of argon is 99.999%), (nitrogen is pure with high pure nitrogen
Spend for 99.999%), and the content of wherein nitrogen is maintained between 20%~30%, open baffle plate after aura is stable, open
Beginning sputtering sedimentation aluminium nitride film, sputtering sedimentation 1~6 hour.
4.2nd, after 4.1 processes terminate, the ratio of argon gas and nitrogen in sputter chamber is progressively adjusted, makes nitrogen content from elder generation
Preceding 4.1 content increases to 50%.Regulations speed is maintained between 0.5sccm/min~4sccm/min, and whole regulation process exists
Completed in 10~20 minutes.
4.3rd, it is that nitrogen content is stable 50% after the completion of step 4.2, does not adjust sputtering power, then sputtered under this atmosphere
Cvd nitride aluminium closes instrument after 10 minutes, terminate film growth.
In 4.1 steps of the invention under relatively low nitrogen content (20%~30%), sputtering reaction is in compound state, in chemical combination
Be conducive to improving the C axle preferrel orientations of sputtering sedimentation aluminium nitride film under state.The content of higher nitrogen in 4.3 steps of the invention
(50%) under, sputtering reaction is in high moderate intoxication state, although being now unfavorable for the C axle preferrel orientations growth of aluminium nitride film,
But aluminium nitride film surface can be made to obtain the crystallite dimension of fine uniform, so as to effectively inhibit aluminium nitride film surface
Abnormal grain growth.In 4.2 steps of the invention, the atmosphere in sputter chamber is slowly varying, and this causes step 4.1-4.3 closely to tie
Be combined, whole sputter deposition process is a continuous thin film growth process, thus avoid atmosphere mutation or again
Do not planned a successor caused by build-up of luminance sputtering in film and stress in thin films is excessive the problems such as cause film separation.
Beneficial effects of the present invention in summary：It can prepare while meeting the growth of C axle preferrel orientations, surface microstructure
Growth is normal, even grain size, surfacing, is adapted to the high-quality aluminum nitride piezoelectric film for making SAW device.
Brief description of the drawings
Fig. 1 is the metallographic microscope test chart (40 times of amplification) of aluminium nitride film prepared by common process.
Fig. 2 is that the SAW device metallographic microscope test chart prepared on aluminium nitride film prepared by common process (is put
It is big 40 times).
Fig. 3 is SEM (SEM) test chart (10000 times of amplification) of the aluminum nitride grain of abnormal growth.
Fig. 4 is X-ray energy spectrum analysis (EDS) test chart of the aluminum nitride grain of abnormal growth.
Fig. 5 is X-ray diffractometer (XRD) test chart of aluminium nitride film prepared by three-steps process.
Fig. 6 is the metallographic microscope test chart (40 times of amplification) of aluminium nitride film prepared by three-steps process.
Fig. 7 is the SAW device metallographic microscope test chart prepared on aluminium nitride film prepared by three-steps process
(40 times of amplification).
Embodiment：
With a special case combination specific steps, the present invention is described further with accompanying drawing below：
1st, substrate is cleaned：We are used with four kinds of substrates of different, silicon (Si (100)) substrate of finishing polish, essence throwing in experiment
Titanium alloy (TC4) substrate, ordinary glass substrate (glass), quartz (quartz) substrate of finishing polish of light.Successively with acetone,
Alcohol, deionized water are cleaned by ultrasonic to substrate surface, and after respectively cleaning 15 minutes, cleaned substrate is dried up with nitrogen gun
Afterwards, be put into the drying baker for be filled with pure nitrogen gas be heated to 100 DEG C dry 1 hour.
2nd, vacuum pre-treatment：Four kinds of substrates that step 1 processing is obtained are positioned over the sample of medium frequency magnetron reaction sputtering system
In sample platform, cavity is closed.It is normal to start magnetron sputtering apparatus, 5 × 10 are evacuated to cavity-4Below Pa.
3rd, pre-sputtering：It is passed through into vacuum cavity in 70sccm high-purity argon gas (purity of argon is 99.999%), opening
RF sputtering power supply pre-sputter cleaning aluminium target (aluminium target purity is 99.999%) surface 15 minutes.
4th, deposition film, includes three steps：
4.1st, high-purity argon gas and high pure nitrogen (nitrogen gas purity is 99.999%) are passed through simultaneously into vacuum cavity, and make it
The content of middle nitrogen is maintained at 30%, opens baffle plate after aura is stable, starts sputtering sedimentation aluminium nitride film, sputtering sedimentation 2
Hour.If without ensuing 4.2 and 4.3, then 4.1 that is, common process, its aluminium nitride film and sound for preparing
Surface wave device such as Fig. 1 and Fig. 2, have substantial amounts of stain in film surface as can be seen from Figure 1, and micrometer-submicrometer level is presented, this
A little stains are the aluminium nitride big crystal grain of abnormal growth, and the crystal grain of these abnormal growths and following film are an entirety, no
It can be washed by common physical method.The aluminium nitride big crystal grain of abnormal growth between interdigital electrode as can be seen from Figure 2
Short circuit between electrode will be caused, so that device failure.Fig. 3 and Fig. 4 are that the aluminum nitride grain of abnormal growth is done
SEM and EDS analyses, the aluminum nitride grain of abnormal growth is micrometer-submicrometer level, and composition is aluminium nitride.Its EDS analysis result
It see the table below.
4.2nd, after 4.1 processes terminate, the ratio of argon gas and nitrogen in sputter chamber is progressively adjusted, makes nitrogen content from elder generation
The 30% of preceding 4.1 increases to 50%.Regulations speed is 2sccm/min, and whole regulation process is 10 minutes.Adjust and complete in atmosphere
Afterwards, sputtering power now should not can again adjust sputtering power because atmosphere changes and has declined.
After 4.3 adjust, nitrogen content is stable, and 50%, then under this atmosphere, sputtering sedimentation aluminium nitride is closed after 10 minutes
Instrument is closed, terminates film growth.After Fig. 5 is using three-step approach growth technique, the aluminium nitride deposited in 4 kinds of substrates of different
X-ray diffraction (XRD) test chart of piezoelectric membrane.It can be seen that in whole test scope, only occurring in that the C diffraction of aluminium nitride
Peak, the aluminium nitride film that this explanation is prepared using this paper three-step approach shows the C axle preferrel orientations of height.Its piezoelectricity
It can be completely used for preparing SAW device.Its aluminium nitride film and SAW device such as Fig. 6 and Fig. 7 for preparing.Can
To find out, the aluminum nitride piezoelectric film of sputtering sedimentation and the SAW device surface of preparation are all very clean on 4 kinds of substrates
Smooth, the crystal grain without abnormal growth does not result in interdigital electrode fracture or short circuit.
The technological parameter of whole mid frequency sputtering process see the table below
Claims (3)
1. a kind of medium frequency magnetron reaction sputtering method of aluminium nitride film, specifically includes following steps：
Step 1, substrate cleaning：The substrate surface of deposition film is carried out to i.e. with acetone, alcohol, deionized water successively ultrasonic clear
Wash, after respectively cleaning 15 minutes, after cleaned substrate is dried up with nitrogen gun, be put into the drying baker for be filled with pure nitrogen gas and be heated to
100 DEG C dry 1 hour；
Step 2, vacuum pre-treatment：The substrate that step 1 processing is obtained is positioned over the sample stage of medium frequency magnetron reaction sputtering system
On, close cavity；It is normal to start magnetron sputtering apparatus, 5 × 10 are evacuated to cavity-4Below Pa；
Step 3, pre-sputtering：The argon gas that 70~80sccm purity is 99.999% is passed through into vacuum cavity, mid frequency sputtering is opened
The aluminium target surface that power supply pre-sputter cleaning purity is 99.999% 15 minutes；
Step 4, deposition film, include three steps：
4.1st, the nitrogen that purity is 99.999% argon gas and purity is 99.999% is passed through simultaneously into vacuum cavity, and made wherein
The content of nitrogen is maintained between 20%~30%, is opened baffle plate after aura is stable, is started sputtering sedimentation aluminium nitride film, splash
Penetrate deposition 1~6 hour；
4.2nd, after step 4.1 process terminates, the ratio of argon gas and nitrogen in sputter chamber is progressively adjusted, makes nitrogen content from step
Rapid 4.1 content increases to 50%；Regulations speed is maintained between 0.5sccm/min~4sccm/min, and whole regulation process exists
Completed in 10~20 minutes；
4.3rd, it is that nitrogen content is stable 50% after the completion of step 4.2, does not adjust sputtering power, then the sputtering sedimentation under this atmosphere
Aluminium nitride closes instrument after 10 minutes, terminate film growth.
2. the medium frequency magnetron reaction sputtering method of aluminium nitride film as claimed in claim 1, it is characterised in that：The substrate is selected
Si (100) substrate, the titanium alloy TC 4 substrate of finishing polish, ordinary glass substrate (glass) and/or the stone of finishing polish of finishing polish
English (quartz) substrate.
3. the medium frequency magnetron reaction sputtering method of aluminium nitride film as claimed in claim 1, it is characterised in that：The work of sputter procedure
Skill parameters selection following table parameter
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| CN105977136A (en) * | 2016-05-27 | 2016-09-28 | 清华大学 | Semiconductor structure and method for preparing the same |
| CN106057640A (en) * | 2016-05-27 | 2016-10-26 | 清华大学 | Semiconductor structure and method for preparing semiconductor structure |
| CN107488828B (en) | 2016-06-12 | 2020-01-03 | 北京北方华创微电子装备有限公司 | Method for forming thin film and method for forming aluminum nitride thin film |
| CN106086801A (en) * | 2016-06-20 | 2016-11-09 | 浙江东晶博蓝特光电有限公司 | A kind of preparation method of PSS base AlN thin film |
| CN106222611A (en) * | 2016-09-22 | 2016-12-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of MF reactive magnetron sputtering preparation method of AlN piezoelectric membrane |
| CN109326696B (en) * | 2018-09-19 | 2021-04-27 | 华灿光电(苏州）有限公司 | Preparation method of epitaxial wafer of light-emitting diode |
| CN112760604B (en) * | 2019-11-01 | 2022-12-02 | 有研工程技术研究院有限公司 | Method for depositing high C-axis oriented aluminum nitride film on diamond substrate |
| CN113755804B (en) * | 2021-08-13 | 2023-09-12 | 中国电子科技集团公司第五十五研究所 | Preparation method of near-zero stress scandium-doped aluminum nitride film |
| CN114481026A (en) * | 2022-01-21 | 2022-05-13 | 深圳大学 | Preparation method of preferred orientation aluminum nitride film |
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