Thin Solid Films 519 (2011) 58465853

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Thin Solid Films

j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / t s f

Deposition and characterization of c-axis oriented aluminum nitride films by radio frequency magnetron sputtering without external substrate heating
Atul Vir Singh a, Sudhir Chandra a,, G. Bose b
a b

,1

Centre for Applied Research in Electronics (CARE), Indian Institute of Technology Delhi, Hauz Khas, New Delhi-110016, India Department of Applied Electronics and Instrumentation, Institute of Technical Education and Research, Jagmohan Nagar, Jagamara, Bhubaneswar-751030, Orissa, India

a r t i c l e

i n f o

a b s t r a c t
Aluminum nitride (AlN) lms were deposited on a variety of substrates (glass, Si, oxidized Si, AlSiO2Si, Cr SiO2Si, and AuCrSiO2Si) by radio frequency (RF) magnetron sputtering using an AlN target. The lms were deposited without external substrate heating. The effect of RF power, ambient gas (Ar and ArN2) and sputtering pressure on deposition rate and crystallinity were investigated. The structure and morphology of the lms were studied by X-ray diffraction, scanning electron microscopy and atomic force microscopy techniques. These investigations revealed that the AlN lms prepared in mixed gas ambient (ArN2) were highly c-axis oriented with moderate surface roughness on all the substrate. A strong IR absorption band was observed around 670 cm 1 which conrms the presence of AlN bond in the lm. The dc resistivity of the lms was measured to be in the range of 1011 to 1012 -cm at moderate electric elds. The application of these lms in piezoelectric based micro-electro-mechanical systems is discussed. 2011 Elsevier B.V. All rights reserved.

Article history: Received 30 June 2010 Received in revised form 20 February 2011 Accepted 22 February 2011 Available online 2 March 2011 Keywords: X-ray diffraction Radio-frequency magnetron sputtering Aluminum nitride Thin lms Microelectromechanical systems Acoustic resonators

1. Introduction Aluminum nitride (AlN) thin lms are gaining much interest among the researchers because of their unique properties such as wide band gap (6.2 eV), high thermal conductivity (2.85 W cm 1 K l), low thermal expansion coefcient (4.2 10 6 K 1 and 5.3 10 6 K 1 for the direction along and perpendicular to the c-axis respectively), high breakdown dielectric strength and highest acoustic wave velocity among the piezoelectric materials (11354 m/s and 5500 m/s for longitudinal and transversal bulk waves respectively, and 5607 m/s for surface wave) [13]. Moreover, it is not a ferroelectric material; so poling is not required for its use in piezoelectric sensor/actuator. These important properties of AlN lms are strongly dependent on the crystalline quality and crystal orientation. An AlN lm oriented along (002) plane with c-axis perpendicular to the substrate is preferentially required for better piezoelectric and acoustic properties [3,4]. Such highly c-axis oriented AlN lms can be used in microelectro-mechanical systems (MEMS) as a piezoelectric material for actuation and sensing. Further, these lms may also be used in modern telecommunication devices for high frequency resonators and lters based on surface acoustic wave (SAW) and lm bulk acoustic resonator (FBAR) devices [57].

Corresponding author. Tel.: +91 11 26591105; fax: +91 11 26596219. E-mail address: schandra@care.iitd.ernet.in (S. Chandra). 1 Present address. 0040-6090/$ see front matter 2011 Elsevier B.V. All rights reserved. doi:10.1016/j.tsf.2011.02.074

Depending on the desired applications, AlN lm can be grown by numerous techniques such as molecular beam epitaxy, chemical vapor deposition, reactive sputtering and pulsed laser deposition (PLD) [815]. Among these techniques, reactive sputtering is preferred for MEMS fabrication on account of lower deposition temperature, which makes it compatible with complementary metal oxide semiconductor (CMOS) technology. Extensive studies have been carried out on preparation of c-axis oriented AlN lms deposited on heated substrate by radio frequency (RF) or direct current (DC) reactive sputtering technique where a pure Al target is sputtered in argon-nitrogen gas [9,1113]. In reactive sputtering using Al target, hysteresis effect is known to cause the instability in the lm growth process due to the poisoning of metal target in presence of nitrogen gas [1619]. It is reported that AlN lm can also be prepared by using an AlN sputtering target with a more stable process but only a few reports are available in the literature [20]. In the present work, we have extensively investigated the preparation of c-axis oriented AlN lms by RF magnetron sputtering using aluminum nitride target. The preparation of c-axis oriented AlN lms having desired properties without substrate heating is highly advantageous in device fabrication. This reduces the deposition cycle time and simplies the deposition system resulting in higher throughput at reduced cost. If the AlN lms are to be used for device manufacturing, this will be a very attractive feature. The primary objective of the present work is to produce highly c-axis oriented AlN lms on various substrates (glass, Si, oxidized Si, AlSiO2Si, CrSiO2Si, and AuCrSiO2Si) without external substrate heating. This aspect

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becomes critically important when the oriented AlN lms are required to be prepared in device fabrication (e.g. FBAR) where the oriented lms must be prepared on a conducting lower electrode such as CrAu or Al. 2. Experimental details AlN lms were prepared on different substrates using an aluminum nitride ceramic target of 3-inch diameter. The depositions were carried out in RF magnetron sputtering system (Alcatel SCM 450) in sputter-up conguration in pure argon and mixed ArN2 (1:1) ambient. The summary of deposition process is given in Table 1. The role of the substrate on the crystallographic orientation of AlN lms was investigated. A variety of substrates were chosen for this purpose keeping in mind the structure of some the commonly used sensors based on ZnO and AlN piezoelectric materials [21,22]. The lms were prepared on: Si, oxidized Si, CrSiO2Si, AuCrSiO2Si, and AlSiO2Si substrates. The sputtering was carried out in ArN2 ambient at 0.67, 1.33, 2.66 Pa pressure at 300 W power. Further, to make the results comparable, the thickness of the lms was kept constant (~ 1 m) for all the samples. The thickness of the lm was measured by reectance measurement (Filmetrics, US; Model: UV-20). X ray diffraction (XRD) measurements of the lms were performed on a Philips X-ray diffractometer (Model: X'pert). Fourier transform infrared spectroscopy (FTIR, BIO-RAD, Digital Division, Model: FTS-40) was used to conrm the presence of AlN bonds in the lms. Surface roughness of the lms was measured by atomic force microscopy (AFM, Nanoscope III A, Digital Instruments). Scanning electron microscope (SEM, Zeiss, EVO 50) was used for observing the columnar growth in the cross-section of the lms. Metalinsulator-semiconductor (MIS) and metalinsulatormetal (MIM) structures were fabricated by using thermally evaporated circular Al dots (2 mm diameter) and the DC resistivity of the lm was calculated from the currentvoltage (IV) measurements (Keithley, 2400 source meter). 3. Results and discussions 3.1. Deposition rate Deposition rate is an important parameter to control the lm thickness. The effect of sputtering pressure and ambient gas (Ar and ArN2) on deposition rate is shown in Fig. 1. It shows that mixing of N2 gas with Ar signicantly reduces the deposition rate which is expected due to the lower sputtering yield in N2 as compare to that in Ar [13,23]. Fig. 2 shows the deposition rates of AlN lms prepared in ArN2 (1:1) ambient as a function of sputtering gas pressure and RF power. It is observed that for a given sputtering pressure, the deposition rate increases almost linearly with RF power [18,19]. It can be further inferred from Fig. 2 that the deposition rate also increases with sputtering pressure for all the RF power values used in the present work. However, the change is less visible at 100 W power

Fig. 1. Deposition rate with sputtering pressure for Ar and ArN2 (1:1) mixture at 300 W power.

as the deposition rates are anyway quite low [21,22]. The results of deposition rate under different sets of sputtering conditions in ArN2 (1:1) ambient are summarized in Table 2. 3.2. Structural characterization 3.2.1. X-ray diffraction In order to investigate the structural properties as a function of sputtering parameters, AlN lms were sputter deposited on glass substrate at 2.66 Pa pressure. Fig. 3 shows a series of XRD pattern of the lms deposited at different RF powers in pure Ar ambient. It can be seen that no preferred orientation is obtained for the entire range of RF power (100300 W) used for the sputtering carried out in pure Ar ambient. Fig. 4 shows the XRD pattern of the AlN lms deposited in a mixed ambient of ArN2 (1:1) on glass substrate. The preferred growth of (002) orientation starts appearing at 200 W power. At 300 W power, the AlN lm grows with strongly preferred (002) orientation as shown in Fig. 4. The possible reason for highly oriented growth at 300 W power is presumed to be the self heating of the substrate and the lm due to plasma bombardment. To conrm this presumption, the deposition of

Table 1 Sputtering conditions used for preparing AlN thin lms. Deposition parameters Substrate temperature Base pressure Target RF power Sputtering ambient Sputtering pressure Targetsubstrate distance Substrate Values No external substrate heating 2 10 4 Pa (1.5 10 6 Torr) AlN (99.9%, 3 diameter) 100, 200, 300 W Ar or ArN2 (1:1) 0.67, 1.33, 2.66 Pa (5, 10 and 20 mTorr respectively) 50 mm N-type Si (100), 2 inch diameter, 510 cm; glass; SiO2 (1 m)Si; Al (200 nm)SiO2Si; Cr (200 nm)SiO2Si; and Au (200 nm)Cr (50 nm)SiO2Si

Fig. 2. Deposition rate at different RF power and sputtering pressure in ArN2 (1:1) ambient.

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Table 2 Deposition rate of AlN lms prepared in different sputtering conditions in Ar-N2 (1:1) ambient. Sputtering perssure Pa 2.66 2.66 2.66 1.33 0.67 (20 mTorr) (20 mTorr) (20 mTorr) (10 mTorr) (5 mTorr) Power W 100 200 300 300 300 Deposition rate nm/min. 2.7 10.0 13.5 10.5 9.6

AlN was also carried out using a specially designed substrate holder which enabled efcient cooling of the substrate during the entire process of lm deposition. The results were compared with those samples which were prepared under identical conditions, except that sample holder was of somewhat different design and not water cooled. The XRD pattern of these samples deposited at 1.33 Pa and 300 W in mixed Ar-N2 ambient is shown in Fig. 5. It shows that the lm prepared using water cooled substrate holder under otherwise identical deposition conditions shows a very weak (002) peak compared to the one obtained for the sample prepared without cooling. It is known that the substrate temperature rises signicantly during the sputtering process and its dependence on RF power has been reported earlier [24,25]. This experiment conclusively conrms our original presumption that self heating during lm deposition plays a crucial role in getting highly c axis oriented lm. The XRD pattern of AlN lms deposited on: Si, oxidized Si, CrSiO2Si, AuCrSiO2Si, and AlSiO2Si substrates are depicted in Fig. 6. It is evident that a strong (002) peak is observed for all the samples prepared in the sputtering pressure range (0.672.66 Pa) at xed 300 W power. The second most intense peak appeared corresponding to (103) plane, except in case of gold coated substrates where (101) peak is the second dominant peak for sputtering pressure of 0.67 Pa. The ratio of the intensity of (002) and (103) peaks is used as an indicator of the structural quality of the lm. Fig. 6(d) shows the XRD pattern of AlN lm deposited on AuCr SiO2Si substrate. The lm prepared at 0.67 Pa pressure shows (101) as the second most intense peak while at 1.33 Pa (103) peak becomes the second most intense peak. The reason for this change in XRD pattern with pressure may be attributed to surface roughness of the substrate and this could be a subject of further investigation. We also observed that on further increasing the pressure to 2.66 Pa the peak intensity ratio I002 / I103 decreased (b10). So, for AuCrSiO2Si substrate, highly c-axis oriented lm was obtained at 1.33 Pa sputtering pressure. At relatively

Fig. 4. XRD pattern of AlN lms on glass substrate prepared at 100, 200 and 300 W RF power in ArN2 (1:1) ambient at sputtering pressure of 2.66 Pa.

high pressures (2.66 Pa) the deposition ux is substantially randomized giving rise to a more isotropic growth or, in other words, creating conditions for non-normal cone growth. For this purpose, lower pressures (0.671.33 Pa) result in lms with a better texture. Accordingly, it is evident that the sputtering pressure of 0.67 and 1.33 Pa is more favorable for the preferred (002) orientation, although c-axis oriented lms were also obtained at 2.66 Pa sputtering pressure. Xu et al. [12] studied the effect of sputtering pressure on the orientation of the lm prepared by reactive sputtering of Al target in N2Ar ambient without external heating of the substrate. They observed that the orientation changes from (002) to (100) as the sputtering pressure was increased from 0.4 Pa to 0.6 Pa. Cheng et al. [13] also reported similar change in preferred orientation from (100) to (002) in RF magnetron reactively sputtered AlN lms deposited under varying sputtering pressures of 0.182.66 Pa (1.420 mTorr). The substrate temperature of 350 C and N2 concentration of 75% was used in their deposition process. Cheng et al. [23] investigated the effect of N2 concentration on the orientation of AlN lms prepared by reactive sputtering of Al target. They observed that under low nitrogen concentration (25%) the AlN lm showed (100) preferred orientation. Increasing the nitrogen

Fig. 3. XRD pattern of AlN lms on glass substrate prepared at 100, 200, and 300 W RF power in Ar ambient at sputtering pressure of 2.66 Pa.

Fig. 5. XRD pattern of AlN lms on Si substrate prepared using (a) water cooled substrate holder, (b) substrate holder without cooling. The lms were prepared at 300 W in ArN2 (1:1) ambient at sputtering pressure of 2.66 Pa.

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Fig. 6. XRD pattern of AlN lms prepared at 300 W in Ar-N2 (1:1) ambient at sputtering pressure of 0.67, 1.33, and 2.66 Pa on (a) Si(100), (b) thermally oxidized Si, (c) CrSiO2Si, (d) AuCrSiO2Si, (e) AlSiO2Si substrates.

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concentration up to 75% resulted in lms with (100), (101) and (002) mixed orientation. On further increasing the nitrogen concentration to 100% they observed the strongest c-axis (002) orientation in the lms. Such dependence of preferred orientation was also observed in the work done by Clement et al. [26] using RF diode reactive sputtering. An abrupt change in the orientation of the lms was observed as the sputtering pressure was changed from 0.53 Pa (4 mTorr) to 0.67 Pa (5 mTorr). These studies indicate the sensitivity of the reactive sputtering process on sputtering pressure to obtain the preferred (002) orientation. Accordingly, even a slight deviation in pressure may cause change in the AlN lm orientation from (002) to (102). Furthermore, it is reported that a small change in self-bias of the substrate is also responsible for strong dependence of preferred orientation. The self-biasing of the substrate during sputtering process depends on the geometry of the system through the stray impedance between the substrate holder and the ground or on any impedance externally added to the system [26]. It is evident that the sputtering parameters need to be controlled critically in a narrow window to obtain desired orientation of AlN lms prepared by reactive sputtering of the Al target. In the present work, we did not observe such a strong dependence of preferred orientation of AlN lms on sputtering pressure. From the view point of process reproducibility in manufacturing environment, it can be inferred that the present method of preparation of c-axis oriented AlN lms using AlN target is a superior and less cumbersome process compared to the method of reactive sputtering of Al target as the sputtering pressure and nitrogen concentration need to be controlled very precisely during the deposition. Scherrer's formula is used to evaluate the grain size of (002) oriented crystallite. Peak position for (002) orientation, full width at half maxima (FWHM) and grain size corresponding to different substrates and sputtering pressure are summarized in Table 3. The distribution of grain size is found in the range of 1726 nm.

Fig. 7. FTIR absorption spectrums of as-deposited AlN lms prepared on double side polished silicon wafer at 300 W in ArN2 ambient.

almost identical for the sputtering pressure range used in the present work. This implies that the change in sputtering pressure does not inuence the chemical composition of the lm. In the region from 2000 to 2200 cm 1, another weak peak is observed which may be assigned to vibration mode of NAlN bonds [27].

3.3. Cross-sectional SEM and surface morphology The cross-section of a representative AlN lm deposited on AlSiO2Si was observed under SEM at 50,000 magnication. As shown in Fig. 8, the columnar structure is clearly visible, which conrms the highly oriented columnar crystals perpendicular to the substrates. Similar columnar growth was also reported in reactive sputtered AlN lms [11]. Hwang et al. [28] reported 10 tilted columnar growth of AlN lm normal to the substrate with diffused interface boundary. The morphology of the lms deposited at the same set of parameters (0.67 Pa and 300 W) on different substrates is shown in Fig. 9. The root-mean-square roughness (Rm) of the lms is tabulated

3.2.2. FTIR transmittance The infrared transmission spectra of as-deposited lms in N2Ar ambient at different pressures (0.67, 1.33 and 2.66 Pa) are presented in Fig. 7. A strong absorption peak near 670 cm 1 is observed. It is attributed to the transverse optical phonon modes {E1(TO) mode} of AlN [23]. This further conrms that the deposited lms were of stoichiometric AlN. The absorption peak position and intensity are

Table 3 XRD (002) peak position, FWHM and calculated grain size of AlN lms (from Scherrer's formula) for various substrates with sputtering pressure (RF Power: 300 W, ambient: Ar-N2). Substrate Sputtering pressure (Pa) 0.67 1.33 2.66 0.67 1.33 2.66 0.67 1.33 2.66 0.67 1.33 2.66 0.67 1.33 2.66 0.67 1.33 2.66 (002) Peak position 2 (degree) 35.93 35.95 35.98 35.86 35.85 35.66 35.93 35.76 35.73 35.99 35.92 36.04 35.98 35.96 35.78 35.88 35.99 35.86 FWHM (degree) 0.32 0.39 0.42 0.50 0.32 0.39 0.35 0.35 0.36 0.40 0.37 0.38 0.36 0.35 0.45 0.42 0.34 0.40 Grain size (nm) 26 21 20 17 26 22 24 24 23 21 23 22 23 24 19 20 24 21

Glass

Si

SiO2

AlSiO2Si

CrSiO2Si

AuCrSiO2Si

Fig. 8. Cross-sectional SEM image of AlN lms on AlSiO2Si substrate observed at 15 with respect to the substrate plane.

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5.0 m

5 m

2.5

2.5

0 0

2.5 150 nm

0 5.0 m

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0 5 m 250 nm 5 m

0 5 m

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2.5

0 0

2.5

0 5 m 150 nm

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0 5 m 100 nm

0 5 m

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0 0

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0 5 m

Fig. 9. AFM images of AlN lms deposited at various substrates at identical sputtering parameters (a) Si, (b) SiO2Si, (c) CrSiO2Si, (d) AuCrSiO2Si and (e) AlSiO2Si.

in Table 4. The roughness of the lms was found to be dependent on substrate used. The minimum roughness (Rm = 6.3 nm) was observed for Au-Cr-SiO2-Si substrate while maximum (Rm = 14 nm) for oxidized Si substrate.

3.4. Bulk resistivity of the lms For the AlN lms to be useful as a piezoelectric material in MEMS and SAW devices, the resistivity of these c-axis oriented lms must also be

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Table 4 Surface roughness of 1 m thick AlN lm deposited on various substrates in ArN2 ambient (Sputtering pressure: 0.67 Pa, Power: 300 W). Substrate Si SiO2Si CrSiO2Si AuCrSiO2Si AlSiO2Si Surface roughness Rm (RMS) in (nm) scan size (5 5) m2 7.7 14.0 9.3 6.3 12.9

target was reported by Bakalova et al. [32]. They observed relatively low resistivity, of the order of 105 cm. The AlN lms prepared in the present studies are of high resistivity (10111012 cm at eld of 50 kV/cm). These are comparable to the bulk resistivity, as reported in the literature [33]. These values of resistivity are considered acceptable for the device fabrication. 4. Conclusion We have investigated the deposition of AlN lms by RF magnetron sputtering of AlN target without external substrate heating. Highly c-axis orientated AlN lms were prepared on various substrates without external substrate heating at 300 W power, 50 mm target to substrate spacing, and 0.672.66 Pa sputtering pressure in the mixture of ArN2 (1:1) gas. The orientation and crystallinity of AlN lms strongly depend on RF power and sputtering gas composition whereas sputtering pressure weakly inuences the preferred growth. XRD analysis clearly demonstrates that highly c-axis oriented lms can be prepared on a variety of substrates. This was further conrmed by cross-sectional SEM image which shows columnar growth perpendicular to the substrates. AFM images revealed the uniform grain distribution of smooth AlN lms on different substrates used in this study. For devices like SAW and FBAR resonators, the resistivity of the lm plays a critical role and high resistivity lms are desired. The lms prepared in the present work exhibit high resistivity in the range of 10111012 cm at moderate electric eld and are suitable for the above mentioned applications. The lms prepared on substrates with metal lms are required for BAW resonators. Sputtering, without external substrate heating, is advantageous in terms of simpler system design and higher throughput. Furthermore, it is clearly demonstrated that the AlN lms meet the requirements of SAW and BAW devices without post-deposition annealing which is an advantage for MEMS integration with CMOS processing. References
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high. For this purpose, MIM and MIS structures using AlN insulating lm were fabricated. Circular electrodes of 2 mm diameter were used as gate electrode for both the structures. The AlN lms were deposited at 1.33 Pa sputtering pressure and 300 W Power in Ar-N2 ambient. Fig. 10 shows the current densityvoltage (JV) plot of (i) as-deposited lm on Si, (ii) post-deposition annealed lm (900 C for 60 min.) on Si and (iii) as-deposited lm on AlSiO2Si substrate. The rst two measurements were done using MIS structures while the last one was done with MIM structure. The IV measurements were restricted to moderate values of electric elds (up to 100 kV/cm) keeping the device structures in view where these lms have potential applications [29]. It can be seen that the JV characteristic is almost identical for positive and negative gate voltages for the MIM structure, as was expected. The current density is below 0.1 A/cm2 for the gate voltage values below 5 V. For the MIS structure, somewhat higher values of current density are observed for negative gate voltage (VG) for asdeposited lm. Annealing of the lm at 900 C improves the insulating properties considerably by reducing the leakage current for both positive and negative voltages. This decrease in leakage current may be attributed to partial removal of the defects by the heat treatment. The electrical conduction of MIS capacitors with thin insulating lm can be explained in terms of Schottky effect, FowlerNordheim tunneling or the PoolFrenkel effect [30]. It is presumed that the current in low eld region is due to the Schottky effect i.e., the potential barrier is decreased with increase in voltage and carriers are emitted. The current in relatively high eld region is mainly due to the FowlerNordheim tunneling current emitted from the cathode. We have not observed current corresponding to Pool Frankel effect in the voltage range used in our case. The detailed study of conduction mechanism of AlN was not aimed in the present work. The resistivity of the lms was calculated for low electric eld (50 kV/cm; VG = 5 V) and found to be in the range of 1011 to 1012 cm. The electrical resistivity of reactively sputtered AlN lms reported by Spina et al. [31] was observed to be in the range of 10121014 cm. The electrical resistivity of the AlN lms deposited by PLD with AlN

Electric Field (E) (kV/cm)

10-2 10-3 1x10-4 0 10 20 30 40 50 60 70 80 90 100
MIS (as-deposited film) MIS (post deposition annealed) MIM (as-deposited film )

Electric Field (E) (kV/cm)

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Fig. 10. JV plot of MIS and MIM structures with AlN lms prepared at 300 W in ArN2 (1:1) ambient at sputtering pressure of 1.33 Pa.

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